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User Manual - PID Eng&Tech

1. CC AOL LA l MFCO1 pricy I L REA bo VvM 1 evol l MFCO2 PEKA i A KEA GAS 2 AI CHO gt ren JL debkIeL 5 2 J vMO2 CDA Let de d j MFCOS Fics SC MU d GAS 3 CHA E VO COD MFCO4 FEA l cn Ki VMO4 vos l MFCOS Fo GAS OUTLET ps Set OP P E DI e VM S cvos ep CO Taa EE E DEE MFCOG FER SS SS ULT eto NIE E CH CLC cn BOSA Vd KML i GAS 6 CH bk VMO6 CV06 l l i E l E E RI M wel aw RA ER E El 70 PID Enga Tech LIC LILIN D 26d AUTOMATIC 6 PORT VALVE TO REACTOR FLOW UP DOWN SELECTION Oo BPO1 V i HOT BOX TE Bec CIE GER t ap CO KOL SL l l MECO1 P A KA VMO1 Cup MFCO2 Fe CH GAS 2 et HHH K VMO2 cvo2 FAA MFCO3 P zs NA Ve Cv03 MFCO4 FE cn Mi l VMO4 CV04 MFCOS P E tle He gt SA D EI VEOS Cv s ae Cer CC E ET DEE FCOG g s fm Por i Ur eet TIF TIF GAS 6 DeL Og VMO6 CV06 71 PID Enga Tech 2nd six port valve activation Figure 4 47 4 7 5 OPTION D1 4 PORT MANUAL VALVE 4 port manual valve Figure 4 48 12 PID Enga Tech 4 port valve option is useful to isolate the reactor and prevent contamination inside when necessary to remove the reactor inside the unit This valve has two positions One for normal operation and one when removing the reactor 73 PID Enga Tech MAPGLIMS WITH 4 PORT MANUAL VALVE T
2. 00 21 06 Days 00 08 54 Days 3 AU E er Ti lv 0 Ja Y o Y 0 gi EA ara jo 17 Reset scale in Y 0 7 Y GCLINE mio Lo Session table v HPLCPUMP c o Y HPLEPUMP R 0 Y UCI su Jo 1 PELTIER o 0 v Pic 0 0 x v si 0 0 ug Y 0 0 0 0 O 0 H 0 TIC HB 0 0 160 o D 10 0 0 500 TOTALIZER RST 0 HPLCPUMP2 C 0 2 0 o 0 v HPLCPUMP2 R 1 0 0 0 UC ut D E 0 0 5 Je KAT Experiment Name 20100505091905 Figure 4 39 64 PID EngaTech Kr MAS ba e Wir WS ar gt Lett Lo EE 17125 3 ao GAS WI SASA 3554 1 Y lel Wa a E EL da od d H Y H zech A 0 EN ol amp Figure 4 40 Reset scale is possible in any moment of the session by means of right button of mouse over scale icon 65 4 7 3 OPTION C MASS FLOW METER IN GASES OUTLET Gases flow is counted at the exit of gases through the installation of a mass flow meter A coalescing filter condenses the liquid before passing through the meter Liquids condensed are removed via the bottom of the filter Measuring principle is the same as described in option A When chossing this option it i
3. Figure 7 5 Configure the fields of the new MFC Maximum flow Units in which the gas flow is expressed Name of the gas of alarm Deviation alarm This alarm is inhibited during the time specified in the Delay Time Alarm in sec operating if during this time the specified deviation is maintained with respect to the set value These parameters are modified by pressing on their corresponding yellow boxes and entering the new values by means of the keys that are displayed on screen Before beginning to work with the equipment it is important to ensure that each reactant gas MFC installed has been properly set up and that all the other MFC s not installed have their fields set to zero Press the Exit key to return to the main menu 138 PID Enga Tech 8 EUROPEAN DIRECTIVES 1 Directive 97 23 EC Pressure Equipment The plant complies with European Directive 97 23 EC and Spain s Royal Decree 769 1999 that lays down the provisions for the application in Spain of said directive regarding the design manufacture and evaluation of compliance of pressure equipment and equipment subject to a maximum allowable pressure PS exceeding 0 5 bar The plant is supplied with Markings and Statement of Compliance as per article 3 section 3 of European Directive 97 23 EC and Spain s RD 769 1999 2 Directive 94 9 EC Equipment and protective systems intended for use in potentially explosive atmospheres The plant is not
4. ossoFlOUD ABS nm oo ON LEVEL CONTROL S om om MAS FLOW CONTROLLERS Dev oF ou o DOOROPENDETECTOR Relay o o OVENOPENDETECIOR Relay OFF OFF om EXTERNAL aam Relay OFF OFF om ON PRESSURE SERVO CONTROL Relay OFF OFF OFF ON ON or ON on Table 4 7 SUMMARY TABLE OF THE ALARM FUNCTIONS REACTOR OVEN HOT BOX HEATER HOT BOX CONVECTOR REACTANTS MFC s INERTS MFC s LIQUIDS PUMP 1 Actions defined by the user in the set up menu for the reaction pressure and temperature alarms on the touch screen of the Microactivity Reference 2 The inhibition session is activated in the event of a pressure alarm with this status persisting until the user resets the alarm on the alarm panel on the touch screen In all other alarm scenarios the inhibition function is deactivated automatically once the system s parameters return within the established control limits 94 PID Enga Tech 5 PROCCESSO CONTROL SOFTWARE 5 1 INTRODUCTION Process control software is an application for data supervision and acquisition designed for systems based on digital communications between process hardware and a personal computer The use of this application allows data acquisition and the remote control of one or several Microactivity Reference units via Ethernet type communications This software has been developed with National Instruments LabVIEW which has the
5. 0 0 0 0 0 0 0 0 0 0 0 0 Name of the experiment 1 Session 5 Session6 Session Session8 Session 9 Session 10 Session 2 Session 3 Session 4 Session 5 Session 6 HEATING REACTION COOLING OPENDOOR CLOSE DOOR 1800 2000 1800 1000 10 x Session2 Session 3 Session 4 Session 7 Session 8 Session 9 Session 10 Figure 5 36 Sessions table Time In this area the total experiment time the consumed session time and the session time remaining can be set In the upper section there is an indicator whose normal mode is OFF and that will turn red when the door is opened or when the inhibition which is activated in case of alarm goes off When the inhibition is activated the PC will stop sending values to the Microactivity and the session time Will stop at that point 114 PID Enga Tech Sessions Control In this area the buttons that manage the session are displayed a Show All to display all the device parameters The previously hidden parameters can be chosen from the whole list by clicking on them so that they remain in the shorter list Choose among all the parameters the ones to work with to do this it is necessary to dropdown the whole list The icon next to them will turn from red to green When pressing SHOW ALL again only the parameters with the green icon will remain The rest will be hidden a Run Stop to start stop the session When clicking on Run the application starts sending sessi
6. PH 34 918 459 930 FAX 34 918 486 454 Enga Tech C Plomo 15 Pol Ind Sur E 28770 Colmenar Viejo www pidengtech com Madrid Spain MICROACTIVITY REFERENCE USER S MANUAL V8 2 Wo Camara 150 14001 y HM E e yt A 1S0 9001 e ees SKS a PARQUE i MA c T EAU VERITAS as BUREAU VERITAS BUREAU VERITAS beo e a CIENT FICO Certification Cortificaion me Cor Certification Certificatio een VIV Y DE MADRID N ES020741 N ES020743 3 i PROYECTO I D i Enga Tech MICROACTIVITY REFERENCE USER MANUAL CONTENTS 1 INTRODUCTION 1 1 1 USING THIS MANUAL 1 1 2 SAFETY INFORMATION 1 2 1 SAFETY INFORMATION 2 UE e RE dE 2 1 2 3 WARNING AND CAUTION CAT 2 1 2 4 ELECTROMAGNETIC COMPATIBILITY eene 3 2 DESCRIPTION OF THE EQUIPMENT 4 2 1 GENERAL DESCRIPTION criadas 4 2 20 PEI MON eege Ee 6 2 3 OPERATING CONDITIONS cooccccccccccccccnnnnnnnnnnnnnnnccnnnnnnnnonononnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnanes 6 2 4 EQUIPMENT APPEARANCE A 6 2 4 4 GENERAL VIEW 7 24 2 FRONT VIEW ccc cece cece eee e ee eeeeeeeeeeeeeeeeeeeeeaaaaaaaaaceeeeeeeeeeeeeeeeeeaaas 7 2 4 3 INSIDE VIEW ssssseseeeeeeeeenem mmn nnn n nnn nennen nennen 8 2 4 4 REAR VIEW e PP o nnn 8 2 45 INSIDE VIEW ELECTRONICS oocccccccnnnnnononcccnnnnnnnnnonononononnnnnnnncccnnnnnnnos 9 3 INITIAL INSTALLATION 10 Sl BEFORE STAR TING sail 10 3 1 1 TEMPERATURE AN
7. C Control valve failure The final elements of pressure and level control are servo positioned micro regulating valves A failure in the control system of these valves triggers an alarm of the same type as that triggered by their master control loops A failure in the position of the pressure control valve generates a procedure similar to that generated by a pressure alarm and a failure in the level control valve generates a procedure similar to that caused by an alarm in the separator s level controller 5 INH Inhibition function Whenever the INH function is activated by any one of the system s alarms the Process Q control application automatically interrupts the performance of interconnected sessions The system s control program will remain in stand by until the operator manually implements the change of session once the cause of the alarm has been resolved gt External alarm A signal coming from an outside system for detecting gases fire or such like may trigger a general alarm in the system that involves disconnecting the hot box heater the reaction oven the liquids pump and the MFC halting the operation of those the user has selected on the external 93 PID Enga Tech alarm set up panel on the system s touch screen triggering the audible alarm buzzer and generating the system s inhibition signal REACTION TEMPERATURE ABS OFF oe nm ON o HorBoxTEMPERATURE ass ON PRESSURECONROL ABS nm oo
8. Relay Peltier 8 9 9 yet gt gt e CH EI 969 9 9 9 6 Port Valve e f H rs S vi 2 3 m d t EN y yes SSR Furnace SSR Hot Box Heaters SSR GC Heater SSR Evaporator Micrometric valve for pressure control opt Electrovalves Pressure sensor opt Gas Mixer Mass Flow Controllers Figure 2 6 3 INITIAL INSTALLATION 3 1 BEFORE STARTING Before the equipment arrives make sure your laboratory meets the following environmental weight power and gas requirements You can find more site preparation information in this chapter Site Preparation Checklist PID Enga Tech O The site is well ventilated and free of corrosive materials and overhanging obstacles Site temperature is within the recommended range Site humidity is within the recommended range Bench space is adequate for the equipment Bench can support the weight of the equipment 1 Power receptacle is earth grounded Electrical supply meets all equipment s power requirements Voltage supply is adequate for oven type Gas supplies meet the requirements of the equipment Gases and air supply meet the pressure requirements and have two stage pressure regulators installed 3 1 1 TEMPERATURE AND HUMIDITY RANGES Operating the unit within the recommended ranges insures optimum instrument performance and lifetime Hecommended temperature range 18 25 C Temperature range 5 40 C Hecom
9. 274 065 E E E 17 Carbon dioxide Io 197 074 v E v 18 Carbon disulfide cs2 3397 06 v v v 19 Carbon monoxide co 125 1 v v v 20 Chlrine JL OG 3218 082 v v v 21 Chlorine trifluoride CF3 4125 04 P P P 22 Cyanogen Low 2376 048 P P P 23 Cyanogen chloride CIN 2743 061 P P P 26 Diborane B2H6 1243 043 P P P 27 Dibromo difluromethane Br2CF2 9361 02 v P v 28 Dichlorosilane SiH2CI2 45060 041 V P V 29 Dimethylamne C2H6NH 2011 037 P P P 31 Dimethylether__ C2H60 2105 039 P P P 32 disilane SoH6 2857 031 v P V 34 Ethylene Ethene on 1261 06 v tE V 35 Ethylene oxide Long 1965 052 P P P 38 Fluorine JL F2 166 091 P P P lt lt m lt lt m lt lt lt m m lt ZIZ lt lt lt lt I E lt X lt mM X lt lt lt lt lt lt 99 Enga Tech 44 Freon 116 C2F6 6 157 0 25 E erenn om Y Freon 13 CCIF3 4 72 V V V Car ieoa rs eje v v v SE NU OS N P Freon 22 CHCIF2 3 936 0 47 Freon 23 CHF3 3 156 0 52 E T E szmer cre 932 ois t E t 53 Germane Gema 345 056 v V V Sa Heium He ovs iM V V V 55 Helium 3 JL 3He 01346 14
10. 5 2 3 HOW LINK THE PC AND THE MICROACTIVITY REFERENCE The Microactivity Reference and the control PC can be linked by Ethernet directly using a cross cable In addition they can be connected to a switch by using a straight cable which will allow having one or multiple pieces of equipment connected to the network In any case the right communication parameters must be introduced in the Microactivity and the PC so that they be linked 5 2 3 1 MA REF COMMUNICATION PARAMETERS These parameters must be set in the touch screen s F1 menu under Communication Setup The default parameters are MA Ref COMMUNICATIONS SETUP IP ADDRESS 192 168 0 s These parameters _IP MASK e255 RO 255 A T J GATEWAY 192 168 0 TCP PORT 1234 Table 5 1 Microactivity Reference Communication Parameters 99 PID Enga Tech In case of using other communication parameters or connecting it to a local network make sure the GATEWAY and IP MASK are the same in the Microactivity and in the PC 5 2 3 2 PC PARAMETERS The PC communication parameters are configured at the network connection window under the control panel To do so follow these steps Right Click on Local Ne
11. Once the installation has been made the following steps are to be performed in order to introduce gases into the system 1 Open the pressurised gas cylinders 2 Adjust the inlet pressure for each one of the gases by means of the pressure reducers 3 Open the on off valves for each gas on the lower part of the front panel At this point the system is ready to operate Inversely upon concluding operations with the Microactivity Reference proceed as follows Reduce the inlet flows to zero for each one of the reactant gases Preferably flush the installation with inert gas for 5 min Close the on off valves on the front panel Whenever possible close the reactant gas cylinders and reduce the pressure of the pressure reducers to zero if the system is leak free the inlet lines to the system will register the inlet pressure In the case of compressed air the installation is to remain permanently pressurised in order to permit the pneumatic operation of the valves and the door on the hot box DUIS 3 2 5 TURNING THE POWER ON Verify that the power switch is in the OFF position o Plug the power cord into the power receptacle Put the circuit breaker in ON position and turn the power on with the frontal switch position 18 PID Enga Tech 4 COMPONENTS OF THE MICROACTIVITY REFERENCE UNIT Figure 4 1 shows a diagram of the items that constitute the Microactivity Reference reactor s arrangement of lines and instrument
12. Figure 3 13 WARNING Before connecting the equipment s power supply make sure that the main circuit breaker is in the OFF position Figure 3 14 Figure 3 13 Figure 3 14 17 PID Enga Tech 3 2 4 GAS INSTALLATION Once the electrical installation has been performed the next step is to install the gases that the Microactivity Reference unit is going to work with To do so all that is required is to connect a 1 8 line preferably of 316 stainless steel between the pressure reducers on the gas cylinders and the system s gas inlet which is to be found on the upper part of the equipment Figure 3 1 The connection is to be made as follows Synthetic air o Inlet pipe Polyethylene 6x4 mm pipe supplied with the equipment 3 m Air o Connection Quick fit connection pressing the pipe supply against the adapter o Inlet pressure 5 bar o It operates on the pneumatic systems for door and oven opening 6 port valves etc Gases 1 2 etc Reaction gases o Inlet pipe 1 8 pipe in 316 stainless steel Heads o Connection Gyrolok 1 8 adapter gases o Inlet pressure 5 10 bar above the operating pressure The inlet pressure for each one of the gases depends on the mass flow controller installed whereby its specifications should be consulted before making the gas connection o The gas inlet position 1 2 etc depends on the arrangement of the mass flow controllers on the equipment Figure 3 15
13. LOADING A CATALYTIC BED IN THE REACTOR Insert the catalytic bed inside the reactor by proceeding as follows 1 Open the reactor hot box by pressing the Door key on the touch screen 2 Disconnect the reactors thermocouple red pin This will trigger the system s temperature alarm which can be deactivated on the touch screen s alarm panel see section 4 5 1 in this manual 3 Using a spanner loose the A connections see Figure 6 1 4 Hold the reactor with a clamp on the upper part B and loose that connection by exerting pressure on C 5 Place the reactor in a vertical position unscrew B and remove the thermocouple from the reactor 6 Empty the reactor and flush with compressed air through the lower end in the opposite direction to the gas flow inlet 7 Insert the catalyst through the upper end of the reactor with a particle size greater than 10 um a small quantity of quartz wool may be inserted beforehand to avoid access of fine particles through the porous plate and if considered necessary pack the reactor with carborundum up to 2 3 cm below the upper end in order to avoid the dead volume Figure 6 1 8 Clean threads B and C insert the thermocouple inside the bed close the reactor and reconnect the gas inlet and outlet lines by means of connections A 9 To avoid a heating peak in the reactor oven switch off the Microactivity Reference before plugging the thermocouple into the hot box Then s
14. Put the level controller in manual mode totally closed 0 Once the system is at working pressure it would be necessary to check if this valve is totally closed or if it is necessary to recalibrate the zero point Puta tap in the gas outlet on the hot box and introduce an inert gas flow in the system He No etc Put the unit at habitual working pressure Close the gas inlet as well as the system on off stopcock for gas and verify that the pressure in the system remains constant over a period of time If this is not the case use a soapy solution to locate possible leaks subsequently dry the entire system When the leaks has been detected and eliminated clean the equipment removing the soapy solution 7 1 2 CLEANING THE UNIT For clearing the external of the unit use a wet cloth with water for preventing dust accumulation For internal cleaning it can be used water or any solvent alcohol acetone etc for eliminate soapy solution rest In case of cleaning with any solvent the user has to manage properly the generated residues attending to its nature 7 2 MONTHLY QUARTERLY MAINTENANCE Depending on the use of the reactor and the reaction products the user should make a monthly or quarterly maintenance consisting on 7 2 1 REPLACING THE FILTERS The reactor is provided with two 15 microns filters that could get blocked as a consequence of the continuous use If that occurs replace the filter by another one
15. Ref Swagelok SG_SS 2F 15 The replaced porous plate could be contaminated with hydrocarbons or other kind of residues The user of the unit must manage these residues asking to an authorized manager and attending to the environmental policy of the laboratory where it is being used 134 PID Enga Tech 7 3 ANNUAL OR LATER MAINTENANCE 7 3 1 REPLACING THE FUSE The Microactivity Reference has incorporated a 3 A fuse at the rear of the reactor for protecting the power sockets For replace it Figure 7 1 turn the equipment off put the circuit breaker in the OFF position and replace it by another one with the same characteristics 3 A 250 V 3 A FUSE Figure 7 1 7 3 2 REPLACING THE KALRETZ SEALS IN THE GAS MIXER If the unit woks with high corrosive gases it should be convenient to replace annually or later the kalretz seals of the check valves before the gas mixer Open the valves body and replace the elastomeric seal by another one same model and material contact with Process Integral Development Eng amp Tech Technical Service The replaced o ring could be contaminated by any corrosive gas The user of the unit must manage these residues asking to an authorized manager and attending to the environmental policy of the laboratory where it is being used 7 3 3 REPLACING THE REACTOR POROUS PLATE Due to a continued use of the unit with high viscosity liquids or substances that generate solid deposits the poro
16. even after the Show All has been turned off Data Table n this area introduce the data that is going to be written on the devices for each session Data can only be input in a session in the session time has been filled out To move from one parameter to another use the arrow keys of the keyboard When the session execution has been launched the current session can be identified because its column will be displayed in blue If there aren t any blue columns it means there is not any session being executed 115 PID EngaTech The input data must be among the ranges allowed by the devices parameters For example the ON OFF devices only accept either a 1 or a O for ON or OFF In the same manner for the controller s output exit enter values between 0 and 100 In the following table the different parameters that can be configured are resumed PARAMETERS ON OFF S E O CONTROLLERS REACTOR TEMPERATURE Pbb Manualreset 100 e femore Sg anual Output contro in manual mode HOT BOX Pbb Manualreset 00 De CN OOOO 1 Manual Output control in manual mode Pbb Manualreset 0 100099 O o Less emo 1 Manual Output control in manual mode LEVEL Set Value ml Set value ramping time Slope for the set point ml min 116 Pbb Manualreset AA CC pm e NM anual Lower limit of the output control Set value s upper limit Set value s upper limit Set value s lower limit Set valu
17. lt is used in processes in which the equipment may be damaged by sudden large scale deviations For example in reactions with thermal self ignition equipment featuring rupture discs etc C Criterion of minimum disturbance The control system is to provide a non cyclic recovery curve precisely to ensure that the cyclic variants do not disturb or influence other system processes This situation is forthcoming in concatenated processes in which the oscillations in one subsystem are the result of oscillations in others In a case like this the decision must be taken to overdamp the control systems or perform the start ups as per manual procedures 4 2 3 CONTROLLERS TUNING The values of the proportional band inverse to the gain integral action time seconds repetition and derivative action time seconds of advance need to be conveniently dovetailed with all the other elements in the control loop so that in the event of a disturbance in the system the latter s response fulfils the control stability criterion The adjustment systems are classified into two categories Experimental methods applied when the process model is unknown They determine the process s static and dynamic characteristics on the basis of one of several measurements obtained from the real process The two most frequently used for closed control loops are the trial and error method test error test and the ultimate gain method developed by Ziegler amp Nic
18. maximum of 24 hours to see previous values use the EXPERIMENT VIEWER Output Control Graph m I U 1 1 00 00 00 00 10 00 00 20 00 00 30 j Lu I 1 1 1 U 00 01 00 00 01 10 00 01 20 00 01 30 00 01 40 00 01 50 00 02 00 00 SCLINE HOTBOX Ml LeveL E isese pressure d 100 MIA 100 www HNC 100 mim mt LI tol o0 tom 0 tol 0 Low Co Lou CI llis lo lo jo 49 3 Time T REACTOR 100 Hi C 0 Loa OO 0 1 I 00 40 00 00 50 00 Figure 5 35 Selection of hours or minutes on the time scale 113 PID Enga Tech 5 3 4 SESSIONS TABLES DESCRIPTION By clicking on Sessions Config Sessions a window with a sessions table for our experiment will appear All parameters and the experiment s time must be introduced in this window The Sessions Table tool bar consists of the following options e Load Table to load a session table that has been created previously e Save Table to save a session table e Print to print the session table e Clean Table to clear all the values in the table e Exit to exit the session table menu 5 3 4 1 How to configure a sessions table This table is divided into five zones TEMPLATE Session Table Test Time 01 43 29 Session Time 00 09 59 Remaning Time 00 06 41 Alias Description SessionTime seg Conditional Jump Control Parameter Experiment Name 20080325081530 Session 1 SECURITY
19. service and repair of this instrument Failure to comply with these precautions violates safety standards of design and the intended use of the instrument Process Integral Development Eng Tech assumes no liability for the customer s failure to comply with these requirements 1 2 3 WARNING AND CAUTION CALLS WARNING A warning calls attention to a condition or possible situation that could Cause injury to tha user CAUTION A caution calls attention to a condition or possible situation that could damage or destroy the product or the user s work See accompanying instructions for more information Indicates hazardous voltages AN Indicates a hot surface AS Indicates earth ground terminal 1 24 ELECTROMAGNETIC COMPATIBILITY This device complies with the electromagnetic compatibility requirements subject to the EN 61326 1997 regulation Operation is subject to the following two conditions 1 This device may not cause harmful interference 2 This device must accept any interference received including interference that may cause undesired operation If this equipment does cause harmful interference to PID Enga Tech radio or television reception which can be determined by turning the equipment off and on the user is encouraged to try one or more of the following measures a Relocate the radio or antenna b Move the device away from the radio or television c Plug the device into a different electrical outlet so
20. system s pressure in the controller 144 PID Enga Tech to the set point with the 3 port Release the joint between the system s gas valve in the by pass position outlet line and the reactor box external left hand side of the reactor and see whether the pressure decreases If it does clean or replace the blocked section If it does not continue by verifying the next cause Release the joint between the gas line and the regulating valve and see whether the pressure decreases If it does replace the regulating valve notify the distributor Check and adjust the zero setting on the The valve s zero setting has been pressure control valve see the section modified Configuration of the V4 0 Servo Digital Unit in the manual Release the inlet line to the separator and see whether the pressure decreases Clean A blockage has formed on the liquid the inlet and outlet lines and the condenser gas separator inlet and or outlet lines tank with ethanol compressed air Otherwise continue by assessing the next possible cause l l Release each one of the sections of pipe GEN Ais a paco tele the and see whether the pressure falls Clean and or replace the blocked section Check the symptom No gases are entering No gases are entering the system ihe eainnt No rise in pressure in the system takn me reacionsysem Perform a leak test on the equipment See Leak in the reaction system the section Performing catalytic t
21. 05 FS C 0 1 bar typical N 0 0190 bar typical H4 tested lt 2 x 10 mbar l s He max error at 90 off horizontal 0 2 at 1 bar typical Na 30 min for optimum accuracy 2 min for accuracy 2 FS 57 PID Enga Tech LP TION 4 5 and or 6 MASS FLOW CONTROLLERS WITH POWER SUPPLY AND VALVES EIN E Fin e E 202 HOT BOX PT 1B0 c Vid 98 PID Enga Tech Internal seals for mass flow controllers are chosen depending on the used substance Next list shows recommended seals Density Conversion Recommended seals Symbol g l 02C factor iam 202C latm Plunger Capillary 1 Acetylene Ethyne on 1172 061 E E E E ww 1293 1 Ivv Iv 3 Allene Propadiene C3H4 1832 043 V V V 4 Ammoia NH3 0763 07 E E E 5S Agn ar 1784 14 vV V vo 6 Asne JL AH 394 066 V P v 7 Borontrichloride BCLS 5227 044 P P P 8 Boron trifluoride Im 3044 054 P P P 9 Bromine pentaflurine pp 780 026 P P P 10 Butadiene 13 Ion 2500 031 v v v 11 Butane Lomp 2705 025 v V V 12 Butne 1 Long 258 029 v v v 13 Butene 2 ci Long 250 032 v v v 14 Butene 2 trans Long 250 03 v v v 15 Carbonylfluoride COF2 298 054 v P V 16 Carbonylsulfide cos
22. 4 7 8 OPTION Q Heated head pump vessel and line for liquids 79 4 7 9 OPTION S Extra liquid evaporator with temperature control 82 4 7 10 OPTION T Temperature control in L G separator 84 4 8 OTHER COMPONENTS OF THE MICROACTIVITY REFERENCE 87 Ad PIFIN G ERROR RETI 87 4 8 2 JOINTS AND VALVES ooooccccccccoccnnccccocccnnnnononnnnnononnnnnnnonnnnnnnnnononnnnnnnnnnanos 87 4 8 8 INSGSIRUMENTATION 89 4 9 PROCESS CONTROL AND AUTOMATION ssn naannnnnnannnnnannnnnsnnnnnnnsnnrnressnnrreonnrrrrsnnne 91 4 9 1 CONTROL LOOPS IN THE MICROACTIVITY REFERENCE 91 492 AUTOMATION Mr 91 4 9 3 SYSTEM SAFETY MANAGEMENT 92 PROCESSQ CONTROL SOFTWARE 95 5 INTRODUCTION Tr 95 Se INSTAEBEATION rana 95 5 2 1 HOW TO INSTALL PROCEGGn 95 5 2 2 HOW TO INSTALL A PROJECT OR MICROACTIVITY CONFIGURATION 5 2 3 HOW TO LINK THE PC AND MICROACTIVITY REFERENCE 99 5 3 DATA ACQUISITION sra aaa 101 99 THE MENU 102 5 9 2 THE CONTROL PANEL cursan aa 104 Enga Tech 5 9 9 THE CONTROL GRAPHS creta ri 111 5 3 4 THE SESSION S TABLE eeeceeeessieeseeeeeeeen nennen nennen nnn rns 114 5 3 4 1 How to configure a session s table cc ceeeceeeeeeeeeeeeeeeeeeeeeaeees 114 5 3 4 2 How to Save a session s table ooooccccoconcccccccnnncccnncnnnccnncnnnnnncnnnnns 117 5 3 4 3 How to open a saved Se
23. 532 Data table 128 MICROACTIVITY REFERENCE User Manual PID 3 Figure 5 53 Data filtering by parameter The data can also be filtered by time On the left side of the table the time of the experiment is shown In the example of figure 5 53 the data is acquired every five seconds although this time depends on the value introduced in the sample time window Acquisition Sample time of the main menu see figure 5 15 To select a certain period of time click on the windows nitial time and Final time A list showing the times when each data acquisition has been done will dropdown Choose a range of time and click on Filter Day 10 08 15 oo 00 9970 Figure 5 54 Data filtering by time 129 MICROACTIVITY REFERENCE User Manual PID 3 Eng amp Tech 5 5 6 Errors report If an error has occurred during the experiment it will be registered in the experiment file The last window of the Experiment Viewer allows for viewing all the error messages if any Figure 5 54 Errors window 5 5 7 How to export the data to an Excel file x The icon Export Excel amp allows saving the data table in Excel x s format By clicking on the icon Export Excel choosing the path for saving the file is allowed Choose or Enter Path of File Save in a My Documents EI ct E3 My Recent Documents Desktop My Documents My Computer File name zl Save as type Excel Files xls
24. A Uu Hu Uu LA LAA US V ALAR 8 9 10 Figure 4 8 The buttons can be in two different states o Green background Activated o Grey background Deactivated 1 Control of gas inlet streams The screen depicts each one of the mass flow controllers integrated within the system showing o Set point yellow background set by the user Pressing on the value calls up a numerical keyboard for entering the desired set point which is stored in the system by pressing the Enter key o Current process value on the lower part This cannot be modified by the user 2 HEAT Heating of the system s gas outlet line It is possible to incorporate a thermocouple in this line opt checking the line temperature on the touch screen over the button If the unit does not incorporate this option this temperature reading appears as a line of points The configuration of this control loop can be set in the screen MISC SETUP in the main menu of the touch screen 31 PID Enga Tech Read out of the gas flow at the reactor outlet provided by a mass flow meter MFM situated on the gas outlet line if this set up option has been installed This value can not be modified manually by the user S1 Additional control options for special configurations of the unit S2 Actuator for an additional loop control opt Both sensor and final control element heaters have to be connected to the AUX 2 connector of the unit lts P I D
25. C on the hot box s temperature controller which it starts operating SET 2 menu on the controller esmero etario The hot box s temperature controller has Set the control mode to automatic Run on been set to manual at 0 the controller s _nd parameter Gees nob operat An alarm has been triggered in the Check the alarm and reset it providing the system that has shutdown the heating on situation that triggered it has been the hot box resolved The forward blades on the turbine are With the equipment disconnected remove rubbing against the ceramic cable the front cover on the turbine inside the hot The turbine does not operate housing or the heating cartridges box it clips off and remove the cabling correctly it does not turn properly Disconnect the equipment switch the circuit or it makes an odd noise breaker to OFF unscrew the left hand side panel or the upper one if necessary and adjust the motor s cooling blades Restore the optimum control parameters for this controller see the section The controllers in this manual The hot box s temperature An alarm has been triggered in the Check the alarm and reset it providing the controller is not working properly system that has impeded the heating of situation that triggered it has been the hot box door open on the hot box resolved Control mode has been set to manual Set the controllers nd parameter to or Rdy instead of to automatic a
26. CHA e i VMO2 CV02 MAM 0 mU BYPASS VALVE o 3 5 PORT 2 POS MFCO3 FE A HUA 345 3 je al CHA VO CVD3 MFC 4 PEA K VMD4 cwo MFCOS Pepo GAS OUTLET p 05 4 VE apre Se opa p VIMUS evos MFCOS Fc E osa Viol cv a QEPHONAL sss eel Lig OUTLET 86 PID Enga Tech 4 8 OTHER COMPONENTS OF THE MICROACTIVITY REFERENCE UNIT Connecting pieces valves instrumentation and other system components have been carefully selected There follows a description of the more important ones or those items that have undergone some form of modification in order to improve the system s performance 4 8 1 PIPING The selection of piping has taken several factors into account such as temperature pressure and type of compounds that are going to flow through it The most widely used material is 316L stainless steel with the maximum operating temperature for the pipe being that determined on the basis of the values for external diameter and thickness using the ASME table for 316L stainless steel pipes for different temperatures For 316 type stainless steel without welding and at 316 C the maximum stress value permitted is 17000 psi The geometry factor for a 1 8 pipe with a wall thickness of 0 02 is 0 367 By applying the expression Maximum operating pressure Maximum stress permitted x Geometry factor A maximum operating pressure is obtained of 6239 psi 430 bar for 1 8 pipes made of 316 stainless steel with a th
27. CURRENT LIMIT 6 S7 TERMINAL RESISTOR 00000500000000 eee TURNS SETTING ALARM RELAY Servo Digital V4 0 unit for the positioning of the micrometric valve for pressure regulation In those units that include the level control system for liquids in the condenser their corresponding Servo Digital unit is to be found to the right of this system Figure 4 28 e Zero calibration S1 The valve s zero setting or the point at which it is fully closed is factory set but frequent and constant use of the equipment may alter that point as a result of minor distortion of the PEEK disc that contains the valve orifice This effect is verified as follows Set the pressure and level controllers to manual mode and fully close the valve 096 Bring the system up to operating pressure Submerge the system s gas outlet into a water filled container and check that there is no bubbling If gas is observed to be escaping the values of the valve s zero point will have to be lowered more closed 90 PID EngaTech To adjust the valve s zero setting set switch Z on the dip switch to On S1 zero see Figure 4 29 The motor is now free for manual positioning by means of the corresponding TOHO controller in manual mode acting on the of control output or by pressing the microswitches Open or Close the valve s new zero setting point at which the system s gas outlet ceases to bubble If the bu
28. PUMP Press Menu and Pump The sequence of parameters is 43 PID Enga Tech Refill time lt is the time required for the piston return stroke Normally it is set at the lowest value 125 ms If cavitation from degassing occurs then a higher value must be used The minimum value is 125 ms and the maximum value is 1000 ms The maximum flow rate depends on the refill time If the refill time is too long a message Invalid settings flashes when you run the program The refill time or flow rate must be lowered Pump Compressibility This data is used to calculate the flow rate compensation for the compressibility of the solvent The minimum value is O and the maximum is 2000 Mbar The default value is 46 compressibility value for the water Compressibility values for the common solvents at atmospheric pressure are listed Xo Mbar 1 Carbon Dioxide 11580 Methanol Acetonitrile Pump Head Size This parameter is the size of the pump head Possible values are 5 10 25 50 100 and 200 It is possible to use any head size with the Gilson 307 pump However to ensure accuracy reproducibility and efficient pulse dampening the flow rate should not exceed 5 ml min Inlet pressure This is the pressure at the inlet of the pump head This allows the accurate pumping of liquefied gas It must be set to the same as the pressure of the aspirated liquid that is the saturating vapour pressure at the ambient temper
29. Purnp Head Model SC ops i Flow Rate Range Pressure Range mL min oe mer 0 050 10 Town 4050 10 14 5 8700 ATID Analytical Mixer 10 10 mL min 1 5 mL 11042204 amp 11D Titanium Analytical Mixer 140 10 mL min 1 5 mL 11042204 amp 11D Titanium Analytical Mixer 0 1 3 0 mL min 0 7 mL 110 220V amp 11D Microbore Mixer 0 1 mL min 5 pl 11042204 Constant flow rate Flow constant volume Dispense and time based sequence Program Head number 5 or 10 Liquid compressibility 2000 Mar Refill time 125 1000 ms Inlet pressure 0 10 MPa Timed events for programming four output contact closures and one input to wait far injection Time adjustable from 10 10 min with increments from 041 1 min depending on the range used Flow control adjustable in ml Armin from 0 0196 100 of the maximum flow rate of the pump head being used pito 969 loops with unlimited linking of files Storage for 10 user programs and four emor fles with a maximum of 25 points and timed events in each program Flow rate 10 pL min 10 mL min Coefficient of variation 0 1 40 6 with aqueous solutions or hydro organic polar solvent mixtures 0 336 96 with hydrocarbons ar chlorinated volatile solvents Maximum accuracy error x 196 with water over the full flow rate and pressure ranges 01 60 MPa 500 bar 8700 psi depending on pump head used Accuracy x 19b ar 0 1 MPa 1 bar 15 psi Repeatability lt 1 050 1 MPa 1 bar 15 psi Pulsati
30. Regulator that generates an outlet pressure of 34 35 bar 46 PID Enga Tech 4 6 2 PRESSURE CONTROL 4 6 2 1 Introduction to pressure control systems in microactivity reactors The use of a reactor such as the Microactivity Reference for catalytic microactivity studies involves the use of extremely low flow streams and usually high pressures This implies extremely low values for the flow or stream coefficient Cv that characterises the regulating valve of around 10 to 10 with this coefficient being defined as the flow of water in US gallons per minute that passes through a valve in a fully open position and with a loss of load of 1 psi To ensure high accuracy in the pressure control of the system in the Microactivity Reference unit as well as a non pulsatile gas flow inside the reactor there exists several different alternatives that are used commercially in systems such as the following Tescom type backpressure Control is only proportional which means it is affected by an offset error These systems are not suitable for microflow systems and they present high dead volumes They generate a pulsatile gas flow through the reactor Electronic back pressure with MFC type valve Despite providing an extraordinarily stable gas flow in the system s pressure control its main drawback appears when the system contains products in the vapour phase in the shape of microdroplets that may accumulate on the control valve s orifice
31. Remote control interface Ethernet EN 61326 1997 Ambient temperature range for operating 5 40 C Ambient temperature range for storing 20 70 C Recommended humidity range 5 80 raro Forced ventilation or convective H ventilation Dimensions cm Height x Width x Depth 70 x 60 x 55 Basic Unit 2 3 OPERATING CONDITIONS The optimum operating conditions for the Microactivity Reference Unit are as follows Pressure Atmospheric 100 bar if the high pressure option is included Temperature Ambient 700 C Feed Liquids and gases Flow of reactants 0 01 100 VPH volume of load per unit of catalyst and per hour for liquids and 10 100 000 for gases e Solid catalyst spheres pellets extruded items etc 2 4 EQUIPMENT APPEARANCE The Microactivity Reference consists of see Figure 2 2 e An integrated unit whose interior houses the hot box and the reaction system as well as all the system s control elements and valves e A Gilson HPLC pump optional for feeding liquids into the reactor e APOC with a remote control system involving communications via Ethernet At the outlet for reaction gases the user may incorporate an in line gas analysis system which will permit accurate monitoring of the reaction PID Enga Tech 2 4 1 GENERAL VIEW HPLC liquid pump optional Control PC Microactivity Reference unit ESPA prepn Figure 2 2 2 4 2 FRONT VIEW MICROACTIUITY Reference Hot
32. THUMEN TATION A CONT TROU E THERIUDCLDCIPLE KEE TEMPERATURE CONTRCE PRESSURE COMTROL Ee SS E Sl niy DATE DESCRIP THO D CHD APPD THEE DRAAD E TOTAL REPROTUC TIGN OF DR Ex Cem es gtt CH his ons OR ATOR FEDM RESPONSE EES Se 7 AS Se p Figure 2 1 IO PID Enga Tech After passing through a line shut off valve the reactant gas streams are fed into the reactor by means of a system of mass flow controllers that provide a known and controlled flow of gases In order to stop the products flowing back through the lines the controllers are protected with check valves fitted with Kalretz elastomer seals elastomeric Teflon When operation involves liquids these are dosed by means of a HPLC alternative positive displacement pump made by GILSON in streams ranging between 0 01 and 5 ml min and pressures of up to 600 bar The liquids are introduced into the system through a low dead volume check valve Liquid and gaseous flows are introduced into the hot box system that includes an electric forced convection heater that allows the process route to be kept at temperatures of 160 C and even 180 C to avoid possible condensation in the system The liquids evaporator is under the heater s forced flow at temperatures of around 15 to 20 C above the rest of the hot box and the pre heater for the gases is also under the direct flow of the heater at temperatures of 10 to 15 C above the rest of the system Once the gase
33. alarm gas detectors etc has to be made with the yellow and green wires The contact is normally open The two wires have to be connected to a relay that is normally open and closes when the alarm activates The actions that the unit makes when an external alarm appears are the following Reactor Furnace OFF Hot box Heaters OFF Inhibition Session ON Buzzer ON The actions of the external alarm on the MFC and the liquids pump are the same ones as configured by the user on the touch screen for the external alarm When the external alarm disappears the unit returns to the operation conditions 5 7 2 CONNECTION TO A GAS CHROMATOGRAPH The connection to the chromatograph is to be made with the brown and white cables The MA Ref unit has to be connected to the Remote Control connector of the GC The contact is normally open closing itself for 1 second when a pulse is sent to the chromatograph Operation lt is possible to activate a cycle to actuate upon a gas chromatograph in the Sessions Setting Panel of Process software This cycle actuates the closing of the electrical circuit that connects with the GC for a duration of 1 second The user can configure the cycle time period between 2 closings in the parameter XTO Figure 5 28 Visualization In this process screen the device for checking the status of the chromatography cycle is configured Figure 5 28 132 PID Enga Tech 6 PERFORMING CATALYTIC TESTS 6 1
34. allows giving different names to the experiment opened Rename Project Select a new name Far the experiment Mame EXPERIMENT 1 s el CARCEL Figure 5 47 Rename an experiment 5 5 3 How to resize a graph The zoom bar allows modifying the appearance of the graphs and also knowing the exact value of a variable through to the tool CURSOR Me a Figure 5 48 Zoom bar The different options are described bellow lt ACTIVE ZOOM The first icon allows zooming between two time values To do this click on the icon and drag the cursor between them Ze ZOOM IN d By clicking on ZOOM IN the graphs will be enlarged by hiding the first and the last five minutes on the scale wu ZOOM OUT This is used to increase the time seen on the X axis The time scale will add 10 minutes every time this function is clicked ES ZOOM TO FIT 125 MICROACTIVITY REFERENCE User Manual PID 3 This function allows for returning to the graphs initial configuration The time scale can also be modified by right clicking with the mouse on the graph background or on the X axis It is possible to choose between hours and minutes Graph Time Siwe dz PS Figure 5 49 Time scale setting Besides the scroll bar makes it possible to move forward or backwards on the graphs CURSOR The cursor tool shows the exact value of a variable at a certain time When clicking on the icon and moving the m
35. also be known As has been noted on several occasions pilot plant operation involves the scanning of different conditions around the operating variables Given that this is the case it is bad practice to select a value of P similar to that of Pc given that a modification in the set point or a modification involving another operating variable may suddenly change the system s gain and destabilise it if the value of P remains below the value of Pc Accordingly as with what is recommended in other empirical methods an appropriate value for P in these systems may be P 1 6 Pc Concerning the appropriate value of I the procedure in which this control action operates may be understood as follows the control algorithm assesses the area comprised between the variable s oscillation curve and the straight line delimited by the set point Accordingly if the time in which the totalling of this area coincides with the period of oscillation its positive part is cancelled out by the negative and the result for the action that is Superimposed onto the proportional action is zero If this operation is performed in a short period of time the result will not reflect the true situation and the resulting control action will destabilise the control system On the other hand if this assessment is performed over the course of two or three cycles the result will continue to be zero with the eventuality that too long will have been spent waiting to under
36. an experiment choose the folder containing it The name of this folder must appear in the upper cell next to Look in To accept click on Current folder Select Project or Experiment Base Path Look in MA REFERENCE Ich ES Data O Graphs My Recent Panel Documents sessions Devices Config dat en Plant Cfg cfg L My Network File name e Places Files of type an Files Y Cancel Current Folder Figure 5 44 The name of the project must appear on the upper cell 123 MICROACTIVITY REFERENCE User Manual PID 3 A new window showing all the experiments contained in the Data folder pops up Select the one and accept Experiment Selection pm E 20080114165204 20060122150046 i Figure 5 45 Experiment selection y Click on the icon in order to delete the highlighted experiments The graphs of the selected experiment will appear automatically Next to the graph on the right side a key with the variable s colors is displayed 20080325081530 File Zoom Tools EEEREBBE lu jin A een Ke MG PATRIOT TEO RRA D omm pre Ms H ome Lee ES Figure 5 46 Experiment s graph 124 PID Enga Tech The time scale shows the time of the experiment It can be changed by right clicking on the background of the graphs or in the X axis 5 5 2 How to rename an experiment The option Rename Experiment inside the File menu
37. and halts the operation of the MFC that the user has selected on the alarm set up panel on the system s touch screen It also shuts down the operation of the HPLC pump setting off an audible alarm as a warning signal for the operator and triggers the safety system s INH inhibition function impeding the software from changing the session automatically gt Operation of the hot box The hot box is fitted with a forced convection heater that consists of a turbine and a heater Its proper operation requires the turbine to be running when the heater is on dissipating the heat and avoiding damage This involves two systems working in parallel provided that the controller sends a control signal higher than 5 mA to the zero passage solid state relay that regulates the heater s power the turbine starts operating and even when this signal is not given whenever the temperature in the hot box exceeds 40 C the turbine will be running The hot box controller s upper limit absolute temperature alarm _E1H is set at 40 C Accordingly as the temperature drops the turbine cools the hot heating cartridges Door closed detector on hot box So as to disconnect the current supplied to the hot box heater when its door is open there is an inductive sensor that detects whether it is open or closed This function does not interrupt the operation of the turbine or act upon any other part of the system 5 Oven closed detector So as to disconnect the
38. current supplied to the hot box heater and the reactor oven when the latter is open there is a magnetic detector on the oven s closing device that detects the position of the reactor s moving section The detection of an open oven interrupts the operation of the hot box heater the supply of power to the oven and triggers the safety system s INH inhibition function impeding the software from changing the session If it becomes necessary to open the hot box door during a reaction procedure this is to be done manually without using the door opening button Manual opening of the door will only interrupt the power supply to the box heater 92 PID Enga Tech gt Flow alarm This alarm is by percentage deviation over the set point If for more than 10 s or time set in the Time Delay Alarm the set flow deviates by more than 10 from its value percentage set on the MFC set up panel on the touch screen the system interrupts the operation of the reactor oven sets off an audible alarm buzzer to alert the operator and triggers the safety system s INH inhibition function impeding changes in the operating session gt Pressure alarm Absolute alarm configured by parameter _E1H on the pressure controller It acts upon the liquids pump and the MFC halting the operation of those the user has selected on the pressure alarm set up panel on the system s touch screen lt is self locking in order to avoid a repetitive cycle of the system in
39. determines the position of the level control valve located in the base of the separator The controllers used are made by the firm TOHO model TTM 005 catering for RS 485 digital communications and are shown in Figure 4 5 Output 1 2 Process value Alarm leds 1 and 2 Set point control output 96 Cursor displacement by the digits in each function Digital signals Decrease button DELI TOHO Access level selector Increase button Figure 4 5 The process value of the controlled variable is displayed in the upper window on the controller green whereas the set point or the control output depending on whether operation is in automatic or manual mode is displayed in the lower window red This set point may be changed by pressing the Func key which allows for selecting each one of the different digits and subsequently changing the value of each digit using the Aand Y keys The Mode button is used to access the different control parameters configured in the controller Process value P Proportional band _ E Integral action s _ d Derivative action s nd Control mode Select with the A and Y keys 20 PID Enga Tech o Run Automatic mode The user is to set the desired value or set point of the variable controlled on the lower screen of the controller which will automatically act on the variable s control output o bd Control start at a given moment When this mode is acti
40. flexibility of a programming language combined with built in tools designed specifically for testing measurement and control Therefore Process software includes all the advantages of LabVIEW Easy to use graphical development environment Tight integration with a wide range of measurement hardware Rapid user interface development for displaying live data Extensive signal processing analysis and math functionality Multiple communication options TCP IP UDP serial and more Support for Windows Vista XP 2000 Cccoo0o00 5 2 INSTALLATION The PC supplied with the unit is provided with 1 Process software 2 A custom made PROJECT or Microactivity configuration This project includes the specific devices each Microactivity is equipped with controllers pump MFC s etc and its flow diagram For each unit there will only be one PROJECT although the user as will be seen later will be able to save it with different names if needed For this reason the software installation is performed in two steps first install the Process and then the Microactivity configuration or project 5 2 1 HOW TO INSTALL PROCESSO The installation of Process involves the following steps When the Process CD is introduced in the computer the installation software automatically opens It is recommended to close all running programs before beginning the installation 95 PID Enga Tech Process Welcome to Process Installer It is
41. folder the following files can be found 120 23007 LOL LZOGOZ b Lacuna de hecho 561 KB 20054050 IA 000003 bt Docus de banshee 843 KB 200047050 1 2006007 0000005 dt no vie aba aznb KB ZG 1720607 DOO Ic ocurrio de deco 853 KB 20097001 1706007 00012 Documento de teha B52 KB 2000706114060 _00015 04 ocio ae aba Bz3 KB 2009700140607 ORB OE Caco ides icona B47 KB 200741001 20907 Og T Fe OO vie cone 622 KB P Graph 2007 1 091 LAO 00001 Ft Documento de texto DER 23007 1051 LAO O0004 Ext Documento de be to 0379 KB 23007 1091 LAOS 00007 txt Documento de texto Ba ER 2004 10391 LA 00010 txt Documento de texto DER SUV LOL LAUS _00013 txt Docamenka de texto H3l ER 20071081 LAOS 00016 Ext Documento de bexto 2004 1 091 LA060 7 00019 txt Documento de texto DG ER Mamilia b Documenta de texto 25303 ma rm rm p pi emp ne SEP LOG LAO hil Firefox Document 5 KB 20071031 1705 07 MS Ee Documenta de bepobo abz KB 2007103112007 QNS Ext Documento de tenait Bbz KB 2007103117087 UB et Documenta de itengia 329 KB 2007103112007 0001 1 Evi Documenta de tenait a4z KB 2007103112709 7 00014 bd Documenta de benda 560 KB 200710311 70807 00017 fe Documento besaba B3 KB 2007103112007 INKL EE Documenta de iere 531 KB PID EngaTech Figure 5 40 Experiment file In the image above an example from the experiment folder content is shown there are
42. following the actions specified in the chapter 8 Maintenance of the equipment for the disposal of toxic or dangerous wastes and attending to the environmental policy in force in the laboratory or company where the equipment is working If the user wishes to get rid off of the unit he must hand it in to an authorized manager or ship it to Process Integral Development Eng amp tech where it will receive the proper treatment 141 PID Enga Tech 10 REACTOR TROUBLESHOOTING SYMPTOM POSSIBLE CAUSES SOLUTION The switch on the front is in the off n main circuit breaker on the rear is Switch the man circuit breaker to ONE The equipment does not switch on The power supply to the equipment has Verify the correct connection of the power not been properly connected supply that is on the rear of the equipment Open the right hand side of the equipment The system s fuse has blown and replace the fuse on the board contact the distributor Check that the Ethernet connection is working properly and verify the system s IP address MISC Menu on the touch The Ethernet connection has not been properly installed wrong network cable eden taba EL screen Verify the configuration of the PC s local area network Reboot both systems There is no communication M between the reactor and the touch Blocking of the microprocessor Ge DESEN GROSS persists please contact the distributor Check the gas installation and
43. heater must be plugged to the AUX2 connector on the rear panel of the unit The operation with this device is the same as it has been described in the previous section HEATER Press the Exit key to return to the main menu COMMUNICATIONS SETUP Set up parameters for the communications via Ethernet between the devices By default the unit is configured with the appropriate parameters to connect it directly with the control PC with a crossed serial cable IP ADDRESS 192 168 0 5 IP MASK 255 255 255 0 GATEWAY 192 168 0 1 TCP PORT 1234 38 PID Enga Tech ZoMMUN IZAT INS SETUP IP ADDRESS IP MASK GATEWAY TCP PORT Figure 4 19 Press the Exit key to return to the main menu PELTIER CONTROL Selection of the Peltier mode COOL For reducing the L G separator temperature Minimum about 1 C HEAT For increasing the L G separator temperature Maximum about 60 C This mode is the recommended for working with high viscosity hydrocarbons in order to avoid plugs in the liquid lines O O Peltier Control 9o This parameter is directly proportional to the cooling heating power supplied to the L G separator values between 0 and 100 96 Duty time s Time of the cooling heating cycle typically 10 seconds el 29 M 9 e AS A A IM PELTIER MODE PELTIER CONFIG PEC TIER CONTROL DUTY TIME Figure 4 20 ADMIN SETUP Screen for the system configuration by a PID Eng amp Tech ad
44. is moved an asterisk appears on the upper bar of the panel and the message bar on the bottom of the control panel turns to light red indicating that a change has been made and needs to be changed See Figure 5 18 105 PANEL Edition Mode Figure 5 18 In the menu screen displayed after right clicking on the mouse any changes made on the panel Save Panel can be saved It also allows to exit the Edit Mode Finish Edit Mode By right clicking over one of the devices a menu will appear with the following options Config By clicking on Config a submenu which allows for the possibility to modify values or to configure the device is accessed controller parameters turn on or turn off devices etc The device will turn green after the value has been changed The new value is automatically sent to the Microactivity Reference unit To see the device s parameters names process value set value output control by choosing Show Hide Parameters Rename the device If the Edit Mode while the equipment is acquiring data is activated the variable values will not be actualized any longer and the values from the last reading in normal mode are kept These values will not change until exiting the Edit Mode and press START acquiring again It is possible to see the current value of a variable even when Process is not acquiring data to do so double click on the red bar of a device s icon The icon will turn green and the val
45. mode Editor Normal The Edit mode allows for modifying the panel moving the icons that represent the different devices Rename and Show Hide Parameter Labels In normal mode all these editing options are disabled Message bar Figure 5 16 Project panel 104 PID Enga Tech NORMAL MODE In normal mode data acquisition and visualization in real time is possible When data acquisition starts the red bar situated on the upper part of the icons that represent each device turns from red to green The design of each device in normal mode is allowed by right clicking on a device To go to Edit Mode right click on the screen and choose Edit Mode EDIT MODE In Edit Mode the message bar is shown in yellow and displays a message indicating that it is in Edit Mode The Edit Mode is also indicated in the panel s upper section next to the name PANEL Edition Mode Figure 5 17 Control panel in Edit Mode When the program is in Edit Mode the acquisition of data stops Each device will show the last read value To refresh a value in Edit Mode click twice on the bar situated on the top of each icon The acquisition of data is disabled until the program is returned to the Normal Mode This mode allows for moving the device s icons To do so place the mouse on top of an icon and drag it while left clicking The names move together with the icons as they are dragged Also the name of the icon can be moved around the icons When an icon
46. the device s screen displays the pressure value below which the system s pressure alarm will be shut off once the situation that triggered the alarm has been resolved 29 PID EngaTech ERROR MESSAGES Message Cause Corrective action Lt Current surge due to a short circuit Reboot the device 8 3 Pressure is being applied to the device Carry out the adjustment of the zero during the adjustment of the zero setting setting at atmospheric pressure The pressure applied exceeds the upper limit o of the pressure range that can be shown The pressure applied must be within gt the range that can be shown on the The pressure applied exceeds the lower limit screen of the pressure range that can be shown Table 4 4 For more information on the different operating modes as well as the different possible configurations for the device consult the manual for the series DP2 pressure sensor 30 PID Enga Tech 4 5 THE TOUCH SCREEN The Microactivity Reference unit has a touch screen which allows for adjusting the various process parameters it displays the following o A main screen which shows a P amp I diagram of the process o Different set up screens which are accessed from the main menu 4 5 1 MAIN SCREEN FUNCTIONS The main screen presents the process flow and has the appearance shown in Figure 4 8 Pressing on the different icons and buttons grants access to the different functions Aalt Macs A A A A
47. the event that its activity ceases even when the problem that triggered it has not been resolved For example in the event of a blockage in the porous plate pressure will increase and the alarm will act upon the feed to the system halting it But this will bring the pressure below the alarm value whereby the system will again start operating in a situation that will again produce the circumstances that will once again trigger the alarm This is why once the pressure alarm has been triggered the system will remain in stand by until the operator proceeds manually to release this locking an action that is to be performed after checking over the system and correcting the anomalous situation The safety system locks this situation until the system operator presses RESET on the pressure alarm once the source of the problem has been located The MFC will not operate until this RESET is pressed even though the pressure value in the system has dropped below the value _E1H Level alarm Alarm configured by the parameter _E1H on the level controller It is absolute type and it acts upon the liquids pump and the MFC halting the operation of those the user has selected on the level alarm set up panel on the system s touch screen It also triggers the audible alarm and the INH inhibition function as the upper limit set has been exceeded This alarm is only available on equipment with liquid feed systems and a liquid gas separator with level control
48. the system and system in the separator if operating with close the level control valve See whether this option the pressure stabilises Perform a leak test on the equipment See Leak in the reaction system the section Performing catalytic tests in this manual Check and adjust the zero setting on the The valve s zero setting has been pressure control valve see the section modified Configuration of the Servo Digital V4 0 unit in the manual The pressure in the system does equipment equipment exceeds the operating pressure not reach the set point stabilising takn me reacionsysem Perform a leak test on the equipment See at a lower value Leak in the reaction system the section Performing catalytic tests in this manual 145 The pressure in the system rises uncontrollably without responding to the set point with the 3 port valve in the reaction position The reactor s porous plate is blocked The pressure in the system varies without stabilising at the set point The sensor s reading exceeds 2 ml or is above zero with the tank empty There is no reading from the level sensor in the separator with liquid in the condenser The sensor s reading exceeds 2 ml or is above zero with the tank empty The level reading in the sensor does not remain stable at the set point No liquids are evacuated from the system pressurised system in which the liquid level rises continuou
49. y D Figure 5 56 Exit window 130 PID Enga Tech 5 5 8 How to capture a graphs image The last menu of the menu bar TOOLS Get Snapshot o Crtl S allows obtaining a snapshot of the graphs and saving them in an image format 5 6 HOW TO EXIT PROCESS To exit Process click on the cross of the main menu Mo Project Project Adquisiti Do vou really want bo exit Pracessim Cancel Figure 5 57 Exit window A message asking Do you really want to exit Process will appear This operation is not immediate Process may need some time especially if the experiment has taken a long time This operation may take some time PLEASE WAIT UNTIL PROCESSI CLOSES AUTOMATICALLY Figure 5 58 5 7 CONNECTION TO A GAS CHROMATOGRAPH The Microactivity Reference unit is prepared for connecting to a gas chromatograph actuating the sampling injection valve to start the analysis Both devices external alarm and chromatograph will be connected to the Microactivity Reference using the wire External Control provided by PID Eng amp Tech with the unit Connector EXTERNAL CONTROL BINDER 680 female 6 pin PIN 5 Without cable PIN 6 Without cable o PIN 1 Chromatograph contact BROWN o PIN 2 Chromatograph contact WHITE o PIN 3 Emergency contact YELLOW o PIN 4 Emergency contact GREEN O O 131 PID Enga Tech 5 7 1 CONNECTION TO AN EXTERNAL ALARM The connection to an external
50. 02C P BAR 7902C 2 5 9 15 17 8 10 16 5 18 5 22 14 5 16 5 14 17 20 23 24 26 Table 2 Composition of metal alloys Source www alloywire com SS316 Table 3 Pressure temperature rating Source Autoclave Engineers 800 690 214 104 HAST C276 1093 418 364 155 BAL 18 4 7 3 4 5 6 10 5 max 3 2 4 2 BAL HAST X INCONEL 600 1200 1212 617 356 525 243 308 36 100 76 2 INCONEL 625 980 827 728 414 1 5 SS310 1100 441 262 241 PID Enga Tech PRESSURE vs TEMPERATURE RATING CURVES NT 600 Tx Inconel 625 80 N CH O o SS316 before 427 0 al o A o S316 after 427 C Hastelloy C276 Percentage of Rated Pressure Room Temperature Hastelloy X N o Pressure calculation example for SS316 Max P 690 bar CURVE SS316 Factor 96 at 500 C 31 Max P at 500 C 0 31 x 690 bar 214 bar 100 200 300 400 500 600 700 800 900 1000 Temperature in C Figure 4 49 PIDEng Tech can also install different types of synterized materials for the reactor 20 um porous plate SS316 Hastelloy C276 Hastelloy X Inconel 600 Inconel 625 and SS310 are available Also when coke formation is possible no porous plate is recommended Selection of the appropriate material for the reactor will be user s responsibility never responsibility of PIDEng8 Tech 17 PID EngaTech 4 7 7 OPTION K NO STANDARD FURNACE
51. 18 020 022 024 026 Gv Figure 4 27 The system that has been designed for operating the valve consists of a high resolution microstep motor These motors consist of electromagnets that are connected and disconnected alternately so that a rotor permanent magnet moves in small steps in the required direction By multiplying the number of coils on the motor or creating complex systems for the switching of the coils regulated by a microprocessor use can be made with stepping motors of 200 steps per turn in set ups with 51 200 steps in one rotation The motor s shaft is coupled to the micrometric valve and to a potentiometer allowing for the position of the valve with 1degree resolution to be read at any given moment The position s control system operates on a digital basis by successive approximation comparing the present position relayed by the potentiometer to that specified by the demand then calculating the number of positions that remain to be advanced and all within an infinite loop that constantly corrects the motor s position with the system s extremely rapid response time To improve the potentiometer s reading of the position a current generator and an instrumentation amplifier has been used eliminating errors and noise stemming from the cabling The pressure control valve is located downstream of the reactor once the reaction gases have passed through the separator condenser The following are the characteristics of the pres
52. ALACI N ESTO ES UN CONTRATO LEA DETENIDAMENTE ESTE CONTRATO ANTES DE BAJAR EL SOFTWARE Y O COMPLETAR EL PROCESO DE INSTALACI N DEL MISMO AL BAJAR EL SOFTWARE Y O PULSAR LA OPCI N CORRESPONDIENTE PARA COMPLETAR EL PROCESO DE INSTALACI N PRESTAR SU CONSENTIMIENTO A LOS T RMINOS DE ESTE CONTRATO Y QUEDAR VINCULADO POR EL MISMO SI NO DESEA CONVERTIRSE EN PARTE DE ESTE CONTRATO Y QUEDAR VINCULADO POR TODOS SUS T RMINOS Y CONDICIONES PULSE LA OPCI N CORRESPONDIENTE PARA CANCELAR EL PROCESO DE INSTALACI N NO INSTALE NI UTILICE EL SOFTWARE Y DEVU LVALO DENTRO DE LOS TREINTA 30 D AS SIGUIENTES A LA RECEPCI N DEL MISMO INCLUYENDO TODA LA LITERATURA ADJUNTA JUNTO CON SUS ENVOLTORIOS AL LUGAR DONDE LO ADQUIRI TODAS LAS DEVOLUCIONES ESTAR N SUJETAS A LAS NORMAS DE DEVOLUCI N DE NATIONAL INSTRUMENTS APLICABLES EN CADA MOMENTO O accept the License Agreement s do not accept the License Agreements Figure 5 3 National Instruments licence agreement In the next window agreement is asked for on two new requirements MS XML4 e IVI Both must be accepted in order to continue by pressing Next gt gt Y Processo License Agreement You must accept the license s displayed below to proceed MSXML4 M END USER LICENSE AGREEMENT FOR MICROSOFT SOFTWARE MICROSOFT XML CORE SERVICES MSXML 4 0 IMPORTANT READ CAREFULLY This Microsoft End User License Agreement EULA is a legal agreement between you ei
53. C and compares it to the order triggering an alarm signal if they do not coincide Use has been made of controllers made by the firm TOHO model TTM 005 for the control of temperature pressure and level 4 20 mA input and output These controllers cater for RS 485 digital communications for communicating with the computerised control system 4 9 2 AUTOMATION Before proceeding to the design of the printed circuit that contains the microprocessor that manages the system for the control and monitoring of the reactor and which is what will manage the Microactivity Reference reaction unit a simulation was made of each one of the systems operating in the microactivity reactor 91 PID Enga Tech 4 9 3 SYSTEM SAFETY MANAGEMENT gt Safety status in the event of a power failure As an initial safety measure the controllers use a non volatile memory to store the latest parameters introduced manually from the keyboard After a power failure the plant returns to these safety parameters or values irrespective of what the latest values were that were sent to the computer As a precaution the system s safety values have to be re entered after any manual modification of the set point in operations performed by the operator independently of the computerised control system gt Temperature alarm The controller s upper limit absolute temperature alarm shuts down the control signal on the reactor oven and on the hot box heater
54. D HUMIDITY RANGES eee 10 3 1 2 VENTILATION REQUIREMENTS sees 11 3 13 BENCHTOP SPACE REQUIREMENTS Ree 11 3 14 ELECTRICAL REQUIREMENTS HH 11 3141 GROUNDING 11 3 142 LINE VOLTAGE Cerne eee ee eee ee eee 11 945 GAS REQUIREMENTS isis 12 3 2 EQUIPMENT INSTALLATION astas tas 12 32 1 UNPACKING THE EQUIPMENT sarna 12 3 2 2 PLACING THE EQUIPMENT ON THE BENCHTOP ees 12 323 ELECTRICAL INSTALLATION sin 12 32A GAS INSTALLATION seta 16 329 TURNING TAE POWER ON sima 16 4 COMPONENTS OF THE MICROACTIVITY REFERENCE UNIT 17 4 1 THE REACTOR AND THE HOT BOS 18 de TAECONTROLLER t 20 42 1 THE REGULATION RARAMETERG senes 20 4 2 2 CONTROL STABILITY CRITERIA Enga Tech 4 2 3 CONTROLLERS TUNING occccccocccncccccccccnncccoccnoncccooncnnnnononncnnnnononnnannnnnnos 23 4 2 3 1 Ziegler amp Nichols Method 4 2 3 2 Method of trial and error 4 2 3 3 Method proposed by PID Eng amp Tech 4 3 THE LIQUID GAS SEPARATOR c ooccccccccocccnnoconcconocononcnononononncnnnnononnnnnnnononnnannnnanennnoss 28 4 4 THE PRESSURE SENSOR FOR ATMOSPHERIC PRESSURE REACTORS 29 45 THE LOUGH SOREEN since 31 4 5 1 MAIN SCREEN FUNCTIONS oocccccccccccccncccccocccnnconoconnnoccnancnnnnononnnnnnnnnnos 31 4S2 VARIN ITE CIE 33 45 9 OTHER FUNG HIEN geed Seeerei 41 4 6 SPECIAL CONFIGURATIONS OF THE MICROACTIVITY REFERENCE 42 4 6 1 THE GILSON 307 HPLC PU
55. E MF c OFF OF HERE LIQUID PUMP EREE Figure 4 13 gt PRESSURE ALARMS Set up menu for the pressure alarm 35 PID Enga Tech FREE PRERE DFF LIGUID PUMP Figure 4 14 As in the previous menu this screen allows the user to select the actions the system is to carry out in the event of a pressure alarm In this case it is advisable to close off all gas and liquid inlets to the system in order to reduce the pressure within it set them to OFP This alarm will remain locked and has to be reset manually on the alarm panel pressing the key Reset Alarm Press the Exit key to return to the main menu LEVEL ALARM only for old Microactivity units Set up menu for the level alarm In this screen the user can configure the unit in order to stop the liquids and the gasses when the alarm in the liquid gas separator goes off MEM RN M a NN AL n d FREE FREE PREE FREE EREE EEEE LIGUID PUMP EREE Figure 4 15 36 PID Enga Tech gt EXTERNAL ALARM Set up menu for external alarm In this screen the user can configure the unit in order to stop the liquids and the gasses when the alarm in the liquid gas separator goes off Fe TE Cd pe He IB AL AREMA FREE FREE FREE FREE FREE FREE Lieuip PUMP FREE Figure 4 16 LEVEL SETUP only for old Microactivity units Set up screen for the level sensor for equipment with this option The description of this s
56. ETA WEM Ss ono Malal UE abr a WEM eye 565605 II PRESSURE 1 E ESSERE LEVEL A E ple MASS FLOWS INHIBITIGH SESSION RESET BUZZER RESET ALARM Figure 4 9 o Temperature Reactor The reactor temperature exceeds the maximum limit specified in its controller 32 O O PID Enga Tech Temperature Hot Box The hot box temperature exceeds the maximum limit specified in its controller By default this limit is set at 40 C when this temperature is exceeded the forced convection is activated in the hot box Accordingly this alarm will normally be triggered although this does not mean that the system is operating out of control Pressure The pressure in the system exceeds the maximum limit specified in its controller Level only for old Microactivity units The level in the liquid gas separator exceeds the maximum limit specified in its controller Mass Flows Alarm for deviation of the flow of any one of the system s mass flow controllers regarding its set point consult the screen Mass Flow Set up Inhibition Session Whenever an alarm is triggered in the system an inhibition session will be activated interrupting the sequence of sessions programmed in the control software and so avoiding situations of risk in the system External External alarm additional to the reactor Open Heactor Detection of open oven Pressure Servo Alarm in the Digital Servo of the micrometric valve for pressure regulation in the syste
57. How to filter the experiment data When clicking on the window Data a table with all the values acquired during the experiment is displayed 127 PID Enga Tech VALUES DISPLAYED IN DATA TABLE MFn Set vale MVn Process Value PV1 Process Value Controller TOHO SV1 Set Value MV1 Control output On Off devices Door Bypass Peltier S1 S2 S3 mH dide cl ed F Flow M Status On Off XON Status On Off Chromatograph Cycle time M1C Control output Heat M10O Status On Off Table 5 7 Values of the parameters All these values can be filtered by name and time so that only a certain range of values is displayed in the table To do so select the desired parameters from the complete list shown in the right side window If two or more devices are to be selected click on them while pressing Ctrl on the keyboard and press y Filter A EA ELE EA Het EDI px a EI GESX MES prio E SL SE GE 0 HS pe Ges R DI 11504 0001 E EE 150 LEI fg SO 11001 nrc Am Jow Deg EE jos DER DEF uu 0 00 100 UCET fat Tr FF 000 10101 ICI sa C w e e e uo x m CCOO oer ser os i6 E T i 1 Der Der 0 00 TEXT ICI son ise ee AA uto mm Lem t E or Lag DEF E Die e d Ss SEH CET tf a A na E na A Ee ur I or EO A m SS en LN d E DEF OFF E na e na CEE nn E MS nao pwivazs o oet eer Ap OFF OFF DEF A ee I c Ea OFT OFT 100 00 3 70 Figure 5
58. INS em its rating cL LT c 4056 e II aw 8 RRE l ll 55 0 100 200 300 400 500 600 700 800 900 1000 1100 1200 38 93 149 204 260 316 371 427 482 538 593 649 Temperature in F C Figure 4 2 Depending on the user s requirements any other reactor size diameter or length or any other construction material Monel 400 Inconel 600 Titanium Grade 2 Nickel 200 Hastelloy C276 Titanium GALAV etc can be used As can be seen in Figure 4 3 the inside of the reactor has been fitted with a 10FRAHC porous plate made by the firm VALCO in Hastelloy C 276 with a pore size of 2 um This plate rests on a 316 stainless steel pipe inserted through the lower end of the reactor thereby allowing for 18 PID EngaTech Reduction to a minimum the dead volume at the outlet Replacing the plate whenever so required without the need to replace the reactor nipple Thermocouple Tubular reactor Porous plate Porous plate support Figure 4 4 The thermocouple type K encased in a 1 5 mm diameter Inconel sheath is inserted through the upper end and is in contact with the catalyst bed without thermowell This allows for reading reaction temperatures with response times in milliseconds The reactor is housed in an oven built without insulation consisting of a 304 stainless steel chassis the inside houses the resistance together with a refractory material 550 W 230 VAC Maximum opera
59. It allows choosing a Project or Microactivity configuration By default there is only one Project for a Microactivity However the user can save this project under different names as will be shown later on and access them at a later time This way for example if the Microactivity is going to be used to test different catalysts a different project can be saved for each catalyst so that the experiments made with each one are organized in different projects In this menu the Communication function can also be found This function allows for checking the connectivity between the PC and the Microactivity Reference To run this test introduce the Microactivity Reference s IP and click on Test If there is communication a Communication OK message will appear 102 PID Enga Tech Communication Config Ethernet C Serial IP Serial Port ise DC ERC WIER Port l 12 38 Figure 5 13 Communication test Q Acquisition When Acquisition is selected a new menu will appear Select Start or Stop or click on the PLAY or STOP icons that appear under the tools bar to plot a graph with the acquired data Project Panels Sessions Graphs Tools Sample Time Figure 5 14 Data acquisition From this menu the Sample Time can be set The Sample Time determines how often in seconds Process is to acquire data The minimum value is 5 seconds Once the new value is introduced click OK The size of the data files will de
60. Launch sessions Click on RUN in the sessions table to begin the first session To start from another session introduce the number of the session and click on Launch When the last session is finished Process will stop acquiring data 5 4 DATA PROCESSING When data acquisition is stopped by clicking on the STOP icon or the last session ends a data file is generated The name of this file is the same that appears on the left bottom corner of the session table see figure 5 36 The experiment data can be accessed in two different ways either through the experiment viewer see point 5 5 of this chapter or by accessing the data folder of each project as explained next To access the data saved on previous experiments go to the project s folder which can be found in the following directory C Program Files Process Plants In this directory find the Microactivity project s folder Find the experiment s results inside the Project s folder In this folder new subfolders are created with the experiments An experiment file is generated every time data acquisition is stopped The experiments are saved with the date in a universal format when they were performed YYYYMMDDhhmmss where YYYY Year when the experiment was performed MM Month DD Day hh The experiment s starting hour mm Minutes ss Seconds In this way the experiments are organized with the oldest experiments at the top Inside an experiment s
61. MP uk nennen nnn nnns 42 4 6 1 1 Frontal view ooccccoccncccccnccccnccnncncconnnonononononononannnonnnnnnnncnononenenanens 42 LN n Boa oo AM e E Eo A 42 4 6 1 3 Technical Gpecitcatons 43 4 6 1 4 Switching on the poump 43 4 6 1 5 Pump operaton 44 4 6 2 PRESSURE CONTRO isso 47 4 6 2 1 Introduction to pressure control systems in microactivity reactors 4 6 2 2 The micrometric vahye eese 47 4 6 2 3 Configuration of the Servo Digital V4 0 unit microstep positioner 4 6 3 LEVEL CONTROL IN THE LIQUID GAS SEPARATOR 53 4 6 3 1 Introduction to level control in microactivity reactors 53 4 6 3 2 The capacitive level sensor A 53 4 7 SPECIAL OPTIONS FOR THE MICROACTIVITY REFERENCE UNIT 56 4 7 1 OPTION A Each other mass flow controllers up to 6 56 4 7 2 OPTION B Scale with digital communications ssss 62 4 7 3 OPTION C Mass flow meter amp coalescing filter in gases outlet 66 4 7 4 OPTION D Additional 6 port valve ooonccnccccnnconccccnnncnnnnnnnanonnnnnnanons 69 4 7 5 OPTION D1 Additional 4 port manual valve seessssss 72 4 7 6 OPTION E TO J Different types sizes and materials for spare reactors with thermocouple and accessories ccccoocccnccnccnccnnncnonancnnncnnnanennnonanncnnnnos 75 4 7 7 OPTION K No standard furnace essere 78
62. O ISOLATE REACTOR 3l G x ala S SE al SC I I l FCU l l l IE r I EE l OD q o gt E MD2 Catz EA T Ce LIQ GUTLET A 74 PID Enga Tech 4 7 6 OPTIONS E TO J DIFFERENT TYPES SIZES AND MATERIALS FOR SPARE REACTORS WITH TERMOCOUPLE AND ACCESSORIES OPTION REACTOR E Quartz 88316 o 1 OA H JNoStandard SS316 Reactor 13 1 mm ID 1 J NoStandard Hastelloy C Reactor 13 1 mmID E o No Standard Hastelloy C Reactor 17 5 mm ID E o No Standard Inconel 625 Reactor 13 1 mm ID KE No Standard Inconel 625 Reactor 17 5 mm ID O J Hastelloy X Reactor 19 PID Enga Tech When choosing a reactor its composition is a critical factor since the presence of some elements may affect or catalyze reactions Also the reaction itself can attack reactor walls due to corrosion phenomena The working temperature and pressure are also a determinant factor For this reason depending on the application and operation conditions reactor materials other than standard SS316 can be recommended for some specific applications The three charts below summarize the characteristics of the different materials used in Microactivity reactors SS316 Hast X Hast C276 Inconel 600 Inconel 625 SS310 Inside x Outside Diam 9 1 x 14 3 13 1 x 19 1 17 5 x 25 4 10 5 13 5 47 55 72 58 min 19 22 MAX TEMPERATURE 2C MAX PRESSURE BAR P BAR 5002C P BAR 65
63. PID Enga Tech the set point and returning to its initial value The adjustment is gradually fine tuned by observing the control output signal and its response to the disturbance created not too severe so as to avoid damage in the process Begin by observing the system s behaviour in on off status A proportional action is then generated whereby the oscillations are suitably attenuated Begin with a wide proportional band small gain which is then gradually narrowed in line with the system s evolution until the required stability is attained damping ratio of 25 between two successive waves Once a suitable value of parameter P has been achieved compromise between stability and error offset the elimination of the offset will be achieved by means of the addition of an integral control action also by trial and error As integral action compromises control the proportional band is to be raised slightly lower gain and beginning with a high value for the integral action in seconds slowly decrease it whilst at the same time creating disturbances in the process by means of changes to the set point Once the proportional and integral action parameters have been tuned the derivative action is increased in small jumps from D 0 whilst at the same time creating disturbances in the process by means of changes to the set point until the process obtains its characteristic cyclic behaviour A suitable value for the derivative action should
64. RE Si v PUMP x v PUMP w RESTOR w GS Session 1 teirion tern jn CR E43 Th I Sesa E Sergio b Serge n pr ion Session g Session mm Cession Senna 2 Deihi d Seton 4 Sersion 5 Deponi tesdion 7 Session H Dessin s Sepan 10 SECURITY HEATING REACTION COCXOLIMG OPEMDOOR CLOSE DOOR Lu Tux ERI LO 1000 10 else se cjo oala se C mm m ou mouse Fsprrimrnl Nares ZG 5DBI S30 Figure 5 39b Experiment file An initial session corresponds to the secure shutdown of the system The second session takes the system to the operating conditions under which the experiment is to be performed e g heat the reactor up to operating temperature The duration of this session is to be sufficient to allow the system to attain stable operating conditions which may be carried out by setting long session times or else by using the condition evaluation function Subsequent sessions correspond to the operating conditions in which catalytic measurements are to be taken The final two sessions correspond to sessions involving the secure shutdown of the system with the last one being for example the same as the session programmed as no 1 In order to fasten the cooling of the system a session for opening the door when the temperature of the reactor is low enough lt 250 C can be configured 119 PID Enga Tech Q Configure the graphics colors scales etc Q
65. SSION S table ceeeeceeeeeeeeeee seen eeeeees 118 5 3 4 4 How iopntaseseioneiable cee ecceeeeseeeeeeeeeeeeeeeeeeaeeeeeeeeas 118 5 3 HOW TO CARRY OUT AN ESPRERHIMENT 119 o4 DATA PROCESSING EE 120 5 5 EXPERIMENT VIEWER 122 5 6 HOW TO EXIT PROCEGtoen nnnm nennen ness nsn nnn rrr nnne nnns 131 5 7 CONNECTION TO A GAS CHROMATOGRAPH esee 131 6 PERFORMING CATALYTIC TESTS 132 6 1 INTRODUCING THE CATALYTIC BED INTO THE REACTOR sssssssnsssssennnnnnnenennns 132 6 2 PROGRAMMING A SEQUENCE OF EXPERIMENTS esee 132 7 MAINTENANCE OF THE EQUIPMENT 133 7 1 WEEKLY MAINTENANCE ooooooccccccccnonnncccnnncoconononnnnncnnnnnnnnnnnnnnonronnnnnnnnnnnnnnnnnnnnnnnnnnns 133 TIA LEAK DETECTION siicticdecsiesarnnnatiscs antioad ace snuascsvsiimucaatetcsvaantsues Quntieucnatetes 133 7 1 2 CLEANING THE UNITA 133 7 2 MONTHLY QUARTERLY MAINTENANCE sees 133 214 REPLACING THE FILTERS sciraxsievcesebzsk tust auk iia e e rap incas 133 7 3 ANNUAL OR LATER MAINTENANCE sees 134 fal REPLACING THE E 134 7 3 2 REPLACING THE KALRETZ SEALS IN THE GAS MIXER 134 7 3 3 REPLACING THE REACTOR POROUS PLATE 134 7 3 8 REPLACING A MASS FLOW CONTROLLER ees 135 8 EUROPEAN DIRECTIVES 138 9 ENVIRONMENTAL POLICY 140 10 REACTOR TROUBLESHOOTING 141 PID EngaTech MICROACTIVITY REFERENCE USER MANUAL 1 INTRODUCTION The Microactivity Reference unit is an autom
66. These systems can not be heated given their electronic nature Control loop with control valve The problem of control in previous systems was resolved by configuring a control loop for pressure whereby the signal from a pressure transmitter is received by a PID controller that produces a control signal that is relayed to a control valve that acts upon the system s output current modulating the circulation flow and thus regulating the pressure The problem posed by this control system is the availability of commercial microvalves that are suitable for microflow systems basically consisting of a cylindrical orifice through which a round rod is inserted whose purpose is to vary the fluid s length of passage through the microvalve These systems feature very low rangeability of around 10 difference of flow that passes through the valve between the minimum and maximum aperture for a specific pressure whereby they are not suitable for a system such as the Microactivity Reference in which widely differing operating conditions are to be studied and whose regulating valve should have rangeabilities of around 160 4 6 2 2 The micrometric regulating valve The Microactivity Reference includes a micrometric regulating valve for pressure control in the reactor as well as for level control in the liquid gas separator in those systems that include this option of very high rangeability consisting of a needle whose displacement creates an increasingly t
67. Vv V V 56 Hydrogen LI 00891 101 V V V 57 Hydrogenbromide HBr 3646 098 P P P 58 Hydrogen chloride HCl 1639 09 V H V 59 Hydrogen cyanide DON 12060 075 P P P 60 Hydrogen fluoride H 08926 2096 P P P El f Hydrogen iodide W 5799 9o97 pp o eO 62 Hydrogenselenide Hose 3663 om 63 Hydrogen sulfide Tos Isobutane cama 268 os v v v 65 Isobutylene Isobutene C4H8 26 028 V V V 66 Krypton r 379 i148 v v V 67 Metanee c 07175 076 VW V V 68 Methylaetyene 1 C3H4 1831 043 V V V 9 Methylbromide Hasr ass IMS VA 70 Methylchloride CH3dl 2300 064 v V V 71 Methyfluoride CH3F 1594 07 VW P V 72 Methylmercaplan CH3SH 2146 053 P P P 73 Molybdenum hexafluoride MoF6 9366 021 P P P 74 Mono ethylamide C2H3NH2 2011 036 P P P 75 Monomethylamne CH3NH2 1419 052 P P P 76 Nen IL Ne 0902 141 VM V V 77 Nitricoide NO 134 097 V P V 79 Nitrogen dioxide NO2 2053 074 P P P 80 Nitrogen trifluoride NF3 3182 05 P P P 81 Nitrous oxide Noci 2984 061 P P P 84 Oxygen difluoride op 2417 064 P P P 86 Pentane LGn 3219 021 VW V V E7 Perchioryl
68. When using a no standard dimensions reactor a no standard furnace is required Standard furnace for standar 9 1 mm ID reactor Figure 4 50 No standard furnace Special furnace for for no standard 17 5 special customer mm ID reactor aplication FT 7 Figure 4 51 Figure 4 52 lL Se Standard furnace No standard furnace Max power consumption W 800W It depends on the application 78 4 7 8 OPTION Q HEATED HEAD PUMP VESSEL AND LINE FOR LIQUIDS This is a special option for pumping heavy hydrocarbons or high viscosity liquids HPLC head pump is heated to 70 C by means of a thermostatic switch while the line is heated by means of an autorregulating heating tape to 100 C This option is particularly suitable for liquids with high viscosity Figure 4 53 Element Power consumption Temperature C Heated Vesse 125 W Heated Head pump 125 W Heating tape 13 W m 79 PID Enga Tech Liquid pump heating system ABCD ABCD ABCD ABCD ABCD Figure 4 54 80 MICROACTIVITY RE FERENCE GAS 1 Kc Tasa lt gt GAS 6 lt OD VMO1 cvol MFCO2 uc LX bae gt VMO2 CV02 Pad gt VMO3 Cv03 MFCO4 Pax es s L2 As ail gt M04 CV04 MFCOS Fc cx D bok VMOS CV05 MFCO6 Ri Le CHA LA VM06 CV06 OPTIONAL User Manual 81 GAS OUTLET PID EngaTech 4 7 9 OPTION S EXTRA LIQUID EVAPORATOR WITH TEMPERATURE CONTROL W
69. able is connected If the unit and the PC are connected through a local network the cable must be straight not crossed 147
70. actor APPEARANCE OF THE DEVICE 1 Display It shows the value of the pressure measurement adjustments error messages and the keypad blocking status 2 Indicator that lights up when the operation of comparative action of output 1 has been activated 3 Indicator that lights up when the operation of comparative action of output 2 has been activated 4 Increase button 5 Decrease button 6 Key for selection of operating mode Figure 4 7 SPECIFICATIONS OF MODEL DP2 21 Range of read out 0 100 kPa 0 1 bar The application of pressures above the maximum read out pressure could damage the device Maximum pressure admissible 490 kPa 4 9 bar Units of measurement bar by default in the Microactivity Reference unit although these may be modified by the user Fluids applicable Non corrosive Response time lt 2 ms METHOD OF OPERATION Once the Microactivity Reference unit has been switched on the pressure sensor will at all times display the pressure drop in the system SYSTEM ALARMS By pressing twice the Mode button the device s screen displays the upper pressure limit If this is exceeded the system s pressure alarm is triggered The actions to be performed by the system in the event of such an alarm are as defined by the user on the pressure alarm screen on the Microactivity Reference s touch screen see section 4 5 2 of this manual By pressing once the Mode button
71. ated and computer controlled laboratory reactor for catalytic microactivity tests Possible unit configurations I ACIC IINIT ATAAHMKCQDLCDIC DDECCOCIIDEY BASIC UNIT ATMOSPHERIC PRESSURE Tubular reactor by Autoclave Engineers with 2 um porous plate Tmax 700 C Thermocouple in catalytic bed without thermowell Reactive system integrated within hot box Tmax 170 C 6 port VICI valve for reactor bypass 3 Hi Tec Bronkhorst mass flow controllers Liquid gas condenser separator tank cooled with Peltier cell Safety system integrated within microprocessor 2 temperature control loops 6 control devices for mass flow controllers Pressure sensor 0 1 bar Operating pressure in basic unit 1 bar Equipment design pressure 100 bar Piping valves and other devices in 316 stainless steel with low dead volume Software Process for monitoring and data acquisition with distributed control Remote control via Ethernet Heater on gas output line for up to 250 C PRESSURE CONTROL Pressure control system Liquid gas separator with HPLC Gilson liquid pump 400 consisting of a servocontrolled level control consisting of bar 0 01 5 ml min micrometric regulating valve a micrometric regulating opace for up to 6 MFC with stepper motor of 1 valve and capacitive level Balance at liquid output accuracy sensor of low dead Mass flow meter at gas output Pmax 100 bar Accuracy 0 2 volume 0 3 ml Special dimensions and
72. ation including 3 mass flow controllers for the gas inlets as well as the pressure control options in the reactor and liquid level control in the liquid gas separator LT mi d RA CLE Dee fm vm MICROACTIVITY REFERENCE DETAILED MAJNSGHYNERGREEN TT Fur X A GEH WANA TT MAP2GL2M5 Figure 4 1 17 4 1 PID Enga Tech THE REACTOR AND THE HOT BOX The tubular reactor consists of a nipple made by Autoclave Engineers model CNLX99012 whose standard model has the following specifications Length External diameter Internal diameter Material Internal volume Connections Seals Tmax recommended Pmax recommended 305 mm 14 5 mm 9 mm 316 L Stainless steel 20 ml SF562CX AE 6F2986 700 C 1350 bar at 25 C 400 bar at 482 C Pmax reactor 100 bar The following graphic illustrates the maximum working pressure for an Autoclave Engineers 316 stainless steel type nipple depending on the temperature BR Pressure Temperature Rating Curve 316 a 304 100 009 W Type 316 5 5 Before 800 427 C m a LIT This curve illustrates maximum working pressure for B NS 10 Type 316 stainless steel tubing valve and fitting bodies at H various temperatures to 1200 649 C expressed as EE a percentage of the R T pressure rating of the component E 60 Thus a component rated 10 000 psi 690 bar R T would 3 be rated 9 000 psi 621 bar 600 316 C or 90 of M
73. ature for the liquefied gas delivered from a pressurized cylinder When using carbon dioxide at a temperature of 22 C the value of the inlet pressure should be defined as 6 MPa A table of inlet pressures is shown below Ambient temperature C 15 20 22 25 30 31 Tc Pressure Po Mpa 51 58 60 65 72 7 4 Pc The default value is O Mpa Input Output parameter setup 1 0 Press Menu and I O The sequence of parameters is High pressure limit f the pressure reading from the manometric module rises above this limit the pump will stop The sequence following a high pressure error is described later in this chapter The pressure can be displayed in three different units bar MPa or kpsi Change the units by pressing the soft key below the units display bar MPa or kpsi The maximum value is 600 bars The default value is 600 Low pressure limit f the pressure reading from the manometric module drops below this limit the pump will stop The minimum value is 0 Default value is O Alarm The alarm is a buzzer which sounds every time there is an error or an invalid setting It can be programmed to be either On or Off This function only controls the operation of the buzzer it does not affect the operation of the pump when there is an error If the alarm is On the warning buzzer will sound every time there is an error An error can be a pressure limit or an invalid setting This parameter can be changed from On to Off and v
74. box door Touch screen Reactor temperature controller Hot box temperature controller Pressure controller for high pressure units when this option is included Level of liquid controller in L G separator when this option is included ON OFF switch Gases shut off valves Figure 2 3 PID EngaTech 2 4 3 INSIDE VIEW Electric forced convection Reactor thermocouple heater 15 um filter Liquid evaporator Autoclave Engineers tubular reactor Reactor furnace 6 port VICI VALCO valve for reactor by passing Micrometric servo controlled valve for pressure control optional 15 um filter Figure 2 4 2 4 4 REAR VIEW Liquid gas separator with level sensor and micrometric servo controlled valve optional Ethernet remote control General protection 220 VAC Power supply Figure 2 5 PID Enga Tech 2 4 5 INSIDE VIEW ELECTRONICS d toto tor to pasos Y 4 e asf 0 0 20 Ca 2 2 090 09 Cha k PERI KM kMkM o O o o o otn o o oto s90 9 0 0 0 0 9 0 0 0 0 02 0 12 V Power Supply a e e Ehd k k k wi e etojo oso AS AA 15 15 5V Power Supply gf IE WK 24 V Power Supply wee Digital servo V4 0 for level control opt Digital Seervo V4 0 for pressure control opt Relay Pump heating E WW af WAR fe fe ef Ze sie Cafe Zeieief 9 o ozo e rj dada 20202 D 20 e Ze Ze e 29 je le e eat e e H
75. ceed in the same way as outlined in section 4 6 2 3 of this manual but acting on the V4 0 servo digital unit corresponding to the level control valve which is accessed by unscrewing the metal plate on the right hand side of the reactor Level control in the separator is carried out by means of the TOHO TTM 005 controller that is located on the front of the reactor see Figure 2 3 whose operation is described in section 4 2 of this manual 54 PID Enga Tech DESIGN OF THE LIQUID GAS CONDENSER WITH LEVEL SENSOR 26 d IEFLON Sp a TEFLON GEI br P NET ii Figure 4 31 55 PID Enga Tech Capacitive level sensor Condenser Regulating micrometric valve Condenser amp level sensor Figure 4 32 4 7 SPECIAL OPTIONS FOR THE MICROACTIVITY REFERENCE UNIT Different options can be added to the Microactivity Basic unit depending on the customer process requirements Any of the options described below can be added to the most common configurations and most of them can be configured simultaneously 4 7 1 OPTION A EACH OTHER MASS FLOW CONTROLLERS UP TO 6 Microactivity Reference basic unit contains 3 Mass Flow Controllers including valves and installations Using this option you can add up to 6 Mass Flow Controllers in a wide range of pressure and flows Figure 4 33 Measuring principle is based on a stainless stell capillary tube with resistance thermometer elements A part of th
76. covering data and graphs from prior or current experiments From here visualizing renaming and configuring the graphs are possible as well as making a filter of all the acquired data When opening the experiment viewer a window with the process value and output control graphs pops up see figure 5 40 The data of each experiment is organized in three different sheets GRAPHS DATA and ERRORS There is also a ZOOM bar by means of which varying the size of the graphs or obtaining the exact value of a variable is allowed No Experiment File zoom Tools Figure 5 41 Initial window of the experiment viewer 5 5 1 How to open an experiment To open an experiment enter the File menu and select Open Experiment Ctrl O 122 PID Enga Tech Open Experiment Chr Delete Experiment Exit Ctrl x Figure 5 42 File menu Next a new window showing the content of the folder Plants will be shown C Program Files Process Plants As it has been said before by default there will be only one Project inside this folder However if the user renames the project with other names they will appear inside this window Select Project or Experiment Base Path Look in Plants D DI ex El 2 MICROACTIVITY REFERENCE My Recent Documents My Computer My Network File name v Places Files of type an Files X Cancel Current Folder Figure 5 43 Project selection window In order to see
77. creen and the procedure for making the level sensor calibration is described in the section 4 6 3 3 of this manual A TUE MAX LEVEL LEVEL 1234567 MIN LEVEL ET 123 FILTER LEVEL LIQUID K 123 45 LIQUID K REF 123 45 Figure 4 17 Press the Exit key to return to the main menu MISCELLANEOUS SETUP For setting up the following parameters 3 PID Enga Tech HEATER MANUAL G UTPUT MANUALS SET POINTCAUT Qs MANUAL OLITPLUT MANUALS SET POINT EnmLToOs Figure 4 18 HEATER Heating of the system s gas outlet line The heater control can be set as o Heater Manual By default In this mode the user can set the control output 96 of the heater in the Output manual field 0 No heating 100 Maximum power of heating In this mode the controller ignores the P I parameters and the set point fixed by the user o Heater Auto For using this mode of control the unit has to incorporate a thermocouple in the system s gas outlet line Working with this mode the user can set the desired set point and the P I parameters for the loop control The controller adjusts the control output CAUTION If the unit does not incorporate this thermocouple the MN selection of Auto mode of control inhibits the line heating even when the button HEAT is activated in the main screen AUX2 Auxiliary control loop for temperature control opt If the unit includes this option the
78. displayed on screen Before beginning to work with the equipment it is important to ensure that each reactant gas MFC installed has been properly set up and that all the other MFC s not installed have their fields set to zero If the unit incorporates a mass flow meter MFM the user has to set its maximum flow in this screen in ml min If the unit does not incorporate this option this field must be set to 0 ml min EE A E MFR MAS FLOR DEI ir ed SES dare talc Figure 4 11 Press the Exit key to return to the main menu ALARMS SETUP This screen allows the user to select the actions the system is to carry out in case an alarm goes off The alarms that can be configured are four temperature pressure level and external alarm 34 PID Enga Tech TEMPERATURE ALARMS PRESSURE ALARMS LEVEL ALA RMS EXTERNAL ALARMS Figure 4 12 gt TEMPERATURE ALARMS Set up menu for the temperature alarm This screen allows the user to select the actions the system is to carry out in the event of a temperature alarm Pressing on the keys selects one of the following options for each o OFF Gases that will be shut down during the alarm fuels inflammables reactants etc o FREE Gases that will maintain the same status they had prior to the alarm Inerts for diluting the concentration of reactants inside the reactor Press the Exit key to return to the main menu E M ls 9 ee T LO l FAL r 3F I7 MFC CHi FRE
79. e Besides it is easy to detect problems in the reaction system when existing inconsistencies in software graph panel Figure 4 37 6109 0 019 Repeatibility Std deviation 0 01 Linearity 0 02g 20 ppm C 10 C 30 C 50 F 86 F 0 01g 7 segment LCD display with backlight Character height 16 mm Display update 10 times per second Display 62 PID Enga Tech OPTION B SCALE WITH DIGITAL CUM LIQUID P 1 ETETA E OPTICA BYPASS VALVE 6 PORT 2 POS GAS OUTLET GAS 6 VMO6 CWO6 OPTIONAL Lig OUTLET 63 O le EngaTech By means of Process software measure of scale can be shown in Process Value Graph PV Graph T 8 Scale graph in Process Value graph grey color Figure 4 38 Rezero adjustment is possible in every session simply indicating 1 in the scale gap in session table window 6 Fin de semana con bomba Kb Session Table Session Time Units Alias 00 21 16 Days 0i d Description Session2 Session 3 Session4 Session5 Session6 Session Session8 Session 9 Session 10 Session 3 Session4 Session5 Session 6 Session 7 Session 8 Session 9 Session 10 REACCI N PARAR ENFRIARZ CERRAR SEGURIDAD CALENTAM2 f 5000 600 1800 1200 10 2700 600 600 Session 1 Sessioni iE SEGURIDAD 1 SessionTime sec 1 y
80. e gas flows through this bypass sensor and is warmed up by heater Rh 56 PID Enga Tech Consequently the measured temperatures T1 and T2 drift apart The temperature difference is directly proportional to mass flow through sensor Accuracy incl linearity based on actual calibration Turndown Repeatability Settling time controller Measurement control system Mechanical parts mE 09i A Material wetted parts stainless steel 316L or comparable 10 FS for ranges 3 5 ml min i Surface quality wetted parts Ra 0 8 um typical 120 FS for ranges lt 3 ml min p A 1 50 Gn digital mode up to 1 187 5 rocess connections compression type or face seal couplings lt 0 2 Rd Seals standard Viton standard 1 2 seconds options EPDM Kalrez FFKM option down to 500 msec Ingress protection housing IP40 Control stability Operating temperature Temperature sensitivity Pressure sensitivity Leak integrity outboard Attitude sensitivity Warm up time Temperature profile Measured AT without flow sm Temperature profile with flow Medium temperature Ambient temperature Sensor tube Temperature Heating Temperature measurement 1 element measurement 2 Turbulence filter Laminar flow element AT T2 T1 in Kelvin C specific heat m mass flow Figure 4 34 lt 0 1 FS typical for 1 l min N 10 70 C zero lt 0 05 FS C span lt 0
81. e s lower limit Output control 96 in manual mode 0 100 IATA Alarm higher limit Alarm higher limit C Output control 0 100 M10 Activate Deactivate Heat 1 Activate O Deactivate Set point for gas n Gas flow in ml min IR Turn on or off the pump n ps Set point for the pump Liquids flow in ml min XON Chromatography cycle M d XTO Time for chromatograpy cycle Time between two analysis Table 5 6 Values of the parameters 5 3 4 2 How to Save a Session The session menu table provides the option to save sessions Save Table to open saved sessions Load Table and to delete all data Clean Table To save an experiment s session table in order to use it later on open the Sessions Table menu and click on Save Table A new window will pop up with the name of other previously saved sessions To choose a name for a new session click on New File and choose Accept A new window will then appear where the new name can be introduced Session Table Load Table Print V Clean Table Exit Figure 5 36 Session table menu 117 Save Session Table File Mame FileName Figure 5 37 Saving a sessions table 5 3 4 3 How to open a saved sessions table When a sessions table is opened the field for the different values appear empty If preferred open sessions table that have been saved previously To do so click on Session Table and then select Load Table When doing thi
82. each one of the digits and then use the A and V keys to increase or decrease the value The standard set up for the Microactivity Reference reactor is detailed in Table 4 1 Table 4 1 Control Reactor Hot box Pressure Level parameter temperature tem SS _EHt 700 j40 dontmodfy Other parameters of major importance that configure this type of controller are those that are shown below in Table 4 2 with their standard values for operation with the Microactivity Reference unit these parameters may vary from one unit to another For verification of a reactor s specific set up consult the technical documentation that is supplied with the equipment 21 PID Enga Tech Temperature Temperature 0 o 2 2 NU Table 4 1 P 1 D values depend on the operation conditions As an example in Table 4 3 the PID parameters for the reactor oven are shown depending on the working temperature 600 300 C P1 40 40 46 2350 D 65 10 MHi 30 30 Table 4 3 There now follows a brief introduction to the different methods that are used for tuning proportional integral and derivative PID controllers and the criteria that are followed for considering that optimum control of the process has been achieved 22 PID Enga Tech 4 2 2 CONTROL STABILITY CRITERIA Stability is the control system feature that makes the variable return to the set point following a disturbance The mos
83. ed to operate separately from the Microactivity Reference unit Figure 3 3 b Connect the connection terminal stop for system alarm as well as the 9 pin sub D connector digital communications on the rear side of the pump Figure 3 3 c Connect the round connector on the end of this same cable to the Pump Control on the rear of the Microactivity Reference Figure 3 3 d Connect the round connector AUX 1 to the AUX 1 on the rear side of the Microactivity Reference and the end of this same cable power cable to the black electric strip Figure 3 4 e Connect the vessel cable to the black electric strip Figure 3 4 The following connections are to be made in the case of the dumper and head Gilson pump calefaction f Connect the pump head cable on the front of the pump to the black electric strip Figure 3 5 d g Connect the pump dumper cable in the rear of the pump to the black electric strip Figure 3 5 e b b Figure 3 3 PID EngaTech a strip slectric b aux 1 c vessel heating Figure 3 4 Figure 3 5 e Installation of the liquid scale see Figure 3 6 a Connect the sub D type connector digital communications to the rear side of the scale b Connect the JACK type plug power supply on the left of the sub D connector c These two connectors are joined in a single round connector that has to be plugged into the corresponding socket on the rear of t
84. em Figure 5 6 Installation complete 5 2 2 HOW TO INSTALL A PROJECT OR MICROACTIVITY CONFIGURATION Before finishing the installation of Process the program allows for the option to install a PROJECT see Figure 5 7 Figure 5 7 Project Installation Option If the project is installed the directory where our project is must be selected the name of the folder containing our project must appear next to Search in see Figure 5 8 Once done accept by clicking in Current Folder on the right bottom corner 98 must be the same in the PC an in the MA Enga Tech The name of the Project folder must appear here Select Project or Experiment Base Path Look in MA REFERENCE e DIr ES 3 Data Ze Graphs My Recent Panel Documents sessions 3 Devices_Config dat Ca f Eq ta Plant Cfg cfg My Documents My Computer Y PEN twork File name aces Files of type LA Files D Cancel Click on current TUM folder to accept Figure 5 8 Project s folder selection The Project is saved inside the Plants folder C Program files Process Plants By default there will be only one project inside Plants but if the user saves the plant with a different name a new folder with the new name will also be created in this directory The other possible option consists on installing the project after Process has been installed by means of an executable file which will copy the project s folder inside Plants
85. en with the device name in which the following parameters can be selected Graph s scale to set the higher and lower value of the variable s graph High and low alarm value These values don t affect the process They just lit a red indicator in the graphic control panel to indicate that a certain value has been surpassed a Graph s color By clicking on the colored window a color palette is opened a Graph s display Click on the tick to hide or show the graph 112 PID Enga Tech REACTOR High Limit 700 00 High Alarm 00 00 Low Limit 0 00 Low Alarm l 0 00 Grahp Color a Grahp Visible S Figure 5 32 Graph configuration for a variable Reactor Temperature Once the values for this device have been set click on OK to save the changes To change from one variable to another click on the different displays The scale shown in the y axis corresponds to the graph whose display on the lower part shows a black border By double clicking on a variable s display the graphs can be hidden To configure the Control Value Graph values follow the same steps In that case the control output percentage will be shown This is why by default the Y axis will show a range from O to 100 Figure 5 33 Output control graphic To modify the X axle right click on the graphic s background or on one of the time values and then select Set Time Scale This option allows choosing the visualization time with a
86. er gt Temperature control of the hot box The signal from the thermocouple located in the hot box is assessed by the controller whereby its 4 20 mA output signal is sent to a solid state zero passage type relay that regulates the power supplied to the box s heater in a proportional manner gt Level temperature control The signal from the thermocouple located in the deposit is assessed by the controller whereby its 4 20 mA output signal is sent to a solid state zero passage type relay that regulates the power supplied to the cartridge in a proportional manner gt There is a fourth zero passage relay for the possible temperature control of a heating pad for heating a gas outlet line an evaporator etc gt Pressure control The signal from the pressure transmitter located upstream of the reactor is assessed by the controller whereby its 4 20 mA output signal determines the position of the pressure control valve gt Level control The signal from the capacitive signal installed in the liquid gas separator is assessed by the controller whereby its 4 20 mA output signal determines the position of the level control valve positioned at the base of the separator gt Flow control The instruments used for dosing the gases into the reactor are in themselves flow controllers Accordingly the reactor s control system simply relays the 0 5 VDC control signals to the MFC The signal recognises the 0 5 VDC output signal from the MF
87. ests in this manual Set the 3 port valve to the by pass position If the system pressure does not decrease check all possible causes of the prior symptom The pressure in the system rises uncontrollably without responding to the set point with the 3 port valve in the by pass position A blockage has formed in the gas outlet line outside the reactor box on the way to the analysis system The needle on the micrometric pressure regulation valve has become stuck at zero Release the gas outlet line where it joins the filter and see whether the pressure The filter on the reactor outlet is blocked decreases If it does replace the filter If it does not continue by verifying the next cause Release the connecting joint between the gas inlet line and the reactor and see whether the pressure decreases If it does empty the reactor and clean the plate by flushing it with compressed air counter current to the gas flow If this is not the solution replace the porous plate inform the distributor Release the gas outlet line before it passes The filter on the reactor gas inlet is through the filter and see whether the blocked pressure decreases If it does replace the filter Restore the optimum control parameters for The controller s PID parameters have this controller see the section The been modified controllers in this manual Incorrect operation of the level control Stop feeding liquids into
88. g these steps Remove the threaded plug back pressure Figure 4 25 and press the Prime key The pump will start pumping liquid at its maximum capacity 5 ml min until the liquid drops in continuous mode that means all the bubbles has been removed Press Stop key to finish venting the pump and connect the threaded plug back pressure Putting the 3 port valve in the position a Figure 4 25 then press the Prime key The liquid will drops in continuous mode and the pressure value at pump s screen will be around 30 bar Press the Stop function key to finish venting the pump and set the valve to its normal operating position Figure 4 25 position b Figure 4 25 45 PID Enga Tech 4 6 1 7 Pump operation After entering the data about the pumping system the pump is ready to run The 307 pump can operate in 3 different modes These modes are Flow The 307 pump provides a constant flow rate The pump starts when the Run key is pressed and stops when the Stop key is pressed Dispense The 307 dispenses a specified volume The pump starts when the Start key is pressed and stops when the specified volume has been dispensed Program The 307 controls a complete system In this mode the 307 pump can create gradients of flow rate open and close outputs to control other instruments and wait for signals from other instruments By default the pump is programmed to operate in Flow mode meaning that it
89. h the circuit breaker to OFF unscrew the right hand side panel and verify the sensor s connection Disconnect the equipment switch the circuit breaker to OFF unscrew the right hand side panel and verify the TOHO level connection Verify the status of the source by unscrewing the right hand side equipment disconnected and without power supply and observe the LED If it is blinking disconnect the controllers on the rear panel one by one until the one causing the short circuit is located the LED will stop blinking On the level sensor s touch screen restore the values obtained in calibration If these are not available re calibrate the sensor see the section Calibrating the level sensor in this manual Dismantle the condenser and the sensor and clean them with ethanol compressed air Restore the optimum control parameters for this controller see the section The controllers in this manual Set the controllers nd parameter to automatic Run Dismantle the condenser and the sensor and clean them with ethanol compressed air Check and adjust the zero setting on the level control valve see the section Configuration of the Servo Digital V4 0 unit in the manual Check that the pump is working properly The liquids pump is not working properly providing the system with a constant stream of liguid The level controller is set to manual fully closed 096 A blockage has formed in the liqu
90. he gases that has not have not been installed on the equipment been installed There is no communication between the touch screen the control PC and the Reboot the equipment equipment hardware Insufficient gas pressure is reaching the Verify that the gas inlet pressure on the equipment equipment exceeds the operating pressure i 1 o The gas flow does not reach the The set point established is below 10 nO o e due UI set point established remaining of the maximum flow of the mass flow ud ae inen ee stable at a lower value controller orocess requirements A reading is recorded on one of the MFC that has not been installed noise Modification has been made of the maximum gas flow established on the touch screen for the configuration of the mass flow controllers Heset the maximum flow value for each one of the controllers see the specific documentation for each MFC 142 The Gilson liquid pump does not switch on with the Microactivity switched off The Gilson liquid pump does not switch on with the Microactivity switched on The Gilson pump does not register the information or the set points relayed to it from the Process software The Gilson pump does not respond to the parameters that are manually entered into the display No liquid is entering the reactor or the flow is unstable Pressure of the head below operating pressure No liquid is entering the reactor Pressu
91. he hot box Scale Control ill ist Figure 3 6 13 PID Enga Tech e Installation of the MFM see figure 3 7 a Connect the sub D type connector digital communications to the rear side of the MFM b Connect the round connector on the end of this same cable to the MFM on the rear side of the Microactivity Reference a Sub D MFM b Round connector MFM Figure 3 7 e Installation of the level of liquids in the condenser level sensor see figure 3 8 a Connect the round connector level sensor to the rear side of the level Sensor b Connect the round connector on the end of this same cable to the level sensor on the rear of the Microactivity Reference 14 Figure 3 8 e Other components On the rear side of the Microactivity Reference s hot box there is a circular type connector for each one of the devices that may be connected to the unit such as o Valve for regulating the level of liquids in the condenser Liquid Valve e Installations of the thermocouple for the liquid gas separator a Connect the thermocouple connector to the TI 2 in the rear side of the Microactivity see figure 3 9 Figure 3 9 15 PID Enga Tech e Installations of the liquid liquid gas L L G separator see figure 3 10 a Connect the sub D connector digital communications on the rear side of the Microactivity Reference and connect the round connector on the end of th
92. hen a vaporisation of liquid s is required upstream of the reactor an extra evaporator s can be added to the unit Figure 4 55 Figure 4 56 If two HPLC pump are installed and vaporisation of both liquids is required then two liquid evaporators can be installed e Extra SS316 evaporator with temperature control 50 C to 450 C e Maximum power consumption 600 W e Maximum liquid flow 8 ml min The precise temperature adjustment is achieved by selection of this variable in the controller Output 1 2 Process value Alarm leds 1 and 2 Set point control output Cursor displacement by the digits in each function Digital signals Decrease button Access level selector Increase button Figure 4 57 82 PID Engatech UPIIUN 5 LIQUID 2 LIQUID 1 GAS 1 GAS 3 GAS 4 GAS 5 GAS 6 t t t i E CEXTRA LIQUID EVAPORATOR WITH e T Bm e e Po E oia NR MECH FTN A ec Ho VMO1 Cvn1 MFC 2 P co ML CHA L vM 2 CVZ MFCO3 ec h HUA Hi VO Cv03 MFCO4 PEN a E arl L er zu Be WYO CMD MFCOS Sich SR an Ad ei VROS CVDS MFCOS Pic e NE CH le 4106 VU OPTIONAL HOT BOX 180 C BYPASS VALVE 6 PORT 2 POS 83 TEMPERATURE CONTROL GAS OUTLET Lig OUTLET PID EngaTech 4 7 10 OPTION T TEMPERATURE CONTROL IN L G SEPARATOR Liquid gas separator included in the basic unit can incorporate a precise temperature control system i
93. hese parameters IP MASK 255 255 255 0 must be the same in the PC an in the MA GATEWAY 192 168 0 1 Table 5 2 Control PC communication Parameter values 5 3 DATA ACQUISITION WITH PROCESSO To open the application double click on the Process icon Figure 5 11 The menu or application manager is the first thing to appear when opening Process In the menu bar contains all the tools to manage the application to control the data acquisition and to manage the other application functions project acquisition panel Sessions table graphs and experiment viewer 101 Enga Tech MA e X Project Adquisitiom Panels Sessions Graphs Tools cquisition New project Open project indicator Start Stop Acquisition Acquisition Exit Process Figure 5 12 Process Main Function Menu New project This function is not available for the user Open project To choose among saved projects Play To start data acquisition Stop To stop data acquisition When it is stopped the database is S generated Close To exit the software Data Acquisition Indicator next to close Displayed in a light green when acquiring data and in a dark green when not acquiring data Table 5 3 Process Main Function Menu Icon Description 5 3 1 THE MENU BAR The name of the Project that is being executed is shown in the screen s upper section The different software functions are shown in the main function menu Q Project
94. hols 23 PID Enga Tech Analytical methods applied when the process model or the equation relative to the system s dynamics are known They are difficult to apply in pilot plant control systems given the absence of reliable processes data and they are only applied when sufficient information is available for the perfect identification of the process model transfer function usually in industrial environments It is worth noting here that the procedures referred to as auto tuning are based on empiric experiences and results obtained in industrial environments which have nothing to do with the processes taking place in a laboratory pilot plant 4 2 3 1 Ziegler amp Nichols method It is the most widespread experimental method for tuning the regulation parameters of a PID controller although it is not recommended when the tuning is carried out mainly with a view to stable transition between different process states variations in reaction temperature for the screening of catalyst activity at different temperatures instead of seeking the long term stability of the same The method allows for calculating the three values of the PID actions on the basis of the data obtained in a quick test of the characteristics of the closed control loop In short it consists in gradually narrowing the proportional band from an initial value e g 15 9o with TO and D 0 whilst small disturbances are created until the process begins to oscillate con
95. ice versa by pressing the soft key Change 44 PID EngaTech e GSIOC Unit identification number A Gilson system can be controlled from a computer using a GSIOC interface and GSIOC cables Each instrument in a system must have a unique identification number to distinguish it from other equipment connected to the GSIOC communications channel The GSIOC identification number in the 307 can be set between 0 and 63 The default value is 1 e Output XX is open Closed There are four relay outputs in the 307 pump numbered 1 2 3 and 4 These outputs are used to control other instruments They can be programmed to open and close during a method run They can also be opened and closed manually The default state is open e Zero pressure reading The Zero soft key is used to set the pressure reading to zero when there is zero pressure in the system This ensures accurate pressure readings when the pump is running Before pressing Zero make sure that the pump has stopped and the pressure has dropped to zero otherwise further pressure indications will be incorrect If the operation is successful the message Pressure reading is zero is displayed If the operation is not successful due to pressure in the system the message Not done check pressure is displayed 4 6 1 6 Venting the pump The system needs to be vented before the liquids pump is operated This involves filling the inlet tank with the liquid that is going to be used and followin
96. ickness of 0 02 and at a temperature of 316 C The pipes selected that constitute the reactor are Pipe TSS285 1 6 pipe with internal diameter of 2 1 mm 0 0857 Declared standards EN 10204 3 1B DIN50049 2 2 PTSS120 1 16 pipe with internal diameter of 0 50 mm 0 020 Declared standards EN 10204 3 1B DIN50049 2 2 4 8 2 JOINTS AND VALVES Check valve for liquid feeding SG SS 2C4 KZ 25 Located on the liquid inlet line to the reactor 316 stainless steel valve with Kalrez sealing material Maximum operating pressure and backpressure at 21 C of 206 bar 3000 psig Trigger pressure of 25 psi Operating temperature of 23 C to 191 C S Cy 0 10 For a valve with a rated pressure trigger spring of 25 psig true trigger pressure ranges between 21 and 29 psig The minimum closing pressure is 17 psig A series of Teflon pieces have been designed to reduce the flow section to the equivalent of a 1 16 pipe as well as the dead volumes in the NPT type joints see Figure 4 66 87 PID Enga Tech HOKE 1CM2 318 eu AGELCOIEK 55 204 Ket 25 HOKE 1CM2 318 ch IL we Este Figure 4 62 3 port T connection VV ZT2 316 stainless steel 1 8 pipe thread connection and orifice of 0 75 mm Operating pressure of 400 bar In order to avoid standard wear and tear on the connecting pieces on a reactor phenomenon that mainly occurs with T shaped connections give
97. id outlet line prior to its collection in the balance The needle on the micrometric level regulation valve has become stuck at zero The valve s zero setting has been modified Set the controller s automatic Run Release the liquid outlet line just after it passes through the micrometric valve and see whether any liquid is coming out of the system If it is replace the liquid outlet line Release the liquid outlet line on the separator and see whether liquid is coming out of the tank If it is replace the regulating valve inform the distributor Check and adjust the zero setting on the level control valve see the section Configuration of the Servo Digital V4 0 unit in the manual _nd parameter to 146 The change in programmed session does not occur PC and Microactivity are not communicating The inhibition function has been triggered as a safety measure in response to a system alarm The communication parameters are not correct The cable is not connected PID Enga Tech This function is automatically shutdown when the situation triggering the alarm has been resolved except in the case of pressure alarms In this case check the alarm and reset it if the situation that triggered it has been resolved Check the communication parameters in your PC Network Connections and in the Microactivity Reference Check the IP address ProcessQ is reading in Project menu Check the cross c
98. ighter fit within an orifice generating a variable section passage that depends on the distance the needle has been moved Figure 4 26 47 PID Enga Tech Plug Rod po JpEbE Figure 4 26 This kind of valve furthermore improves rangeability control precision as displacement is not performed linearly but rather by means of the turning action of the rod caused by a micrometric screw lf the shaft of the screw allows for 10 turns from the fully open position through to the fully closed position and each turn is a full 360 fitted with an actuation system which has been designed for this unit and which distinguishes the position with an accuracy of 1 degree of circumference there is a total of 3600 possible states for the relative orifice needle position which means a precision for the system s pressure control of 0 1 bar without permitting sudden variations in the gas flow at the reactor outlet of more than 5 of the total flow passing through the reactor bed In a study carried out with 8 commercial micrometric regulating valves the one providing the best results in the Microactivity Reference reactor operating with flows below 50 ml min and pressures higher than 50 bar is one made by Hoke model 1315G2Y which has the following specifications Maximum operating pressure 345 bar at 21 C Range of operating temperatures from 54 C to 232 C it may be found fitted inside the hot box so avoiding the formation of co
99. interfere with cooling and limit access to the top of the instrument A WARNING Be careful when lifting the unit Because it is heavy two people should lift it When moving the equipment be aware that the back is heavier than the front 3 2 3 ELECTRICAL INSTALLATION The unit s electrical installation is performed as described forthwith A For reasons of safety do not connect to the mains until the full installation of the equipment has been completed The installation of the external devices that are described will be only possible if they have been chosen as a configuration option of the Microactivity Reference reactor e Installation of the liquid gas separator Peltier Connect the end of the cable power supply to the Peltier round connector that is to be found on the rear side of the reactors hot box as shown in Figure 3 1 xD um LU Figure 3 1 e Installation of the liquid pump Before installing the pump make sure the on off switch to be found on the rear side of the pump is in the off position o Figure 3 2 PID Enga Tech Figure 3 2 The following connections are to be made see Figure 3 3 3 4 a Connect the power cable to one of the two 220 VAC power sockets on the rear side of the unit These power sockets will cease to supply power when the equipment is switched off by means of the switch on the front so it is not advisable to connect analysis equipment or other devices that ne
100. is same cable to the RS 485 on the rear of the L L G separator b Connect the round connector peltier on the rear of the Microactivity Reference and connect the round connector on the end of this same cable to the Peltier connection on the rear side of the L L G separator c Connect the round connector AUX2 on the rear side of the Microactivity Reference and connect the round connector on the end of this same cable to the Alarm connection on the rear of the L L G separator d Connect the cable with a thermocouple connector to the TI 1 in the rear of the Microactivity Ref unit Note If you connect the L L G separator you have to disconnect necessary connections of the L G separator Figure 3 10 e Gas outlet on the system Leading to the analysis system A heater is included for this line see Figure 3 11 16 PID Enga Tech Figure 3 11 e Connection to Ethernet The direct connection between the Microactivity Reference and the control PC is performed by means of the crossed cable supplied with the equipment connecting it on the rear of the reactor box Ethernet Remote Control Figure 3 12 When the connection is made via Ethernet it is made with a category 5 UTP connection cable for Ethernet networks with a RJ45 connector The Ethernet connection between the PC and the Microactivity Reference is reduced to 10 Mbts base T Figure 3 12 e hereactor s power socket is on the lower rear of the reactor
101. ivated from the software The set point must be introduced in the touch screen Activate ON v Output Control wem P Figure 5 26 Heat design window f ALARM They are circular displays that inform about the system alarm state When the alarm is activated the display changes from green to red g PUMP Under pump the liquid flow and activation RUN and deactivation STOP of the pump is allowed o2 Osto Fa en Figure 5 27 Pump design control window h SCALE 110 PID Enga Tech The Scale Design option allows resetting the scale to zero by pressing on the red button of the window SCALE cm QD o Figure 5 28 Scale rezero window i CHROMATOGRAPH The Microactivity Reference unit is prepared to be connected to a gas chromatograph by actuating the sampling injection valve to start the analysis see point 5 7 CONNECTION TO A GAS CHROMATOGRAPH With Process Q it is possible to activate a cycle to close every given time the electrical circuit that connects to GC during one second The user can configure the cycle time how often the circuit is closed in the chromatograph design window CHROMA State fa Actuar Ti Wi E Figure 5 29 Chromatograph design window 5 3 3 CONTROL GRAPHS The graphs created in real time by Process show the measured values Process Value Graph and the output control signal Output Control Graph To see the graphs choose Graphs in the tool bar and selec
102. l keypad 3 Pump head 4 Pump head fastener o Inlet to pump head 6 Outlet from pump head 7 Connections to manometer module 8 Side attachment 9 Side screws Figure 4 23 4 6 1 2 Keyboard 1 Power indicator 2 Screen 3 Function keys Their function is displayed on the screen and changes according to the menu 4 PRIME The pump runs with maximum flow until STOP is pressed 5 HELP Displays messages and instructions related to the system with no effect on pump operation 6 CANCEL Clears the last entry without storing it in the memory 7 ENTER Confirmation key 8 Numerical keypad Figure 4 24 omes EST kel la JEJE Eg E I Je 42 PID Enga Tech 4 6 1 3 Technical Specifications Purnp Pump Heads X stainless steel W rnsing compartment for aqueous salt solutions 20 1M Ti z titanium Operating Modes Programmable Parameters Pressure Pulse Dampening Communication Interface Display Panel Front Panel Liquid Contact Materials Power Requirements Environmental Operating Temperature R Manufacturing Standards Instrument Dimensions iw xdx hi Instrument Weight with head Shipping Weight with head Programmable redprocating pump with single pistan interchangeable head constant stroke and fast refill motion internal feedback pulse damperer and pressure
103. lead to the stabilisation of the controlled variable a few cycles after a disturbance 4 2 3 3 Method proposed by PID Eng amp Tech Based on the accumulated experience of PID Eng amp Tech in the tuning of pilot plant or laboratory processes where the system gains are high transport delays are lower than normal in industrial environments and where the system s readiness to respond to changes in the set points is especially prevalent a new method has been designed for tuning said parameters based on the experience acquired in the control of processes It is relatively easy to predict the value of the proportional band that is suitable for a process if one bears in mind the physical interpretation of this concept If the proportional band located around the set point is understood to be the area within which the controller goes from providing a control output of O to 100 and if manual manipulation has been made beforehand of the final control element in the process conditions the operator may know for example that in a pressure control system the valve must remain closed until a pressure of 86 bar is achieved when the aim is to reach 90 bar and as of that moment the control action may be performed to regulate the set point This indicates that the proportional band should have a value of 8 bar 4 above and 4 below the set point If it is taken into account that the operating interval is 100 bar this 8 bar proportional band corresponds t
104. low Meters F 0 20 m sourcing internal seals on O 10 0 15 ml min G 4 20 m sourcing Y Viton factory standard 1h 0 15 D 15000 misin E EPDM 2M 0 10 0 250 l min K Kalrez FFKIVI 3M 0 200 0 1250 l min for PN amp DO Flow Controllers DM Q 10 0 500 ml min 1h 0 0 5 7 0 90 Lymn zM 0 10 0 100 Leger Figure 7 3 Gas Determined by the user Maximum flow Determined by the user Inlet pressure Determined by the user 5 Place the new MFC in the distributor screwing it in from the lower panel and attaching the end connectors it is advisable to attach a label indicating the gas it contains and its operating flow Place it in such a way that the arrow is pointing to the right indicating the direction of gas flow Connect the control cable to the MFC Screw the right hand side panel back onto the Microactivity Reference unit Switch on the unit Configure the MFC installed on the touch screen of the Microactivity Reference unit Pressing F1 on the touch screen grants access to the main menu CONFIG SETUP SAN 137 PID Enga Tech PLUS a B LN LE n ua l MASS FLOW SETUP ALARM SETUP LEVEL SE PUE ADMIN SETUP MIsc SETUP ABOUT PID COMMUNICATIONS SETUP PELTIER CONTROL Figure 7 4 Press on the field MASS FLOW SETUP The configuration menu for the mass flow controllers will be displayed e es EE el E Ee A A orn HA FLOW UNIT lA MFM MAS FLOM EFE ea
105. m Level Servo Alarm in the Digital Servo of the micrometric valve for regulating the liquid level in the liquid gas separator Press the Exit key to return to the main menu 9 BYPASS Operating the reactors by pass valve Access is provided by means of the Bypass key When this icon is depressed the valve is in by pass mode isolating the reactor 10 DOOR Opening closing of the hot box door It is operated by pressing the Door key 4 5 2 MAIN MENU Press the F1 key on the touch menu to access the main menu from where the following set up screens can be accessed A e LEN We MASS FLOW SETUP ALARM SETUP EE VEL SE TUF ADMIN SETUP ae oe NI ABOUT PID COMMUNICATIONS SETUP PELTIER CONTROL Figure 4 10 MASS FLOW SETUP Set up menu for the mass flow controllers MFC The following is displayed for each one of the system s MFC s 33 PID Enga Tech o Maximum flow These values are determined in accordance with the number of controllers of the equipment o Units in which the gas flow is expressed Name of the gas o of alarm Deviation alarm This alarm is inhibited during the time specified in the Delay Time Alarm in sec being triggered if the specified deviation persists during this time with respect to the set value O All these parameters may be modified by the user by pressing on their corresponding yellow boxes and entering the new values by means of the keys that are
106. make sure i the system s air inlet pressure is 5 bar Disconnect the equipment switch the circuit breaker to OFF unscrew the right and left hand side panels on the equipment and check the orange polyurethane No communication is established between the reactor and the control PC The door on the reactor does not open and on the by pass valve Leaks in the compressed air lines or does not operate poor coupling of the pneumatic connections Check the gas installation and make sure No gas pressure reaches the equipment the gas cylinders are open Dees stopcocks on the front panel Open the on off stopcocks No gases are entering the equipment A system alarm has been triggered that has shutdown the gas inlet Check the alarm and reset it providing the situation that triggered it has been resolved Increase the pressure on the gas inlet see the specifications of the MFC or lower the operating pressure Disconnect the equipment switch the circuit The cable that connects the MFC to the breaker to OFF unscrew the right hand board has been badly connected loose side panel on the equipment and check the connection of the MFC cables The pressure in the system is close to the pressure in the gas cylinders The flow of one of the gases varies without keeping to the set point A maximum flow has been set on the MFC configuration panel on the touch Zero set all the fields for those MFC that screen for one of t
107. materials bar Control loop and of reactor Control loop and 100 bar capacitive sensor Extra VICI VALCO valve for pressure transducer Digital communications special purposes Digital communications 1 1 USING THIS MANUAL To ensure the correct use and operation of the Microactivity Reference unit it is advisable to proceed as follows Read the general description of the equipment in chapter 2 Install the instrument as shown in chapter 3 Read the description of the equipment s components in chapters 4 and 5 Following the operating instructions outlined in chapter 6 1 2 SAFETY INFORMATION 1 21 SAFETY INFORMATION This unit meets the following EN 61010 1 2001 and it has been designed and tested in accordance with recognized safety standards and designed for use indoors If the bugs Tech instrument is used in a manner not specified by the manufacturer the protection provided by the instrument may be impaired Whenever the safety protection of the Microactivity Reference unit has been compromised disconnect the unit from all power sources and secure the unit against unintended operation Refer servicing to qualified servile personnel Substituting parts or performing any unauthorized modification to the instrument may result in a safety hazard Disconnect the AC power cord before removing covers 1 22 SAFETY SYMBOLS Warnings in the manual or on the instrument must be observed during all phases of operation
108. mended humidity range 50 60 96 Humidity range o 80 96 Hecommended altitude range Up to 2000 m After exposing the unit to extremes of temperature or humidity allow 15 minutes for it to return to the recommended ranges 3 1 2 VENTILATION REQUIREMENTS Do not obstruct air flow around the instrument 3 1 3 BENCHTOP SPACE REQUIREMENTS The equipment dimensions are the following Height 100 cm Height Width 85 cm Depth 75 cm Depth Width PID Enga Tech 3 1 4 ELECTRICAL REQUIREMENTS 3 1 4 1 Grounding MN CAUTION A proper earth ground is required for MA Ref operations To protect users the metal instrument panels and cabinet are grounded through the three conductor power line cord in accordance with International Electrotechnical Commission IEC requirements The three conductor power line cord when plugged into a properly grounded receptacle grounds the instrument and minimizes shock hazard A properly grounded receptacle is one that is connected to a suitable earth ground Proper receptacle grounding should be verified Make sure the unit is connected to a dedicated receptacle The use of a dedicator receptacle reduces interference CAUTION Any interruption of the grounding conductor or disconnection of the power cord cause a shock that could result in personal injury 3 1 4 2 Line Voltage The unit is designed to work with a specific voltage make sure your lab has the appropriate voltage option for the
109. ministrator The password is not available for the user of the unit 39 PID Enga Tech Figure 4 21 ABOUT PID Product information P dpa ME a E c d e MICROACTIVITY REFERENCE POD VER v3 18 22 10 2806 HARDWARE VER MICROS YER ABCDEF ADKSERY VER ABCDEF Al EngaTech Integral Development Eng amp Tech LG Plomo 15 Polig Ing Sur Colmenar iejo Madrid Seain Tel 34 9391845993 Wu pidenatech com Figure 4 22 This screen provides information regarding the company PID Eng amp Tech as well as the software versions installed in the unit o Pod Ver Software for the touch screen o Hardware Ver Software for the control panel o Micro3 Ver Control software o Adkserv Ver Embedded software Press the Exit key to return to the main menu 40 PID Enga Tech 4 5 3 OTHER FUNCTIONS Adjustment of contrast of the touch screen This function is accessed by means of the System key on the touch screen and may be increased or decreased using the F3 and F4 keys 41 4 6 SPECIAL CONFIGURATIONS OF THE MICROACTIVITY REFERENCE 4 6 1 THE GILSON 307 HPLC PUMP PID Enga Tech The Microactivity Reference reactor provides the option of working with liquids introduced into the system When this option is required the system is fitted with a HPLC positive alternative displacement pump made by the firm GILSON 4 6 1 1 Front view 1 Digital screen 2 Numerica
110. n a range from 0 C to 65 C when necessary Control system is based on a Peltier cell described in chapter 4 3 A A A a AN Thermocouple for temperature control in L G separator Peltier cell xli L Pl e le Jm D E ee IN AR AA mu L k 1 EI i J x DES mui 4 kt b le Figure 4 58 d 810 Hoo a 1 SES Peltier button in t touch screen 4 ILL D e LA A 4 e 42 e Figure 4 59 i S ER mm LL Lm E I As described in liquid evaporator control temperature control in L G separator is made by means of a controller but Peltier button must be ON in touch screen to let Peltier cell heating and cooling 84 PID Enga Tech Peltier control setup in screen menu must be configured previously A pe LEN Wa E TLulr MASS FLOW SETUP RAEE E ERI LEVEL SETUP ADMIN SETUP MISC SETUP ABOUT PID COMMUNICATIONS SETUP PELTIER CONTROL Figure 4 60 mdi 200 E A UN 9 os A e T Rol FELTIER MODE Peltier button in touch screen FELTIER CONFIG FELTIER CONTROL DUTY TIME Figure 4 61 Peltier control is usually established in 95 and duty time in 10 s 85 PID Enga Tech OPTION I CTEMPERATURE CUNTRULLER FUR L G SEPARATOR LIQUID H HOT BOX 180 C TEN OPTIONAL FUN AOL NIE MFCO1 FN UY GAS 1 gt I Ka mmm E pm vMO1 CvO1 i l MFCO2 FE i 7 L GAS 2
111. n the difficulty in using a counter spanner selection has been made of VICI VALCO connecting pieces mounted onto the structure of the hot box thereby enabling them to be manipulated with a single spanner Bushing SG SS 200 61 PID 316 type stainless steel 1 8 extra long threaded connection pipe As per Standards ASTM A 182 ASTM A 479 and CMTR certificate Operating temperatures ranging between 200 C and 426 C Swagelok has custom made extra long bushing pieces for the Microactivity Reference unit They permit the inlet and outlet of process lines passing through the insulation separating the hot box and the thermal separation chamber from the rest of the mechanical assembly These pieces are not commercially available Reduction element VV IZR21L 1 8 VICI pipe thread reduction connection to 1 16 pipe thread 916 type stainless steel Non return valve SG SS 2C2 1 Kalrez 316 stainless steel Joint in chemically compatible Kalrez Teflon elastomer As per Standards ASTM A 182 ASTM A 479 and CMTR certificate Maximum operating pressure of 2185 psig 150bar at 190 C Cy 0 1 In order to avoid the multiple connections required for the feed arrangement of various gases and so as to favour the mixture of the same a distributor has been designed in 316 stainless steel that reduces the number of joints and whose interior is fitted with a helicoidal feature that forces the gas stream through
112. ndensates in the orifice Dyna Pak gasket which ensures the tight sealing of the rod without excessive compression of the same Construction material 316 Stainless steel Dead volume lt 0 2 ml Connections 1 8 Original orifice Replaceable in 316 stainless steel The need to operate in the proximity of the close contact between the orifice and the needle inevitably leads to wear on the needle caused by rubbing Consequently the disc containing the orifice on these valves 5 mm diameter 1 8 mm thickness and orifice 1 19 mm has been replaced by a replica made of PEEK polyetheretherketone a chemically inert material that has an excellent mechanical performance withstanding high operating temperatures and featuring self lubricating properties with great hardness and resistance to distortion properties The disc may be replaced as often as necessary if it has been distorted by continuous use of the valve The manufacturer s original Cy curve may be seen in Figure 4 27 Modification of the orifice on the valve and its replacement with another made of PEEK alters its Cy curve near to the closed position Experimentally an excellent regulating performance is achieved in Cy scenarios of 10 that is the modified valve accurately regulates flows of even 40 or 20 ml min with pressures of 60 to 90 bar 48 PID EngaTech 3 STEM 047 ORIFICE NUMBER OF TURNS OF VALVE HANDLE 002 004 006 008 O10 012 014 O16 0
113. ns GAS 6 GAS 5 GAS 4 GAS 3 GAS 2 GAS 1 Figure 7 2 4 The MFC installed in the equipment has to have the same characteristics as the one being replaced check enclosed MFC specifications Mass Flow Controllers HI TEC by BRONKHORST model EL FLOW IDENTIFICATION No F 211C FAC 11V Figure 7 3 136 Enga Tech gt Model number identification F N N NAA NNN A A A NN A Base Valve anty Nominal range Mater Factory selected 2 Contraller Communication 140 T Supply voltage Pressure rating Y A R amp 232 analog ne control B 24 Video DeviceNet B4 bar B AS232 analog n a control D ri 28 Vde analog 1 100 bar D RS5232 DeviceMet nic control FLOW BLS Profibus Modius 2 200 har E R amp 5232 DeviceNet mo control 3 400 bar M Riz532 Modbxus RTU vc contml Connections md out N AS232 Modbus ATU nto control 1 Ve OD compression type Ranges P AS232 Profibus DP ntc control 3 CH OD compression type for PNGa PNTOO Flow Meters Controllers R5232 Profibus DP nto control 3 amm OD compression type DZ 0 0 7 20 8 ml min R Haan FLOW BUS dc control 4 12mm OD compression type 18 104 Q 8 0 254000 ml min 5 R5232 FLOW BUS Go control 5 Wa OD compression type TAC TAV 0 20 0 ID l min B 20 mm OD compression type 2AC 2AM Q AD 0 250 min Analog output Y H prd Face seal male 3AC IAM O 200 0 T amp 70 Limm A 0 5 Vdc El other B 0 T0 Vde for PH200 PNAOD F
114. o a value of P 896 96 F S If this is the first time this process is initiated precautions may be taken such as increasing this value with a view to overdamping the system and in addition carrying out the system s first start up below a hazardous position remembering that the offset in this system is unknown and may equally be positive or negative The application of this procedure to any kind of system may allow for foreseeing the suitable value of P by simply sensing when the controller should begin to change its control outlet so as not to overrun the order An interesting possibility for advanced operators is to perform this initial trial and error on the value of P with a high value of integral action which will avoid the offset phenomenon without affecting the stability of the solely proportional action This high value of integral action should correspond to for example 2 or 3 values of the oscillation period which for rapid systems pressure flow level etc will correspond to 20 60 s and for slow systems temperature pH in 25 PID Enga Tech buffered solution etc to 200 600 s It tends to be relatively easy to deduce a system s period of oscillation by bearing in mind the characteristics of the same Once the system has been started up with this estimated value of P in all probability following one or two trial runs around the set point the value of Pc is found whereupon the critical oscillation period will
115. on lt with water at 1 mL min and pressure gt 9 MPa Dampener volume 0 6 mL at atmospherk pressure 15 mL at 60 MPa Via Gilson UniPoint System Software Fe 232 or GSIOC four inputs and four relay outputs 2 x 24 character LCD Keypad and built in help messages 316L stainless steel titanium sapphire ruby PTFE PCTFE and HDPE Frequency 50 50 Hz Voltage 100 120 or 220 240 mains voltage fluctuations not to exceed 10 af the nominal voltage AUC Meets applicable Safety and EMC certification standards CE certified 33x33x 15 cmilix 13x6 in 11 5 kg 25 4 Ibs 154 kg 34 Ibs 4 6 1 4 Switching on the pump Before operating the liquid pump the electrical and mechanical installation of the system needs to be performed at this point it is advisable to consult the pump s user handbook When the pump is switched on the switch is to be found on the rear the screen displays a message indicating the model of the pump as well as the version of the control software as shown below Pump Model 307 V x xx Following this message the pump s main operating screen is displayed 4 6 1 5 Setting up the pump Once the electrical installation is completed as described in the chapter 3 2 3 of this manual it is necessary to configure the pump if the MA Ref reactor includes the pump it is already configured at PID Eng amp Tech laboratories so it is not necessary for the customer to do it again Setup pump hardware
116. on return valves and if necessary replace Check the alarm and reset it providing the situation that triggered it has been resolved 143 PID Enga Tech The reactor s thermocouple has not been Verify the thermocouple s connector inside connected properly the hot box The reactor s thermocouple is not Replace the reactors thermocouple with working properly another of identical characteristics Disconnect the equipment switch the Poor connection of the thermocouple s circuit breaker to OFF unscrew the left There is no temperature reading in the reactor bed damping cable on the 18 pole wire hand side panel on the equipment and housing check the connections to the 18 pole wire housing The reactor s temperature reading The TOHO reaction temperature Introduce the factory set default parameters eg controller has been configured in the controller If these are not known IS Incorrect bu incorrectly olease contact the distributor Restore the optimum control parameters see the section The controllers in this manual Control mode has been set to manual Set to automatic Run in the controller s or Rdy instead of to automatic _nd parameter An alarm has been triggered in the system that has shutdown the reactor oven oven not fully closed door open on hot box The parameter _EH1 on its controller Re set the value of parameter EH1 to 40 has been modified Temperature above
117. on the Verify all the liquid inlet lines on the system PID Enga Tech These sockets are not energised when the equipment is switched off plug the pump into another socket separate from the unit or switch on the equipment Change the fuse See the section Electrical installation in this manual Turn the switch on the rear of the pump to the l position Reboot the pump If this is not possible control of the same is to be maintained in manual mode Reboot the pump If this is not possible control of the same is to be maintained by digital communications through the Process software Pressure must range 10 15 bar in the pump head Install a backpressure prior to the inlet on the liquid non return valve Only feed liquids when the operating oressure is above 10 15 bar Check the alarm and reset it providing the situation that triggered it has been resolved Pressure must range 10 15 bar in the pump head Install a backpressure prior to the inlet on the liquid non return valve Only feed liquids when the operating pressure is above 10 15 bar There is no liquid in the pump tank Fill the tank with the reactant liquid Set the valve to the suitable position see the section Venting the pump in this manual or in the pump manual Check the alarm and reset it providing the situation that triggered it has been resolved Replace the evaporator Verify the status of the n
118. ons from session number one The number of the experiment will appear then on the left bottom corner of the window To stop data acquisition click on the STOP icon in the tools bar or in the Acquisition menu Every time the acquisition stops a file named after the experiment will be saved View By introducing the number of a session in VIEW the scroll bar will move in order to bring it to the middle of the table Launch lt launches the session entered in the cell above the button Sessions Table The session name and time can be introduced in this area The following options can be configured Q Alias Session name Q Description Short session description start stop etc Session Duration In seconds Next Session Number of the session with which the actual session wants to be linked In order to connect two sessions both sessions need to have a time value Device Table n this area the parameters of the Microactivity Reference devices are displayed When opened only the main parameters for each device are shown but all the parameters can be displayed by pressing on Show All By clicking on Show All all the designable parameters are displayed The ones with a red cross don t appear in the short display when Show all is deactivated Select any parameter by clicking on its name so that they are activated in the table The cross will turn into a green tick Y which indicates that the parameter will be shown
119. operating conditions modifying the total gas flow it would be necessary to change the maximum number of turns If the gas flow increases and the valve has to open up to 70 75 for controlling the desired pressure it would be advisable to increase the number of turns If the gas flow decreases and the valve opens just 5 15 for controlling the desired pressure it would be advisable to decrease the number of turns It is recommended that the valve opens from between 20 to 65 for controlling the desired pressure For changing the number of turns proceed as following Locate dip switch S8 of the driver see Figure 4 29 Check that the switch 4 on dip switch S8 is in the Off position see Figure 4 29 The number of turns is determined with switches 1 2 on 3 on dip switch S8 Turn off the unit With the help of a screwdriver change the position of the switches 1 2 and 3 according to the table above Turn the unit on again The valve is now configured with the new number of turns 92 PID Enga Tech 4 6 3 LEVEL CONTROL IN THE LIQUID GAS SEPARATOR 4 6 3 1 Introduction to level control in microactivity reactors In those systems in which the aim is to monitor the reaction in real time continuous collection has to be made of the condenser liquid in the liquid gas separator for its subsequent analysis In the reactor operating at atmospheric pressure the removal of condensed liquids in the se
120. or with a very low dead volume With this system when liquid is present between the isolated probe and the chassis on a metal tank this liquid behaves as a dielectric altering the electrical capacity of a condenser system An RC oscillating circuit such as the one shown in Figure 4 30 will then provide a frequency signal proportional to the system s capacity and which is therefore proportional to the amount of liquid in the tank Without considering geometric issues in the design of the tank this circuit s output signal will be directly proportional to the height of the liquid in the tank ee sU q e Sz Umbral 1 2 R4 Vi Umbral 0 RC Oscillating Circuit Oscillating Circuit behaviour Figure 4 30 This system s output signal is also proportional to the dielectric constant of the substance that acts as the dielectric Accordingly the greater the difference of dielectric constant between the process liquid and the air or gas that occupies the space not taken up by the liquid the greater the output signal the system will generate The capacitive level sensor used is inserted through the upper part of the liquid gas separator described in section 4 3 of this manual and consists of a 3 mm diameter probe that is 53 PID Enga Tech electrically isolated from the rest of the system by means of elastomer type seals chemically compatible and withstanding pressures of up to 400 bar The design of the liquid gas separa
121. ouse over the graph a cross shaped cursor appears This cursor will jump from one variable to another the mouse is moved On the upper part next to the icon the name of the variable and its value at a time will be shown both for the process value graph and for the output graph EXP1 File zoom Tools qM a f d Er Ge PAJA O d e TY EDT B mmm pum SEE deu Figure 5 50 Cursor function 126 PID Enga Tech To exit CURSOR click again on the icon 5 5 4 How to change the color and scale of the graphs By double clicking on each line a wndow named PLOT DATA will appear on the right upper corner of the graphs In this wndow Y axis scale and the colour for each variable can be changed Also hide or show a variable Go from one variable to another clicking on the arrows situated below this window The Y axis scale will be that of the one whose name appears on the cell NAME of this window Hide show graph Mame Color Variable name Pup Maximum Minimum 5 0 Han Arrows for changing from one variable to another Limits of the scale Figure 5 51 Graph configuration window To hide or show a graph activate the tick situated on the cell situated on the right upper corner The colour of the graph can be changed clicking on the coloured square This action will pop up a color palette ME LI nanaaannnaanaaannag History ajaja ajajaja MOMO EN 2 2556 368 o Figure 5 52 Colour palette 5 5 5
122. parator has to be performed manually by an operator but this procedure is not possible in equipment that is operating at pressure higher than atmospheric because the loss of the hydraulic seal on the liquid products at the bottom of the separator would lead to a major leakage of gasses into the atmosphere and possibly cause an accident In this case the liquid gas separator has to have a control loop at a specific liquid level A control valve is operated to maintain the liquid level constant continuously removing each new drop that is formed in the separator Other commercial systems applied in pilot plant situations base this level reading on systems that record the differential pressure between the ends of the separator Thus the pressure at the base of the separator is that corresponding to the pressure in the installation plus the pressure corresponding to the height of the liquid column present in the separator Yet this technique presents serious problems when it is used in the measurement of a microvolume the errors inherent to this technique when measuring the level of a tank that collects the condensates in a system that increases at the rate of for example 0 05 ml min renders this technique unviable for use in a reactor for studying catalytic microactivity 4 6 3 2 The capacitive level sensor With a view to resolving the problems posed in systems of this kind a liquid gas separator has been designed with a capacitive type level sens
123. pend on the sample time the shorter the time the bigger the size of the files will be E Set Sample Time Insert Sample Time seg Figure 5 15 Sample time setting Panels The next function Panels allows the opening of the Microactivity Reference diagram in which the flow diagram can be seen as well as the different devices controllers alarms indicators etc From this menu the user will also be allowed to change the name of the panel 103 PID Enga Tech Q Sessions In this setting a session table for the experiment can be configured so that each session is a step of the experiment In this table the times for each session and the devices parameter values must be specified Graphs In this function the Process Value Graphic and the Output Control Graphic which show the progress of the experiment can be opened Experiment Viewer Through the experiment viewer the graphs of previous or current experiments can be seen and configured 5 3 2 THE CONTROL PANEL The control panel appears in the screen every time a project is opened If it is closed or hidden it can be reopened or taken to the front by selecting Open Panel in the tools bar The variable values can be viewed and modified from the control panel These different choices can be selected by right clicking the mouse on the different devices The message bar at the bottom of the screen shows messages related to the panel state and its operating
124. re of the head close to operating pressure No liquid is entering the reactor Pressure of the head significantly above operating pressure The pump is connected to the 220V sockets on the rear of the equipment rear panel has blown or is missing The pumpss electrical installation has not been performed correctly The on off switch is in the 0 position If a prior manual control has been made on the pump s display it is not possible to establish digital communication with the PC and vice versa If a prior digital communications control has been made between the PC and the equipment it is not possible to perform manual control on the display and vice versa No backpressure has been installed and operation is at atmospheric pressure Vent the pump releasing the liquid inlet line There is a leak in the system s liquid inlet An alarm has been triggered in the system that has shutdown the system s liquid inlet No backpressure has been installed and operation is at atmospheric pressure The 3 port valve on the pump is not in the normal operating position injection from the tank An alarm has been triggered in the system that has shutdown the system s liquid inlet A blockage of solid deposits has formed in the evaporator Faulty operation of the liquid non return valve An alarm has been triggered in the system that has shutdown the system s liquid inlet The 3A 250V fuse in the fuse box
125. rol always must be introduced in the cell MV1 of the Design window or in the session s table The upper limit of the alarm AIHi which is the same as the controllers E1H can also be introduced from the Design window This value will trigger the configured alarms see 4 5 2 C ON OFF DEVICES These displays are associated to the units ON OFF devices These are devices which only have two options either ON or OFF This is the case for the door the bypass the Peltier cell for the liquid gas separator and the auxiliary buttons S1 S2 and S3 on the touch screen 108 PID Enga Tech ON OFF DEVICES ON Open OFF Close Bypass ON Activate yp OFF Deactivate OFF Deactivate DCN S NN OFF Deactivate Table 5 2 Configuration of ON OFF devices When configuring these parameters at the sessions table ON is equal to 1 and OFF is equal to 0 These displays look like a clear green button when they are ON and a darker green button when they are OFF Bypass E Figure 5 22 The design window for these displays allows for choosing between both options na s Figure re 5 23 ON OFF device design window d INDICATORS In this type of displays a value is shown but it cannot be designed by the software since they are just indicators By right clicking over the display it can be renamed TIL Lo Figure 5 24 e HEAT GC LINE This device allows for visualizing the control output on the upper window and seeing its s
126. rometric regulating valve that registers the same temperature as the hot box and which provides a continuous and constant flow of gases at the outlet In those systems that are not fitted with the optional pressure control this flow goes straight to the outlet Once pressure control has been performed the flow of reaction gases is directed out of the hot box for subsequent measurement and or analysis by means of a system of for example chromatography in gaseous phase The Microactivity Reference unit is fitted with a system of local control and remote control based on communications via Ethernet by means of the Process control application The equipments safety system is integrated within a microprocessor that is separate from the computer Accordingly the alarm signals from the various control loops are centralised in the microprocessor which operates as programmed to do so with respect to the system s different alarm situations These actions are triggered on a self contained and immediate basis independently of the communications with the computer thereby upholding the system s safety as it not only continues operating in the event of failure in the computer system but in addition its safety system remains operative The operation and configuration of the safety system are described later on in this manual PID Enga Tech 2 2 SPECIFICATIONS Frequency 60 50 Hz 1 Maximum power consumption of Hot Box heaters 4 heaters of 165 W
127. s a list of previously saved sessions appears Session Table Selection Figure 5 38 Loading a sessions table 5 3 4 4 How to print a Sessions table Print a sessions table by clicking on Print in the sessions table menu Printing is allowed in two different ways to print on a configured printer Print to printer or to a file in htlm format Print to File 118 5 3 PID Enga Tech HOW TO CARRY OUT AN EXPERIMENT To carry out an experiment remember to follow these steps a First check Process communication parameters Make a Communication test Project 2 Communication to check whether Microactivity and PC are correctly linked Secondly in the function menu select Microactivity project under Open Project The window with the flow diagram of the unit shows on the screen If any changes on the panel are made save the changes by clicking on Save Panel in the same menu which is displayed by right clicking If the unit is going to be operated without sessions introduce all the values into the touch screen and into the controllers The progress of the experiment can be followed by pressing the start icon in order to acquire data If the experiment is going to be carried out with a sessions table as the example shown in Fig 5 36 it is advisable to follow the following recommendations I EMETLA TE TIE TET session Time ae Alias Pescripliun wssionlime seq v PRESSU
128. s parameters and mode control auto or manual can be set in the MISC SETUP screen If the unit incorporates the thermocouple for this option the temperature loop control is shown over the S2 button 3 Additional control options for special configurations of the unit PELTIER Cooling heating of the liquid gas separator The peltier configuration can be done in the PELTIER CONTROL menu of the touch screen where the user selects the action cooling heating and the desired output control for regulating the separator temperature If this function is deactivated the separator will be at ambient temperature A display on the upper part of the tank shows the read out for the liquid level in the liquid gas separator expressed as a percentage of the total volume of the tank if the level sensor has been installed in the equipment This value cannot be modified manually by the user ALARM Consultation and deactivation of the system s alarm When an alarm is triggered in the system the icon Alarm will begin to flash accompanied by a buzzer By pressing on this icon the alarm panel will be displayed see Figure 4 9 where the cause of the alarm may be consulted the icon that is flashing and deactivated o RESET BUZZER button for deactivating the buzzer o RESET ALARM button for deactivating the alarm provided that the situation of risk that triggered the alarm has been corrected in the system PA HE Le AL AEM Maia las ARR
129. s have been preheated and liquids evaporated these streams merge and flow to a 6 port valve This valve is operated by remote pneumatic control through the computer or by means of the touch screen and allows for selecting from two possible alternatives for the flow path either towards the reactor or rerouting it towards the system s gas outlet by passing the reactor When the flow of reactants is directed towards the reactor it passes through 10 um sintered filters made of 316 stainless steel at both the inlet and outlet of the reactor thereby protecting the arrangement of valves from possible finely separated catalyst particles At the reactor outlet and after passing through the 6 port valve the reaction products pass out of the hot box to the liquid gas separator that may be fitted with a high resolution capacitive level sensor This system allows the condensation of liquids at low temperature In the standard series unit the liquids accumulate inside the condenser and need to be removed manually by the user If the option has been chosen that includes the level control system in the separator this removal is performed automatically providing samples of reaction liquids within extremely short periods of time without accumulation or dilution over time The upper part of the separator features the outlet for gases which are reintroduced into the hot box and are directed to the pressure control system consisting of a servo positioned mic
130. s possible to include a calculating device TOTALIZER in monitoring Process software Gas outlet Mass flow meter Coalescing filter Figure 4 42 66 PID Enga Tech As in option B scale mass flow meter option makes easier calculating mass balance Coalescing filter prevent moisture at the mass flow meter inlet Maximum flow of mass flow meter have to be introduced in mass flow setup menu Ee e E Ewe el Eet e uk Figure 4 43 MFM value is shown in PVgraph and touch screen as shown below Figure 4 44 67 PID EngaTech OPTION C MASS FLUW METER amp CUALESCENT FILTER LIQUID HU Great Ceri Brra55 VALVE amp PORT 2 POS GAS OUTLEJ gt LC VUE VU OPTIONAL Lig OUTLED 68 PID Enga Tech 4 7 4 OPTION D ADDITIONAL 6 PORT VALVE Additional six port valve Figure 4 45 One 6 port valve is installed in the Basic Unit Additional 6 port valve is installed with one of these purposes chosen by the user e By passing the L G separator This option can be useful when there is no need to pass the reactor products through the L G separator For example liquids are not pumped to the reactor only gases e Selecting the reactor flow UP DOWN Figure 4 46 69 PID Enga Tech OPTION D 2nd AUTOMATIC 6 PORT VALVE TO L G SEPARATOR BY PASSING LIQUID 1 C 3X Cl i l GB HOT BOX TE i1809c TE we
131. sign window b CONTROLLLERS The display representing the TOHO controllers placed in the unit s front panel Reactor TEMPERATURE HOT BOX TEMPERATURE PRESSURE LEVEL and auxiliary controllers AUX1 AUX2 if they have been installed has three cells one where the set point is shown a second one for the process value and a third cell for control output REACTOR Device name Acquisition alarm indicator 0 Set point Process value 0j Output control signal Figura 1 Controller s icon In order to modify the controllers parameters from the panel right click on the icon The controller parameters that can be modified are the following 107 PID Enga Tech Fl To operate in manual SWI 450 RP1 D E mode tick on Manual PL 40 MH1 30 m and introduce an output control MV1 n 360 ML1 0 Dif is SM aoo Pbb 0o Sat AR 800 S Figure 5 21 Design of a controller window The set value and the controller ramp can be modified in the upper part of the display Under these values some additional parameters are shown CONTROLLER S PARAMETERS Pbb Manualreset Table 5 1 Design parameters of the controllers The controller can operate in automatic mode or in manual mode In order to work in manual mode activate the option in the Design window of the controller see Fig 5 20 or 1 in the parameter MD in the session s table see 5 3 4 1 In manual mode an output cont
132. sly without responding to its set point The maximum and minimum levels of oscillation set in the calibration of the sensor have been modified The sensor is dirty PID Enga Tech On the level sensor s touch screen restore the values obtained in calibration If these are not available re calibrate the sensor see the section Calibrating the level sensor in this manual Dismantle the condenser and the sensor and clean them with ethanol compressed air The sensor has not been properly Check and properly adjust the sensor connected connection on the rear of the equipment Incorrect controller configuration Restore the controller to its original parameters The sensor is not working properly The level sensor is not connected to the board The TOHO level controller is not connected to the board The power source 15 15 5 is short circuiting power LED blinking or is faulted LED off If this occurs there will be no level reading if the equipment is fitted with this option The maximum and minimum levels of oscillation set in the calibration of the sensor have been modified The sensor is dirty The controller s PID parameters have been modified Control mode has been set to manual or Rdy instead of to automatic The sensor is dirty The valve s zero setting has been modified Replace the level sensor contact the distributor Disconnect the equipment switc
133. st as a thermoelectric couple generates a difference of potential when its connections register different temperatures Siebeck effect when a difference of potential is applied to the thermoelectric couple a difference of temperature is generated between the connections Peltier effect The application of a 15 VDC difference of potential and a 3 A current in the Peltier cell generates a temperature difference between the panels of approximately 30 C If a forced convection heat sink is used to bring the temperature of the hot panel to 25 C then and to uphold this temperature difference of 30 C the temperature of the cold panel must fall below 5 C and when placed in contact with a metallic block temperatures of around 0 C will be achieved in that block The cooling of said container may be activated in two ways Via the main screen of the touch screen see section 4 5 1 of this manual Via the process control software see section 5 5 3 of this manual Regarding equipment that is not fitted with a level control in the separator the removal of the condensed liquid is to be performed manually 28 PID EngaTech 4 4 THE PRESSURE SENSOR FOR EQUIPMENT AT ATMOSPHERIC PRESSURE This device is only available in those pieces of equipment that operate at atmospheric pressure which do not include the pressure control option in the reactor chapter 4 6 2 in this manual Its purpose is to register the pressure drop inside the re
134. strongly recommended that you exit all programs before running this installer Applications that run in the background such as virus scanning utilities might cause the installer to take longer than average to complete Please wait while the installer initializes Figure 5 1 Process installer A window asking which directory Process is to be installed in will pop up next To ensure the right installation it is recommended to choose the default locations C Program Files Process C Program Files National Instruments Click Next gt gt to continue the installation V Processo Destination Directory Select the primary installation directory All software will be installed in the following location s To install software into a different locations click the Browse button and select another directory Directory for Process C Archivos de programa Process Directory for National Instruments products C Archivos de programa National Instruments Figure 5 2 Installation directories Next if accept the software license agreement is accepted first the National Instruments license will appear After selecting accept the License Agreement the installation process in NEXT can be continued 96 PID Engatech Y Process License Agreement You must accept the license s displayed below to proceed CONTRATO DE LICENCIA DE SOFTWARE DE NATIONAL INSTRUMENTS INSTRUCCIONES PREVIAS A LA INST
135. suitable level of intrinsic immunity ability to operate without detriment to quality in the presence of a magnetic disturbance that enables it to operate in accordance with the purpose for which it was designed Figure 8 1 The Microactivity Reference unit complies with Directive 98 336 EEC having passed all electromagnetic compatibility tests required by the same Figure 8 1 shows pictures of the Microactivity Reference unit in the anechoic chamber where part of said tests were carried out 4 Directive 2006 95 EC Low Voltage LVD Electrical Safety former 73 23 EEC This declaration is based on the full compliance of the equipment with the Harmonized Standard EN 61010 1 2001 for Safety requeriments for electrical equipment for measurement control and laboratory use Part 1 General requeriments approved by the approved by the European Committee for Electrotechnical Standardization CENELEC 140 PID Enga Tech 9 ENVIRONMENTAL POLICY Process Integral Development Eng amp tech bakcs the environment focusing its activities towards the minimization of the impacts to surroundings with the commitment from management to follow the principles included inside the policy The different devices and operations with relevant environmental injuries have been described in this manual porous plates filters o rings solvents and main board battery PID Eng amp tech ask the final user to be responsible with the environment
136. sure control system Range of operating pressures atmospheric 100 bar Control accuracy 0 1 bar Variations in gas flow at the reactor outlet 596 Maximum heating temperature of the valve 200 C the valve is inside the hot box see Figure 2 4 Pressure control is carried out by means of the TOHO TTM 005 controller that is to be found on the front of the reactor see Figure 2 3 and its operation is described in section 4 2 of this manual 49 PID Enga Tech 4 6 2 3 Configuration of the Servo Digital V4 0 unit microstep positioner The Servo Digital V4 0 microstep positioner that is a part of the pressure and level control systems on the Microactivity Reference units is factory set with the optimum parameters for the equipment correct operation which means that the end user should not need to configure this unit In case that the customer needs to modify these parameters here we include a detailed description of the printed circuit in the microstep servo digital unit Access to it involves unscrewing the metal plate on the right hand side of the reactor as shown in Figure 4 28 OPEN CLOSE S6 ADDRESS J6 ANALOG INPUTS e ens S1 ZERO J4 ZERO SENSOR POTENCIOMETER LED S J7 RS 485 2 S3 S4 ANALOG J3 MOTOR INPUTS CONFIGURATION mp r gt IC E Ge J2 15VDC AUX il a P 3 a ast BE cau E S A ilele rs MS CR us afafa L ha Ze c S J1 15 VDC jo we INPUT qune E R17 MOTOR is z
137. t commonly used criteria for determining control stability are the following A Criterion of minimum area or of damping ratio This is the criterion of widest application especially regarding processes in which the duration of the deviation is as important as the value of the same According to this criterion the control is to ensure that the area of each oscillation in the control output signal following a disturbance is minimum experience shows that stability criteria should be applied onto this signal and not on the process variable In other words to achieve a minimum error in the shortest time possible Experience in industrial control processes indicates that this area will be minimal when the proportion between the peak to peak amplitudes of the first two consecutive cycles immediately following the disturbance is 1 4 In other words the damping ratio between these consecutive peaks must be 25 lt is a compromise criterion between stability in the controller s response and the speed or rapidity with which the manipulated variable returns to a stable value Proportions percentage higher than 25 gives greater stability but they lengthen the time required for attaining stationary state Proportions percentage lower than 25 may reduce the time it takes to reach stationary state but they cause instability in the system B Criterion of minimum amplitude The control system is to keep the amplitude of the deviation to a minimum
138. t either Process Value Graph or Control Value Graph During an experiment execution they can be closed and reopened again by using this menu 111 PID Enga Tech E Process Value Graph A p 1 1 1 1 1 1 1 1 1 1 1 1 3 00 00 00 00 10 00 00 20 00 00 30 00 00 40 00 00 50 00 01 00 00 01 10 00 01 20 00 01 30 00 01 40 00 01 50 00 02 00 00 Time scatg2 pump T GAS1 N2 GAS2 AIR GAS3 H2 HOT BOX LEVEL L GSEP Ml PRESSURE 2200 HiN L 3 10 Haw COI 500 mal CC 400 HA COI 400 Ha COI 600 HiM 40 Ha COI 600 Him CI 100 HN CH 2395 Low 2050 Lon L 3 0 Long toil o0 toro o tonal 0 LOMO 20 LOMO 0 LOMO 0 toa CI ilo 2083 5 jo 100 4 so so 79 TET 27 oi Figure 5 30 Process value graph The displays representing the devices that are in the panel can be seen in the screen s lower section In each display the following characteristics of each variable are shown device s name its color in the graphic two values indicating the device s range two alarm gauges or indicators high and low and a tick that hides or shows the graph when clicked on In the lower section the last real value read is shown in a white cell VARIABLE NAME GRAPH COLOR HIGH AND LOW LIMITS OF THE SCALE HIGH AND LOW ALARM LIMITS PROCESS VALUE Figure 5 31 Variable s Configuration To configure the scale the color and the alarm values right click over the desired control and select the Config option A window will op
139. take an action that would have corrected the error earlier a situation that is clearly never desirable Therefore low values of are damaging and high values of albeit not damaging are not convenient But if the value of in these pilot plant systems is adjusted to the period of oscillation the situation resulting from a significant change in a process variable or set point in which the system s gain becomes more pronounced and therefore a change occurs in the system s period of oscillation could lead to process instability as the time spent in calculating the area of this new situation has not been sufficient to allow for the compensation of the positive and negative areas of this oscillation Thus for this type of systems it is advisable to select a value for parameter that is higher than the critical oscillation period Tc 1 2 Tc Concerning the derivative action and always bearing in mind how problematic its use is for non advanced operators the option should be taken not to use it in rapid systems the gains on pilot systems are very high due to the immediate response to a disturbance as a result of their low damping capacity For systems that evolve slowly and due to their nature of overtaking the process s evolution relatively narrow values improve systems response to overshoot phenomena during start up procedures Thus for systems in which these phenomena are frequently repeated during the operating proced
140. tate On with a light green and OFF with a darker green on the lower part HEAT Figure 5 25 The output control and the HEAT COOL mode must be configured in the touch screen 109 PID Enga Tech As explained in 4 5 2 Main Menu HEAT is configured in the touch screen in MISCELLANEOUS SETUP The operation mode can only be selected in this menu by pressing the button HEATER MANUAL and change it to HEATER AUTO If it is in manual mode it will be necessary to introduce an output control in the design window or in the sessions table parameter M1C whereas to operate in automatic mode a set point must be introduced in the touch screen of the Microactivity Reference see 4 5 2 To configure this device proceed as follows Q Select the operation mode in the menu MISCELLANEOUS SETUP of the TOUCH SCHREEN Q If HEATER MANUAL has been selected it is possible to activate or deactivate it from the sessions table introducing 1 or O respectively in the parameter M10 or from the control panel ON or OFF The output control 0 10096 can also be introduced from the table parameter M1C or from the control panel a If an automatic control is preferred select HEATER AUTO in the menu MISCELLANEOUS SETUP and introduce a set point in the touch screen the output control is not required now To use this mode it is necessary to connect a thermocouple in the TI1 of the back panel In this case HEAT can only be activated and deact
141. te a temperature range of 20 C to 60 C and a range of pressure between 0 8 bar and 1 1 bar as a basis for design and intended use of products Consequently the Microactivity Reference unit is not designed for operating under potentially explosive atmospheres but as a result of improper use of the unit or a lack of maintenance of the same the unit could generate a potentially explosive atmosphere It is the responsibility of the end user to assess the risks implement suitable safety and protective measures as well as locate the equipment in special laboratories with inflammable gas 139 PID Enga Tech detectors in order to reduce to a minimum the risks stemming from operation of the equipment The Microactivity Reference unit caters for connection to an external alarm that would trigger the unit s secure shutdown 3 Directive 2004 108 EC Electromagnetic Compatibility Directive EMC The Microactivity Reference unit as per Directive 98 336 EEC of 3 May 1989 is considered to be equipment that may cause electromagnetic disturbances or whose operation may be affected by said disturbances given that it is a piece of equipment or installation that contains electrical and or electronic components It is therefore to be constructed in such a manner that The electromagnetic disturbances generated are limited to a level that enables the apparatus to operate in accordance with the purpose for which it was designed The apparatus has a
142. that the device and the radio or television are on separate d Make sure that all peripheral devices are also certified e Make sure that appropriate cables are used to connect the device to peripheral equipment f Consult your equipment dealer Process Integral Development Eng amp Tech or an experienced technician for assistance g Changes or modifications not expressly approved by Process Integral Development Eng amp Tech could void the user s authority to operate the equipment 2 DESCRIPTION OF THE EQUIPMENT 2 1 GENERAL DESCRIPTION As may be observed in the P amp I diagram shown in Figure 2 1 the system consists of a fixed bed tubular reactor with the catalyst bed placed inside upon a porous plate The flow inside the reactor is up down whereby the reactant mixture is fed through the upper part of the reactor and the reaction products are obtained through the lower part E P F3 T m i eS m LX E f Pe HOT BOX FAM f i i E Ls MAX iare en Ve i OPTIONAL REACTOR MOC 1 TROU manaa ihe APC Mew TRIC EX HAST Cam te BBC Has PDC leen ia MAST X lite BE Man PE vli ETA A gt OPTIONAL INTERNAL DIAMETERS Hiren standard TX hea 1 mel im MANUAL OPERATED VALVES El MANUAL OPERATED BALL VALVE a esses DAC PRISSIHE WAL WT 0 ACTUATED VALVES EM VICI PORTRPOSITION VALVE E a EOL LDD VALT METALMENT E FAE MASS FLOW CONTROLE MST
143. the strands on this propeller encouraging their mixing see Figures 4 67 and 4 68 88 O le Engatech Figure 4 63 GAS MIXER lt 170 gt SS 2C2 1 10 NPT 1 8 lt 30 m NPT 1 8 NPT 1 8 a Figure 4 64 Reactor filters SG SS 2F 15 Located on the reactor s gas inlet and outlet lines 316 type stainless steel 1 8 pipe connections Porous panel of 15 um SS316 4 8 3 INSTRUMENTATION Pressure transducer SWT A08 89 PID Enga Tech lt 0 1 FS IP65 connector IP67 cable EN 50 081 1 and EN 50 082 2 Table 4 6 Mass flow meters and controllers F201C FAC 11 X A study has been performed on the features of different mass flow controllers in terms of their reliability accuracy control valve design operation in the lower run of the operating range and performance at high pressure with the instruments made by the firm Hi Tec Bronkhorst being selected as those best suited to a Microactivity reactor Each controller is calibrated to perform the measurement of a specific compound although the option exists to use them with compounds of a different factor to the unit s original calibration When using another gas special attention is to be paid to the elastomer s compatibility with the new process gas Calibration at source is undertaken by means of equipment with NMI certification The specifications of these ins
144. ther an individual or a single entity and Microsoft Corporation for the Microsoft software identified above which may include computer software associated media printed materials and online or electronic documentation SOFTWARE By downloading installing copying or otherwise using the SOFTWARE you agree to be bound by the terms of this EULA If you do not agree to the terms of this EULA do not install or use the SOFTWARE The SOFTWARE is protected by copyright laws and international copyright treaties as well as other intellectual property laws and treaties Microsoft or its suppliers own the title copyright and other Uimtellactuel nenmartrz nichte im the SETI S RE The GOFTW ARE Ze Heoncod nat cold O accept the above 2 License Agreement s 9 do not accept all these License Agreement s Figure 5 4 Microsoft Licence Agreement Once the license conditions are accepted Process installation will begin in the next screen Start Installation Once completed a message will appear in the next window Figure 5 6 97 PID Enga Tech S Process Start Installation Review the following summary before continuing Adding or Changing Process Files Click the Next button to begin installation Click the Back button to change the installation settings Figure 5 5 Beginning of Process installation v Processo Installation Complete The installer has finished updating your syst
145. ting temperature 800 C Low thermal inertia Automatic opening system with temperature warning system The entire system is contained within a hot box made of 304 stainless steel which interior holds an electric convection heater Its maximum recommended operating temperature is 190 C 19 PID Enga Tech 4 2 THE CONTROLLERS 4 2 1 THE REGULATION PARAMETERS The Microactivity Reference unit uses P I D controllers for the following control loops Reaction temperature The signal from the thermocouple located in the catalyst bed is analysed by the controller whose output signal is relayed to a solid state zero switching relay that regulates the power supplied to the oven proportionally to the control signal The power the oven receives corresponds to a signal between O and 200 VAC typically between O and 140 VAC proportional to the control signal Hot box temperature The signal from the thermocouple located inside the hot box is analysed by the controller whose output signal is sent to a relay that regulates the power supplied to the box s heater proportionally Pressure control The signal from the pressure transmitter installed upstream of the reactor is analysed by the controller whereby its output signal determines the position of the pressure control valve Level control The signal from the capacitive level sensor installed in the liquid gas separator is analysed by the controller whereby its output signal
146. tinuously This value of P receives the name of ultimate proportional band or critical proportional band Pc Measurement is now made of the period of these oscillations Tc in seconds that is the time that elapses between two consecutive oscillations when the system is at its critical proportional band The controller parameters that will produce a response with the 25 damping ratio are calculated as per Proportional band 1 5 Pc Integral action s 0 5 Tc Derivative action s 0 1 Tc The optimum selection of the controller parameters is always a compromise solution and one that depends on the skill of the operator Thus for a process in which there is a considerable transport delay it will be advisable to use high values of the proportional band On the other hand high values of P imply considerable sluggishness in the system s response to external disturbances or those of the system itself Typical values in semi industrial processes for the P and D control parameters are Fast systems pressure flow P 0 25 l 1 120s D 0 10s Slow systems temperature P 0 50 60 600 s D 2 60s 4 2 3 2 Method of trial and error This is carried out with the controller and the process operating in standard mode The general procedure basically involves starting up the process and performing repetitive tests on each control action beginning with the proportional band introducing disturbances by changing 24
147. to be used in potentially explosive atmospheres Directive 94 9 EC on the approximation of the laws of the member states concerning equipment and protective systems intended for use in potentially explosive atmospheres in its chapter Article 1 section 4 lays down that The following are excluded from the scope of this Directive Equipment intended for use in domestic and non commercial environments where potentially explosive atmospheres may rarely be created solely as a result of the accidental leakage of fuel gas The guidelines on the application of Directive 94 9 EC of May 2000 state in their section 4 1 2 a that Equipment is only considered to be within the scope of the directive if it is intended either in whole or in part to be used in a potentially explosive atmosphere the fact that an intended potentially explosive atmosphere might be present inside the equipment is not relevant Furthermore indicating Products that are not designed for use under atmospheric conditions 1 do not fall within the sphere of application of Directive 94 9 EC even when an explosive atmosphere may form under atmospheric conditions during start up disconnection or maintenance This would form part of risk assessment on the part of the user and could lead to the specification of ATEX apparatuses for installation of a near by container 1 Directive 94 9 EC does not define atmospheric conditions The relevant standards indica
148. tor with level sensor incorporated is featured in Figure 4 31 where the parallelepiped piece may be observed as well as the electrical insulator and the probe that electrically insulated in this tank becomes the condenser s second plate The photograph of the assembly Figure 4 32 provides a detailed view of the piece that constitutes the system s electrical insulator and other parts in Teflon which besides guiding the assembly serve to eliminate the system s dead volumes The separator level sensor assembly is connected to a micrometric regulating valve that is connected to a microstep motor like the one used in the system s pressure control see section 4 6 2 of this manual which means that recording the level inside the tank and operating said valve allow for the removal and collection of liquids on an automatic and continuous basis in real time with a control accuracy of 0 01 ml As in the case of the system s pressure control system the Servo Digital V4 0 microstep positioner unit that includes the level control system in the separator on Microactivity Reference units is factory set with the optimum parameters for the correct operation of the equipment which means that the end user should not in principle configure this unit However frequent and continued use of the sensor may in time make it necessary to carry out the zero calibration of the valve or select the number of turns of the same In these cases the user is to pro
149. truments are as follows AISI 316L stainless steel 1 8 connections 1 F S accuracy 0 1 F S repeatability Operating range between 5 and 100 Operating temperature between 10 C and 70 C Input and output signal 0 5 vdc Temperature signal TC KIA ID 0600 HO K type thermocouple Inconel 600 mm in length mini male high temperature 220 C plug 1 5 mm diameter with temperature range between 200 C and 1250 C Presents derivation and hysteresis as of 900 C Class 1 tolerance as per standards IEC 584 2 1 5 C or 0 4 xT C Bypass valve VV AT36UWTY 6 Ports with 2 positions 1 8 Maximum operating pressure 1500 psig Maximum operating temperature 230 C Standard port diameter 0 75 mm 316 stainless steel Valcon T rotor material A actuator valve separation with AT60 high temperature actuator 90 PID Enga Tech 4 9 CONTROL OF PROCESSES AND AUTOMATION 4 9 1 CONTROL LOOPS FOR THE MICROACTIVITY REFERENCE The Microactivity Reference reactor uses closed loop controllers with proportional integral and derivative type re feed of the signal for the following control loops gt Reaction temperature control The signal from the thermocouple located in the catalyst bed is assessed by the controller whereby its 4 20 mA output signal is sent to a solid state zero passage type relay that regulates the power supplied to the oven in a proportional mann
150. ttons Open or Close are pressed the motor moves the shaft in 5 jumps Once this has been performed return the Z switch to the Off position The new zero setting will be saved in the memory S8 N turns selector 2 Z switch Valve zero point 1 P switch Potentiometer zero point Micro switch Close Micro switch Open e GR Dam KI m EST LII E IM481H Figure 4 29 To return to the initial default zero setting E turn of the potentiometer turn switch P on the dip switch S1 to On and then to Off The new zero will be set on the 2 turn of the potentiometer Turn off the unit Turn on the unit again Once the previous step has been completed open the valve 5 and check that the there are bubbles at the gas outlet If there are not the values for the valve s zero setting will have to be raised more open To set the zero point for the liquid valve the user has to follow the same procedure as the described before 91 PID Enga Tech e Selecting the number of turns S8 This parameter represents the number of turns that the valve will perform from 0 to 100 of the control output from fully closed to fully opened By default the pressure and level control valves on the Microactivity Reference are set with the number of turns that ensures optimum performance under the unit s normal operating conditions However if the user changes the
151. two folders containing the graphics data txt files in ASCII format with the data acquired during the experiment the alarms that have gone off and an html file where the sessions tables are kept Files with a txt extension are files in the ASCII format with columns separated by tabs These files can be opened with any text editor and with most spreadsheet programs which allows designing graphics with the data recorded These type of programs because they allow easy data processing There is also a file Alarm File txt in which all alarms are registered in case they have gone off during the experiment The first txt file is named after the experiment name the same as the folder s name As files are being created these files are named with the same name plus an added number which indicates the order in which they were created This way as with the experiments the files are being placed in order as they are created To change the name of an experiment it is advisable to do it through the experiment viewer whose menu allows for it Finally if a sessions table in the experiment is saved a HTML file is created with the data from the table This file can be opened with any Internet browser It can be also opened with a text file or a spreadsheet program that supports HTML files 121 MICROACTIVITY REFERENCE User Manual PID 3 5 5 EXPERIMENT VIEWER The experiment viewer is the last menu in the tools bar It allows for re
152. twork Connection and select Properties Choose Internet Protocol TCP IP click on Properties and press OK Local Area Connection Properties General Authentication Advanced Connect using HE AC om 10 100 Mini PCI Ethemet Adapter This connection uses the following items le Client for Microsoft Networks File and Printer Sharing for Microsoft Networks Blog Packet Scheduler Intemet Protocol TCP IP Description Transmission Control Protacol Intemet Protocol The default wide area network protocol that provides communication across diverse interconnected networks Show icon in notification area when connected Figure 5 9 Internet Protocol TCP IP Introduce the communication parameters 100 PID Enga Tech Internet Protocol TCP IP Properties ES You can get IP settings assigned automatically if your network supports this capability Otherwise you need to ask your network administrator for the appropriate IP settings Obtain an IP address automatically Use the following IP address IP address 182 168 D 1 Subnet mask 255 255 255 0 Default gateway 192 168 0 1 Use the following DNS server addresses Preferred DNS server Altemate DNS server Figure 5 10 Control PC Communication Parameters PARAMETROS DE COMUNICACIONES DEL PC IP ADRESS 192 168 0 1 T
153. ue of the variable will be actualized once DESCRIPTION OF THE CONTROL PANEL S DEVICES The different devices are represented by different displays depending of whether is a MFC a TOHO controller an alarm an ON OFF device bypass door Peltier cell auxiliary buttons for the touch screen S1 S2 S3 a heated line HEAT a pump etc 106 PID Enga Tech All devices are displayed with their names by default above the drawing The user can modify the name of the device as explained before Edit Mode By right clicking one of the devices a submenu appears with the choices to show the variables names or to design the device The devices can be designed in either the Normal Mode or the Edit Mode In both cases the value that is input in the device is sent to the machine a MASS FLOW CONTROLLERS The controllers have a bar in the upper section that fluctuates between green and red indicating whether the machine is acquiring new data or not This also works as an alarm indicator when the alarm goes off the indicator starts to flash N2 Device name Acquisition alarm indicator Set point Process value Figure 5 19 MFC s icon The upper window shows the set point assigned to that variable and underneath this value the real value or process value is displayed By right clicking over the device the Design function which allows for the modification of the gas flow is accessed in ml min Figure 5 20 MFC De
154. unit The voltage requirements for the equipment are printed near the power cord attachment Voltage 110 230 VAC 5 Frequency 60 50 Hz 196 Max power consumption 2000 W 3 1 5 GAS REQUIREMENTS Make sure your lab has the appropriate gas installation for working with the unit Air supply 5 bar Gases Depending on the unit configuration The pressure of each reactant gas in the installation must be higher than the working pressure on the unit and corresponding to the mass flow controllers that the unit incorporates 3 2 EQUIPMENT INSTALLATION Before starting be sure to have available all the necessary tools and pieces for the installation 3 2 1 UNPACKING THE EQUIPMENT Unpack the unit carefully and inspect the shipping containers for damage If a container is damaged or shows signs of stress notify both the carrier and Process Integral Development Eng amp Tech PID bugs tech Keep all shipping materials for inspection by the carrier Check the items received against the packing lists If there are discrepancies notify Process Integral Development Eng Tech immediately Keep the shipping containers until you have checked their contents for completeness and verified instrument performance 3 2 2 PLACING THE EQUIPMENT ON THE BENCHTOP The unit requires a benchtop that can support its weight plus that of other equipment you will use with it The area must be free of overhanging obstructions that might
155. uoride MMME EM EM E ao Performettyiene GR 483 o V P V 90 Phosgene 1 COCA 4413 047 P P P 91 Phosphie PH3 159 073 V P V Phosphorous 92 pentafluoride PF5 5 694 0 3 lt lt lt lt e eEjli im m e SIISII S lt m m lt 60 Enga Tech 94 Propylene Propene EO 1 915 0 4 1 443 se A E 96 Silicon tetrafluoride SiF4 4 683 o 37 Sulfurylfluoride SO2F2 4 631 os 98 sufurdiodde soz 2922 068 t E t L99 Sulfurhenafluoride Sf6 eme om t E 100 Sulfur tetrafluoride SFA 4 821 0 34 P 101 E SiHCI3 6 044 0 33 102 Trimethylamine C3H9N 2637 028 P P P 103 Tungslen hexafluoride WF6 1329 025 P P P 104 Vinylbromide C2H3Br 472 046 V V V 405 Vinichleride E 2865 047 NA rior xenon j e ses 488 E EPDM N Neoprene H Hypalon T Teflon P E s V Viton Mass flow setup men is configured pressing F1 key in touch screen ee i H I c3 MASS FLOW SETUP ALARM SETUP LEVEL SETUP ADMIN SETUP ABOUT PID COMMUNICATIONS SETUP PELTIER CONTROL Figure 4 35 61 PID Enga Tech a e li a Lues een et ed ENEE MFM pl FLOR DEP ee CE SG BEI MFC configuration Figure 4 36 4 7 2 OPTION B SCALE Scale with digital communications is used for weighing the liquid stream outlet in real time This option is very interesting to calculate mass balanc
156. ure desirable values may be D 0 07 Tc 26 PID Enga Tech Clearly experience will determine the optimum values for the tuning of a control loop with these recommendations being nothing more than an approximate departure value It is important to stress that by making use of these parameters an advanced operator will be able to draw a variable s approach curve to its situation of stability following a disturbance 2f PID Enga Tech 4 3 THE LIQUID GAS SEPARATOR The Microactivity Reference unit includes a liquid gas separator of low dead volume consisting of a stainless steel tank on whose walls liquids condense at high pressure and low temperature Once they have passed through the reactor the reaction gases are drawn outside through the rear of the hot box where the separator is located see Figure 4 6 and where liquid condensation takes place Upon leaving the separator the gases are again introduced into the hot box flowing to the pressure control system provided that the unit has this set up option Figure 4 6 The separator consists of a solid piece of 316 stainless steel in which a perforation of 65 mm in depth and 8 5 mm in diameter has been drilled as well as other machining corresponding to the system s inlet and outlet and which acts as a condenser by means of a Peltier cell A Peltier cell consists of two facing ceramic panels between which there are hundreds of thermoelectric couples Ju
157. us plate of the reactor could get blocked identifying this fact by an increase of the pressure of the system In this case the user must contact with the Process Integral 135 PID Enga Tech Development Eng amp Tech Technical Service to substitute it by another plate of the same characteristics or of higher porosity The replaced porous plate could be contaminated with hydrocarbons The user of the unit must manage these residues asking to an authorized manager and attending to the environmental policy of the laboratory where it is being used 7 3 4 REPLACING A MASS FLOW CONTROLLER The replacement of one or more MFC may be caused by Their faulty operation in this case the user is to verify that this performance is not due to an unsuitable gas inlet pressure consult the specifications of the MFC that are included in the equipment s documentation or to an incorrect configuration of the MFC on the touch screen see section 4 5 2 in this manual Changes in the user s requirements insofar as the type of inlet gas or the flow supplied is concerned The steps to be followed for replacing a MFC are as follows 1 Switch off the Microactivity Reference unit and switch the main circuit breaker to OFF 2 Unscrew and remove the right hand side panel on the Microactivity Reference 3 Locate the MFC that is to be replaced see Figure 7 2 disconnect the control cable unscrewing the unit s lower panel and releasing the end connectio
158. utomatic Run Disconnect the equipment switch the circuit The pressure sensor is not connected to breaker to OFF unscrew the right hand the board side panel and verify the sensor s connection Disconnect the equipment switch the circuit The TOHO pressure controller is not breaker to OFF unscrew the right hand connected to the board side panel and verify the TOHO pressure connection Verify the status of the source by The power source 15 15 5 is short unscrewing the right hand side equipment circuiting power LED blinking or is disconnected and without power supply faulted LED off If this occurs there will and observe the LED If it is blinking be no level reading if the equipment is disconnect the controllers on the rear panel fitted with this option one by one until the one causing the short circuit is located the LED will stop blinking The pressure in the system rises The pressure controller is set to Set to automatic Run in the controller s uncontrollably without responding manual fully closed 0 _nd parameter The controller s PID parameters have been modified The reactor s temperature controller is not working properly Check the alarm and reset it providing the situation that triggered it has been resolved The rear blades on the turbine for cooling the motor are rubbing against the turbine mount The controller s PID parameters have been modified There is no reading of the
159. vated the red LED RDY on the front of the controller is lit up o Man Manual mode The user is to set the variable s control output e g heating power 0 100 on the lower screen of the controller As a general rule the user has to operate under RUN mode when the variable s set point is set or MAN when the control output is set but never under RDY mode the LED RDY on the front is to remain off e nut The variable s control output 9o This parameter will be modified by the user whenever operating under manual mode never under automatic o Regarding the temperature control this parameter indicates the of heating of the heater o Regarding the pressure and level controls this parameter indicates the of opening of the control valve fully closed at 0 and fully open at 100 The parameter AH1 on the SET 2 set up menu represents the maximum control output for the controller access this menu by depressing the Mode key for 2 sec press the Func key and enter a 2 in the cursor using the A key Move through the different menu parameters by pressing Mode until the desired parameter is reached e E1H Upper alarm limit Value of the variable above which the system s alarm is to be triggered Although these parameters have already been set with their optimum control values for operation of the Microactivity Reference unit they may be modified whenever necessary by using the Func button to go to
160. will always provide a constant flow determined beforehand by the user This means that operating the pump is perfectly straightforward 1 Enter the desired flow in ml min using the numerical keypad and press Enter Any flowrate may be set that ranges between 0 01 and 100 of the size of the pump head 5SC head 5 ml min If the flow introduced exceeds this value the message Invalid settings is displayed on the screen after pressing Run In such a case the value has to be modified During pump operation the flow may be modified as often as required without having to stop it 2 Press Run to start up the pump 3 Press Stop to stop the pump This is the normal operating mode For further information regarding all the other operating modes as well as the different set up options for the pump and troubleshooting consult the Gilson 307 pump s handbook N Attention It should be noted that the system is usually controlled by the Process acquisition software Therefore the pump operates on a remote basis by means of digital communications Control of the pump ceases to be manual as described above and all modifications in its operating mode are to be made through the control PC If it is required to use the pump s keyboard and functions it will be necessary to reboot the pump When the pump is to operate at atmospheric pressure outlet pressure atm it is necessary to install at the liquid outlet a Back Pressure
161. witch the equipment on again 10 Perform a Leak test See section 7 1 1 of this manual 6 2 PROGRAMMING A SEQUENCE OF EXPERIMENTS For programming a sequence of experiments proceed as outlined in section 5 4 of this manual How to carry out an experiment In general terms the sessions that constitute the experiment should be configured as follows An initial session corresponds to the secure shutdown of the system The second session takes the system to the operating conditions under which the experiment is to be performed e g heat the reactor up to operating temperature The duration of this session is to be sufficient to allow the system to attain stable operating conditions which may be carried out by setting long session times or else by using the condition evaluation function Subsequent sessions correspond to the operating conditions in which catalytic measurements are to be taken The final two sessions correspond to sessions involving the secure shutdown of the system with the last one being the same as the session programmed as no 1 133 PID Enga Tech 7 MAINTENANCE OF THE EQUIPMENT 7 WEEKLY MAINTENANCE 7 1 1 LEAK DETECTION It is necessary to perform a leak test when The user opens the reactor for replacing the catalyst bed The user detects a problem in pressure control To check the unit for leak proceed as follows Put the pressure controller in manual mode totally opened 100

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User Manual - PID Eng&amp;Tech

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User Manual - PID Eng&Tech