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MICROACTIVITY - REFERENCE

1. Pod Ver Software for the touch screen Hardware Ver Software for the control panel Micro3 Ver Control software Adkserv Ver Embedded software O00 0 Press the Exit key to return to the main menu 4 5 3 OTHER FUNCTIONS Adjustment of contrast on 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 39 PID EngaTech 4 6 SPECIAL CONFIGURATIONS OF THE MICROACTIVITY REFERENCE 4 6 1 THE GILSON 307 HPLC PUMP The Microactivity Reference reactor provides the option of working liquids 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 Numerical keypad 3 Pump head 4 Pump head fastener 5 Inlet to pump head 6 Outlet from pump head 7 Connections to manometer module 8 Side attachment 9 Side screws Figure 4 18 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 Oooo ma J is pressed i E Je Je i 5 HELP It displays messages and instructions regarding the system with no effect on pump operation HE CANCEL i j 3 gz j f 6 CANCEL It clears
2. OFF OFF ON ON Z Table 4 7 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 3 The actions of the external alarm on the MFC and the liquids pump will be the same as those configured by the user on the touch screen for a pressure alarm 69 PID Engatech 5 PROCESS 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 Use of this application permits data acquisition and the remote control of one or several Microactivity Reference units via Ethernet type communications 5 2 INSTALLATION OF PROCESS The installation of Process control software involves the following steps Insert the CD ROM containing the Process control into the CD reader drive Itis advisable to close all other Windows applications that are running Run the setup exe file on the CD To do so use Windows Explorer or the Run option on t
3. PH 34 918 459 930 FAX 34 918 486 454 Eng amp Tech C Plomo 15 Pol Ind Sur E 28 0 Colmenar Viejo www pidengtech com Madrid Spain m E MICROACTIVITY REFERENCE USER S MANUAL V6 150 9001 PARQUE am Kemer 1 zate gee x SPIN OFF 180 14001 a ka PARQUE BUREAU VERITAS BUREAU VERITAS Co a Certification Certification aden CSIC DE MADRID C_ _ anii prawane N 7000195 MA PROYECTO tet 1 MICROACTIVITY REFERENCE USER MANUAL CONTENTS INTRODUCTION 1 USING THIS MANUAL 2 SAFETY INFORMATION 1 2 1 SAFETY INFORMATION 1 2 2 SAFETY SYMBOLS 1 2 3 WARNING AND CAUTION CALLS 1 2 4 ELECTROMAGNETIC COMPATIBILITY 1 1 DESCRIPTION OF THE EQUIPMENT 2 1 GENERAL DESCRIPTION 2 2 SPECIFICATIONS 2 3 OPERATING CONDITIONS 2 4 EQUIPMENT APPEARANCE 2 4 1 GENERAL VIEW 2 4 2 FRONT VIEW 2 4 3 INSIDE VIEW 2 4 4 REAR VIEW 2 4 5 INSIDE VIEW ELECTRONICS INITIAL INSTALLATION 3 1 BEFORE STARTING TEMPERATURE AND HUMIDITY RANGES VENTILATION REQUIREMENTS BENCHTOP SPACE REQUIREMENTS ELECTRICAL REQUIREMENTS 3 1 4 1 GROUNDING 3 1 4 2 LINE VOLTAGE 3 1 5 GAS REQUIREMENTS 3 2 EQUIPMENT INSTALLATION 3 2 1 UNPACKING THE EQUIPMENT 3 2 2 PLACING THE EQUIPMENT ON THE BENCHTOP 3 2 3 ELECTRICAL INSTALLATION 3 2 4 GAS INSTALLATION 3 2 5 TURNING THE POWER ON Ww WW W 1 up 1 WF AUN COMPONENTS OF THE MICROACTIVITY REFERE
4. When one session is linked up to another the system will maintain the values set for all those variables that are not modified in the change of session whereby it will not be necessary to re introduce their value in the new session O0 2 PID Engatech Sessions may be linked up with each other in a random manner as per the user s wishes without having to follow a numerical order 1 2 3 etc However this system is not recommended as in this case monitoring of the reaction on the session configuration panel becomes much more complicated and increases the risk of incorrect programming of the sessions as well as of becoming caught up in endless loops Once the session configuration panel has been completely filled in press the key Apply that is to be found on the lower part to store the parameters entered in the system s memory With this action the panel will remain active on the screen thereby allowing for better monitoring of the experiment and rapid access to the modification of session parameters PLEASE NOTE These modifications will not be registered in the application until the key Apply is pressed Pressing the key Accept closes the session configuration panel 5 5 4 DATA PROCESSING AND GRAPH PRESENTATIONS The values of the variables acquired by Process may be exported to an Excel spreadsheet for subsequent processing The procedure to be followed is as follows 5 5 4 1 Recovering data from the
5. 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 i set to Set to automatic Run in the controller s manual fully closed 0 _nd parameter system s pressure in the controller 101 PID EngaTech uncontrollably without responding Release the joint between the system s gas to the set point with the 3 port 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
6. 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 Release each one of the sections of pipe Blockage in the by pass valve or in the d hether th falls Cl as preheating and or mixer lines and See wheter 1e pressure oan g and or replace the blocked section No gases are entering the system Check the symptom No gases are entering the equipment No rise in pressure in the system Perform a leak test on the equipment See Leak in the reaction system the section Performing catalytic tests in this manual Set the 3 port valve to the by pass position If the pressure in the system 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 The pressure in the system rises Release the connecting
7. O stare o aaf o n aid o 2 v O oio a eo0o00o0000000g050 oe ae ereores a Ocis0 0000000 ojalrez a 9176 SUOUHLNG o0o0o000o0o0oo0oqo00q00q0q00q0000 on 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 23 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 0 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 48 PID EngaTech To adjust the valve s zero setting set switch Z on the dip switch to On S1 zero see Figure 4 24 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 Op
8. 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 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 a
9. 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 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 98 PID Engatech 10 REACTOR TROUBLESHOOTING SYMPTOM POSSIBLE CAUSES SOLUTION The switch on the front is in the off Press the switch on ne mone position The main circuit breaker on the rear is Switch the main circuit breaker to ON off 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 distributo
10. 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 the 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 The gas flow does not reach the The set point established is below 10 It is not advisable to operate below 10 of set point established remaining of the maximum flow of the mass flow ng i SiG per ae ne dared stable at a lower value controler controller with another that is suited to the process 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 Reset the maximum flo
11. 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 AN Attention It should be noted that once the system is controlled by the Process acquisition software and therefore the pump operates on a remote basis by means of digital communications control of the pump ceases to be manual as has been described up until now and all modifications in its operating mode are to be made through the control PC If the need arises to use the pump s keyboard and functions it will be necessary to reboot the pump When the pump is going to work at atmospheric pressure outlet pressure atm it is necessary to install at the l
12. MFC SP2 Micro3 Micros Micro3 52 To actuate upon a gas chromatograph Connector External Control Micro3 ChromQ ChromON o 0 Deactivated cycle Opened contact lilt a o 1 Activated cycle The circuit closes during 1 s in a cycle mode RC TEMP Auto Manual i ips te 3 ae ar Time specified in CyTime AC TEMP Piopesional Band CyTime Cycle time in seconds RAC TEMP Integral Time RC TEMP Derivative Time RC TEMP MY H limit RC TEMP MW L limit HB TEMP Set Point 0 170 HB TEMP Auto M anual HB TEMP Output HB TEMP Proportional Band HB TEMP Integral Time HB TEMP Derivative Time HB TEMP MY H limit HB TEMP MY L limit PUMPOT Set Point PUMPOT RUN PUMPOT STOP 4 Cancel Help Figure 5 24 87 Ys of Ad TA DECE l I VITY R E f El al PID EngaTech MICROACTIVITY Reference PMP1 a _ STATUS GC Cycle ae i Activated x Deactivated Figure 5 25 88 PID Engatech 6 PERFORMING CATALYTIC TESTS 6 1 LOADING THE CATALYTIC BED IN THE REACTOR Insert the catalytic bed inside the reactor by proceeding as follows Open the reactor hot box by pressing the Door key on the touch screen 2 Disconnect the reactor s 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 release the reactor at connections A se
13. R rig TAn r Hian Lo ied ipa H HOSMJE EAT E DEL pm E tA POULT A So zl z Pada Ling uai Co apaiia anpii Fy Wa H amA EL AA wOOHewe og Ow AL ey bel Me ao LH eles bse HE Of W WULF Be BE THALES Ti La F on EA AD LARLA E p LEEA iM Bears WL eS SS Alita Tr Sterns tit Sis eee Pal AE Soi HoH M0 l ree Ss o4 dja KET He Ged PISS Es qdcd e OL EZR ae oF ayd ee OS ia Are rae TA im Figure 4 1 17 PID EngaTech 4 1 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 305 mm External diameter 14 5mm Internal diameter 9mm Material 316 L Stainless steel Internal volume 20 ml Connections SF562CX Seals AE 6F2986 Tmax recommended 700 C Pmax recommended 1350 bar at 25 C 400 bar at 482 C Pmax reactor 100 bar The following graphic illustrates the maximum working pressure for type 316 stainless steel nipple of Autoclave Engineers depending on the temperature I Pressure Temperature Rating Curve 316 SS a 304 A im SS 90 Besa cw z _ 5 5 Before 800 F 427 C ao pt ft ft pe Of Rated Pressure R T 0 100 38 sian ll This curve illustrates maximum Ta pressure for Type 376 stainless steel tubing valve and fitting bodies at various temperatures ta 12
14. SAFETY SYMBOLS Warnings in the manual or on the instrument must be observed during all phases of operation 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 amp Tech assumes no liability for the customer s failure to comply with these requirements 1 2 3 WARNING AND CAUTION CALLS AN 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 Indicates a hot surface Indicates earth ground terminal OPPA PID Engatech 1 2 4 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 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
15. 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 acetona 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 POROUS PLATES The reactor is provided with two 10 microns porous plates that could get blocked as a consequence of the continuously use For replacing them take out the filters from the unit open the filters body and remove the 10 microns porous plate Replace it for a new one supplied as an equipment spare part Ref Vici Valco 10FR4 If as a consequence of this maintenance the filter body has leaks it is recommended to replace it by another one Vici Valco VA_ZBUFR2F10 90 PID EngaTech Figure 7 1 The replaced porous plate could b
16. 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 the strands on this propeller favouring their mixing see Figures 4 37 and 4 38 Figure 4 37 63 Engatech GAS MIXER lt 170 gt HOKE 6133M2Y A lo A oO co lt 10 gt NPT 1 8 NPT 1 8 lt 30 Y m wo N ro NPT 1 8 Figure 4 38 Reactor filters VV ZBUFR2F Located on the reactor s gas inlet and outlet lines 316 type stainless steel 1 8 pipe connections 2 mm 0 080 interior cavity Porous panel of 10 um in Hastelloy C reference 10FR4HC 4 7 3 INSTRUMENTATION Pressure transducer SWT A08 Measurement range FS 0 4 FS 10K Table 4 6 64 PID EngaTech 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 th
17. be stored in the system until the Accept button is clicked Sample Rate Sample Rate 5000 m Ok Cancel Figure 5 14 With the acquisition of parameters the control PC will store the different parameters registered by the Microactivity Reference unit in its memory but no experiment will be sent In order to send an experiment or programmed sequence of sessions to the unit proceed from the Session Configuration Panel as explained in the following section 5 5 3 THE SESSION CONFIGURATION PANEL The configuration of the process sessions is the next step to be performed by the user once the name of the experiment has been defined see previous section and data acquisition has started with sessions understood to be each one of the process states or steps in each one of which each variable has a specific set point The Process application allows for the creation and configuration of as many sessions as required which are to be carried out progressively as defined by the user The linking of these sessions or steps will make the process develop along the path desired and defined by the user The session configuration panel is accessed as follows 1 On the functions bar use the mouse s left button to click on the tab Sessions 2 In the new window displayed select the option Configure Sessions 000039_ Catalyst Name _ Assay Name MicroactivityReference Experiment Acquisition Pese Profiles D
18. experiment in process To recover data from an experiment that has just been run in Process and which remains active the control software has not been closed carry out the following steps 1 On the functions bar use the mouse s left button to click on the tab Data 2 Select the option Variable Figure 5 17 EE F 7 000020_ Catalyst Name _ Assay Name MicroactivityReference Experiment Acquisition Sessions MESEN Help hi ajat Bate P Figure 5 17 3 A window like the one shown in Figure 5 18 will open where the user may select the variables whose data are to be recovered e g RCTemp Pressure etc Clicking on the red crosses the user selects the desired variables Peltier Door ByPass N2 200 ml min MFC SP N2 200 ml min Ethylene 150 ml min Ethylene MFC SP Ethylene 150 ml min SPEthylene Methane 200 ml min Methane MFC SP Methane 200 ml min SPMethane Valvel Valve2 RC TEMP Output RC TEMP HB TEMP Output HB TEMP PUMPO1 Purga2 MFC SP Purga2 Pressure Output Pressure Inhibition Micro3 x xKKKKKKK KKK KKK KKK KK K Figure 5 18 83 PID Engatech 4 Once the variables have been selected click on Load data and data columns will appear in the right hand side of the window displaying the following a On the left the time variable in the format dd mm yy h min sec b On the right the values acquired of the selected variable 5 Click on the right button of the mous
19. greater stability but they lengthen the time required for attaining stationary state Proportions 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 It 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 proc
20. ies Address e Network Connections LAN or High Speed Internet Network Tasks 1394 Connection E Create a new connection Connected Firewalled Set up a home or small Tei 1394 Net Adapter office network Change Windows Firewall Local Area Connection settings Connected Firewalled UC Realtek RTL8139 810X Family See Also i Network Troubleshooter Other Places E Control Panel My Network Places My Documents 3 My Computer Details Network Connections System Folder Figure 5 1 Select Internet Protocol TCP IP and click on Properties t Local Area Connection Properties General Authentication Advanced Connect using EJ Realtek RTL8139 310 Family Fast This connection uses the following tems El Client tor Microsoft Networks B File and Printer Sharing for Microsoft Networks Gos Packet Scheduler Internet Protocol T CPP E Install Uninstall Description Transmission Control Protocollnternet Protocol The default Wide area network protocol that provides communication across diverse interconnected networks C Show icon in notification area when connected Notity me when this connection has limited or no connectivity Figure 5 2 Set the communication parameters 71 PID Engatech Internet Protocol TCP IP Properties eo General You can get F settings assigned automatically if your network supports t
21. in the equipment are to have the same characteristics as the one being replaced check the specifications of the MFC that are enclosed in the documentation Mass Flow Controllers HI TEC by BRONKHORST model EL FLOW IDENTIFICATION No F_211C_FAC_11V Figure 7 4 93 1 02 oO PID Engatech F N N NAA A A A N N A SUPPLY VOLTAGE 0 Valve only H Sensor only A 15 Vdc 1 Sensor B 24 Vdc G Controller N O D 15 24 Vdc OUTPUT SIGNAL PRESSURE RATING 0 64 bar Ba 0 10 V C 0 20 mA sinking 2 200 bar D 4 20 mA sinking 3 400 bar F 0 20 mA sourcing G 4 20 mA sourcing K 0 5 Vw cable compensation SENSOR RANGE L 10 V w cable compensation te ree Ree a 15 ml min 1C 0 15 0 15000 ml min CONNECTION OUTLET THLE 100 l min DAGU Oe eas 250 l min compression type SAC 0 100 0 12501 min For flow ranges of sensors with M in their model 6 mm compression type 12 mm compression type number please see table at page 6 x compression type 20 mm compression type x face seal male other oom Te amp oom Om amp Ww bh SPECIAL Control with Vary P Valve OM 0 10 0 500 ml min SEALS 1M 0 500 0 10000 ml min E EPDM BM Dia LOD x aan 100 1 min P Elastomeric PTFE Z Other Figure 7 4 Gas Determined by the user Maximum flow Determined by the user Inlet pressure Determined by the user Place the new MFC in the d
22. is not possible control of the same is to be maintained by digital communications through the Process software There needs to be a pressure of 10 15 bar in the pump head No backpressure has been installed and _ Install a backpressure prior to the inlet on operation is at atmospheric pressure the liquid non return valve be ed l Only feed liquids when the operating No liquid is entering the reactor or pressure is above 10 15 bar the flow is unstable Pressure of Vent the pump releasing the liquid inlet line the head below operating The pump has not been properly vented PHNP g q pressure on the reactor There is a leak in the system s liquid inlet An alarm has been triggered in the Check the alarm and reset it providing the system that has shutdown the system s situation that triggered it has been liquid inlet resolved There needs to be a pressure of 10 15 bar in the pump head No backpressure has been installed and _ Install a backpressure prior to the inlet on operation is at atmospheric pressure the liquid non return valve Only feed liquids when the operating No liquid is entering the reactor SEEE aove O Pressure of the head close to T operating pressure The 3 port valve on the pump is not in Set the valve to the suitable position see the normal operating position injection the section Venting the pump in this from the tank manual or in the pump manual An alarm has been trigger
23. of 316 stainless steel in which a perforation has been drilled of 65 mm in depth and 8 5 mm in diameter 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 Just 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 this tank 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 performe
24. 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 micrometric 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 com
25. 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 1150 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 If must be set to the same as the pressure of the aspirated liquid that is the saturating vapour pressure at the ambient temperature 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 5 1 58 60 65 7 2 7 4 Pc The default value is O Mpa Input Output parameter setup I O Press Menu and I O The sequence of parameters is High pressure limit If the pressure reading from the manometric module rises above this limit the pump will stop The sequence following a high pressure e
26. see the section Configuration of the Servo Digital V4 0 unit in the manual 103 PID Engatech 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 The inhibition function has been triggered as a safety measure in response to a system alarm The change in programmed session does not occur triggered it has been resolved When saving a Process ene oe ea The program is still acquiring data from haps eh bal nara a no display is made of the screen prog q g cannot be acquiring data from the unit the equipment RUN status n for allocating the name to the press the STOP key template 104
27. 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 89 PID Engatech T MAINTENANCE OF THE EQUIPMENT 7 1 WEEKLY MAINTENANCE 7 1 1 LEAKS DETECTION It is necessary to perform a leaks test when The user opens the reactor for replacing the catalyst bed The user detects a bad control in pressure control For checking leaks in the unit proceed as follows Put the pressure controller in manual mode totally opened 100 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
28. the latest entry without storing it in the memory 7 ENTER Confirmation key 8 Numerical keypad Figure 4 19 40 PID EngaTech 4 6 1 3 Technical Specifications Purnp Purp Heads X stainless steel W rinsing compartment for aqueous salt solutions 30 1M Ti titanium Mixing Modules Operating Modes Pump Parameters Programmable Parameters Pressure Pulse Dam pening Software Communication Interface Display Panel Front Panel Liquid Contact Materials Power Requirements Fregrammae redprocating pump with single piston interchangeable head constant stroke and fast refill motion internal pulse dampener and pressure feedback Purnp Head Model Flow Rate Range mLmiri O O1eS ADIO AoH G Pressure Range pal bar 145 8700 1 0 14 58700 1 0 Ww 145 8700 1 60 B11D Analytical Mixer 10 10 mLitmin 1 5 mb 1 1220 S110 Titanium Analytical Mixer 10 10 rmLimin 1 5 mb 11107220W S110 Titanium Analytical Miser 0 1 3 0 mbimin 0 7 mb 110 220 ATID Microbore Miser lt 0 1 mbfmin 65 pl 110220 Constant flow rate Flow constant volume Dispense and time based sequence Program Head nurnber Sor 10 Liquid compressibility 2000 Mbar Refill time 125 1000 ms Inlet pressure 0 10 MPa EELE Timed everts for programming four cutput contact closures and one input to wait for injection Time adjustable from 17 10 min with increments from 001 1 min depending onthe range
29. the touch screen in that moment in the field MAX LEVEL is saved the maximum value of the lavel sensor calibration This value is not the sensor response with 2 ml of liquid but the estimated response of the sensor for 10 ml of liquid in the condenser MAX LEVEL Hz Zero FREC 2 ml Zero x 5 If we set the sensor range in 2 ml the increase in level inside the separator due the fall of a drop of liquid would represent a very high percentage regarding the maximum calibration value 2 ml which would imply a very poor control procedure with very sudden changes in the position of the control valve To avoid this the sensor range is extrapolated to 10 ml once is tested the linearity between the sensor response and the level of liquid inside the condenser In this point it is very important to check that the sensor range is configured at 10 ml in the TOHO controller _SLH parameter in SET 2 With these parameters the level controller gives a REAL reading of the level of liquid inside the liquid gas separator in ml By graphically plotting the sensor frequency against the amount of water present in the system it can be verified that the system s response is perfectly linear which enables a relationship to be established between oscillation frequency and the volume of water present in the tank 57 Calibrating the sensor for any other fluid X different from water PID EngaTech In order to verify li
30. to be found on the upper part of the equipment Figure 3 9 The connection is to be made as follows Synthetic air O O O O Inlet pipe Polyethylene 6x4 mm pipe supplied with the equipment 3 m Connection Quick fit connection pressing the pipe against the adapter Inlet pressure 5 bar It operates on the pneumatic systems for door and oven opening 6 port valves etc Gases 1 2 etc Reaction gases O O O Inlet pipe 1 8 pipe in 316 stainless steel Connection Gyrolok 1 8 adapter 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 The gas inlet position 1 2 etc depends on the Reaction gases arrangement of the mass flow controllers on the equipment Figure 3 9 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 i Reduce the inlet flows to zero for each one of the reactant gases Preferably f
31. turbine or act upon any other part of the system gt Oven closed detector So as to disconnect the 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 changing 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 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 67 PID EngaTech 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
32. 00 F 649 C expressed as a percentage of the R T pressure rating of the component Thus a component rated 70 000 psi 690 bar R T would be rated 9 000 psi 621 bar 600 F 316 C or 90 of its rating Pf ft ft TA aa aa TT ST HaT E ET 200 300 400 S010 pog 700 gog 900 1000 tiog 1200 93 149 9 204 260 316 371 427 462 538 593 649 Temperature in F C 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 6AL4V etc can be used As may be seen in Figure 4 2 the inside of the reactor has been fitted with a 10FR4HC 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 Reducing to a minimum the dead volume at the outlet Replacing the plate whenever so required without the need to replace the reactor nipple Thermocouple gt Tubular reactor gt Porous plate Porous plate support Figure 4 2 The thermocouple type K encased in a 1 5 mm diameter Inconel sheath in 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 r
33. 00 s D 2 60s 24 PID EngaTech 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 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
34. 022 024 026 Cv Figure 4 22 The system that has been designed for operating on the valve consists of a high resolution microstep motor Such 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 1 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 order 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 it has been used a current generator and an instrumentation amplifier 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 pre
35. 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 it if 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 indicate 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 labor
36. GE E LP Past EE FE FEE FEE GATEHAT EE FE FEE FEE TCP PORT E REH Figure 4 14 Press the Exit key to return to the main menu 37 PID Engatech PELTIER CONTROL Selection of the peltier mode o COOL For reducing the L G separator temperature Minimum about 1 C o 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 Peltier Control This parameter is directly proportional to the cooling heating power supplied to the L G separator values between 0 and 100 Duty time s Time of the cooling heating cycle typically 10 seconds ee a a a C a t T Rol PEEVE HODE PELTIER CONFIG PELTIER CONTR L DET EME Figura 4 15 ADMIN SETUP Screen for the system configuration by a PID Eng amp Tech administrator The password is not available for the user of the unit Figura 4 16 38 PID EngaTech m ABOUT PID Product information ie ee Oe ee ee MICROACTIVITY REFERENCE POD VER v3 16 22 16 2666 HARDWARE VER v3 19 61 64 2005 MIcROGSs VER ABCDEF ADKSERY YER ABCDEF Wilh Integral Development Enge Tech cA Plomo 15 Folig Sing Sur colmenar Yiejo Madrid Spain Tel Wid ela Figure 4 17 This screen provides information regarding the company PID Eng amp Tech as well as the versions installed on the unit
37. Ibs 4 6 1 4 Switching on the pump Before operating the liquids pump the electrical and mechanical installation of the system needs to be performed which means 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 pump as well as the version of the control software as shown below Pump Model 307 V x x Following this message the pump s main operating screen is displayed 4 6 1 5 Setting up the pump Once the electrical installation is done as is 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 no necessary for the customer to do it again Setup pump hardware PUMP Press Menu and Pump The sequence of parameters is 41 PID Engatech Refill time t is the time required for the piston return stroke Normally it is set at the lowest value 125 ms If cavitation of 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
38. Move the device away from the radio or television c Plug the device into a different electrical outlet so 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 PID Engatech 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 HOT BOX VIVVVVY E O E OOOO Samer ea Soom Sac Sonn Soa Figure 2 1 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 va
39. NCE UNIT 4 1 THE REACTOR AND THE HOT BOX 4 2 THE CONTROLLERS 4 2 1 THE REGULATION PARAMETERS PID Eng amp Tech PID EngaTech 4 2 22 CONTROL STABILITY CRITERIA 4 2 3 CONTROLLERS TUNING 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 4 4 THE PRESSURE SENSOR FOR ATMOSPHERIC PRESSURE REACTORS 4 5 THE TOUCH SCREEN 4 5 1 MAIN SCREEN FUNCTIONS 4 5 2 MAIN MENU 4 5 3 OTHER FUNCTIONS 4 6 SPECIAL CONFIGURATIONS OF THE MICROACTIVITY REFERENCE 4 6 1 THE GILSON 307 HPLC PUMP 4 6 1 1 Frontal view 4 6 1 2 Keyboard 4 6 1 3 Technical Specifications 4 6 1 4 Switching on the pump 4 6 1 5 Setting up the pump 4 6 1 6 Venting the pump 4 6 1 7 Pump operation 4 6 22 PRESSURE CONTROL 4 6 2 1 Introduction to pressure control systems in microactivity reactors 4 6 2 2 The micrometric valve 4 6 2 3 Configuration of the Servo Digital V4 0 unit microstep positioner 4 6 3 LEVEL CONTROL IN THE LIQUID GAS SEPARATOR 4 6 3 1 Introduction to level control in microactivity reactors 4 6 3 2 The capacitive level sensor 4 6 3 3 Calibrating the level sensor 4 7 OTHER COMPONENTS ON THE MICROACTIVITY REFERENCE 4 7 1 PIPING 4 7 2 JOINTS AND VALVES 4 7 3 INSTRUMENTATION 4 7 4 LIST OF PARTS FOR THE MICROACTIVITY REFERENCE 4 8 PROCESS CONTROL AND AUTOMATION 4 8 1 CONTROL LOOPS IN THE MICROACTIVITY REFERENCE 4 8 2 AUTOMATION 4 8 3 SYSTEM SAFETY MANAGEMENT PROCESS CO
40. NG PID Engatech MICROACTIVITY REFERENCE USER MANUAL 1 INTRODUCTION The Microactivity Reference unit is an automated and computer controlled laboratory reactor for catalytic microactivity tests Possible unit configurations 3ASIC 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 LEVEL 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 Space for up to 6 MFC with stepper motor of 1 valve and capacitive level Balance at liquid output accuracy sensor of low de
41. NTROL SOFTWARE 5 1 INTRODUCTION 5 2 INSTALLATION OF PROCESS 5 3 COMMUNICATION PARAMETERS CONFIGURATION 5 3 1 COMMUNICATION PARAMETERS OF THE MA REF UNIT 5 3 2 COMMUNICATION PARAMETERS OF THE PERSONAL COMPUTER 5 3 3 INITIATING THE PROCESS APPLICATION 5 4 USING PROCESS 5 4 1 STARTING PROCESS APPLICATION 5 4 2 THE FUNCTIONS BAR 5 4 3 THE PROCESS SCREEN 5 4 4 THE PROCESS CONTROL GRAPHS 5 5 PERFORMING AN EXPERIMENT 5 5 1 CREATING AN EXPERIMENT 5 5 2 DATA ACQUISITION 5 5 3 SESSION CONFIGURATION PANEL PID Engatech 5 5 4 DATA PROCESSING AND GRAPH PRESENTATIONS 5 5 4 1 Recovering data from the experiment in progress 5 5 4 2 Recovering data from prior experiments 5 5 5 SAVING EXPERIMENT TEMPLATES 5 5 6 CHECKING THE ALARMS 5 6 CONNECTION TO A GAS CHROMATOGRAPH 5 6 1 CONNECTION TO AN EXTERNAL ALARM 5 6 2 CONNECTION TO A GAS CHROMATOGRAPH 6 PERFORMING CATALYTIC TESTS 6 1 INTRODUCING THE CATALYTIC BED INTO THE REACTOR 6 2 PROGRAMMING A SEQUENCE OF EXPERIMENTS 7 MAINTENANCE OF THE EQUIPMENT 7 1 WEEKLY MAINTENANCE 7 1 1 LEAKS DETECTION 7 1 2 CLEANING THE UNIT 7 2 MONTHLY QUARTERLY MAINTENANCE 7 2 1 REPLACING THE FILTERS POROUS PLATES 7 3 ANNUAL OR LATER MAINTENANCE 7 3 1 REPLACING THE FUSE 7 3 2 REPLACING THE KALRETZ SEALS IN THE GAS MIXER 7 3 3 REPLACING THE REACTOR POROUS PLATE 7 3 4 REPLACING A MASS FLOW CONTROLLER 7 4 DETECTION OF LEAKS 8 EUROPEAN DIRECTIVES 9 ENVIRONMENTAL POLICY 10 REACTOR TROUBLESHOOTI
42. P Purga2 Pressure Output Pressure Inhibition Micro3 KRXOKKKKKXKXKQOKKKXO KOKO KKK 5 5 4 2 Recovering data from prior experiments For recovering data from prior experiments the user should proceed as follows Open a new Process session if there is an experiment running the user can open a second Porcess session at the same time clicking on the application icon Figure 5 4 In Process functions bar select Experiment Load Experiment Figure 5 20 ProcessA Sane Acquisition Sessions Data Help 6 amp amp ty aiad Dee PH o F New experiment Load experiment Exit Figure 5 20 Select the experiment to recover Series No Catalyst Name _ Test Name adb When the user is loading an old experiment in a Process session it is no possible to acquire data or sending programmed sessions to the reactor with this session but it is possible with another Process session So in this mode the Start and Stop acquisition buttons are deactivated In this mode it is no possible too to save experiments Once the experiment is loaded click on Data Variable and select the variable that the user wants to check the data as described in the previous section 84 PID Engatech Click on the right button of the mouse select Copy all data to clipboard Now these data can be pasted in any data sheet Excel Origin Txt etc The format of the Excel columns
43. TEMP Auto Manual RC TEMP Output AC TEMP Proportional Band RC TEMP Integral Time RC TEMP Derivative Time RC TEMP MV H limit RC TEMP MY L limit HB TEMP Set Point HB TEMP Auto Manual HB TEMP Output HB TEMP Proportional Band HB TEMP Integral Time HB TEMP Derivative Time HB TEMP MV H limit HB TEMP MY L limit PUMPO1 Set Point 0 0 528 PUMPO1 RUN PUMPO1 STOP 4 Cancel Help Figure 5 16 The following parameters are to be set for each one of the sessions Name Name of the session Alias Description optional Brief outline of the session Time sec Time expressed in seconds the session is going to last Once this time has elapsed the system will go on to carry out the next session which will be the one specified in the box Index next session e Evaluate condition Option not available in the version Process 1 0 2 options switch from one to the other with the mouse s left button 80 PID Engatech O X The system will not evaluate any condition it will jump to the next session when the established session time has elapsed o Wl The system will evaluate the condition set forthwith The jump to the next session specified in Index next session will occur in the event of any one of the following situations When the specified condition has been fulfilled e g Treactor gt 500 C When the established session time has expired Variable Variable to be evaluated in the condition e g T
44. absolute temperature alarm shuts down the control signal on the reactor oven and on the hot box heater 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 changing session automatically gt Operation of the hot box The hot box is fitted with a forced convection heater that consists of a turbine and 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 gt 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
45. ach 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 95 PID Engatech 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 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
46. ad Mass flow meter at gas output Pmax 100 bar Accuracy 0 2 volume 0 3 ml Special dimensions and 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 PID Engatech 1 2 SAFETY INFORMATION 1 2 1 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 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 tha AC power cord before removing covers 1 2 2
47. an increasingly tighter fit within an orifice generating a variable section passage that depends on the distance the needle has been moved Figure 4 21 45 PID EngaTech _ Plug Rod aa E Figure 4 21 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 If 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 such as 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 f
48. and select the liquid Once the level sensor is calibrated and the equipment making reaction the user should select the reaction product liquid in this screen If this is unknown or it is a mixture the user can select the option OTHER and estimate the mixture dielectric constant LEVEL SENSOR CALIBRATION css ee Gee al a Ethanol Methanol DIELECTRIC K 123 45 isopropanol ome ME RETURN Figure 4 31 56 A PID EngaTech Prior to starting calibration observe that the oscillation frequency registered on the screen in the field Level is practically constant This value corresponds to the sensor s baseline volume of liquid in the tank 0 and can be saved on memory pressing the button MIN in the touch screen the value is saved on the field MIN LEVEL Use a graded syringe to insert 0 5 ml of deionised water through the liquid inlet orifice Keeping the liquid outlet sealed with the plug insert the needle right inside the tank to avoid the meniscus effect at the inlet mouth The touch screen will display a step up in the control graph as a result of the increase in frequency Wait for the system to stabilise and make a note of the frequency value registered Repeat the above operation 3 more times until 2 ml of liquid have been introduced into the tank each time making a note of the oscillation frequency value Once there is 2 ml of liquid in the condenser press the button MAX on
49. ata Help Sessions Setting iN aint A njai P BH Properties Selector Figure 5 15 19 Process variables PID Engatech Display will immediately be made of the Session Configuration Panel which is presented below Figure 5 16 Sessions that configure the process Control Panel and Sessions Setting Ey ii al Run Session 1 100 1 Initial o Bu k No Session Running Session 1 Session 2 Session 3 Session 4 Session 5 Session 6 Session Session 8 Session 9 Session 10 Session 11 Session 12 Name Initial Temp Incr Reaction Reaction2 Stop End SessionName SessionName SessionName SessionName SessionName SessionName Alias Initial Inerl React Reac2 Stop1 End SessionAlias SessionAlias SessionAlias SessionAlias Session4lias SessionAlias Description initial Incr React Reac2 Stop1 End ssionDescripti ssionDescripti ssionDescripti ssionDescripti ssionDescripti ssionDescripti Time sec 30 1800 900 1800 600 10 0 0 0 0 0 0 2 f x x x x x x x x x x x x Variable Oper gt lt gt lt Value Jump to Session 2 3 4 5 6 End End End End End End End Device Property YalueS1 Value 2 ValueS3 ValueS4 VYalueS5 Value S6 Value 7 ValueS8 Yalue 59 Value S1 0 Yale 511 Yalue 12 Micro3 Peltier Micro3 Door Micro3 ByPass Micro3 MFC SP1 Micro3 MFC SP2 Micro3 MFC SP3 Micto3 51 Micro3 2 Micro3 ChromON Micto3 CyTime RAC TEMP Set Point RC
50. atories with inflammable gas 96 PID Engatech 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 98 336 EEC Electromagnetic compatibility The Microactivity Reference unit as per Directive 89 336 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 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 97 PID Engatech 9 ENVIRONMENTAL POLICY Process Integral Development Eng
51. ay be included The choice of catalyst test and equipment will determine the name of the experiment that is to be performed being expressed as follows e g 000029 SiC_Trial_MicroactivityReference10 Name of equipment Test Catalyst No of exneriment nerformed in eauinment automatic 5 5 2 DATA ACQUISITION To start the system acquiring the plant s parameters click on the button that is to be found on the functions bar the system will start registering the parameters of the Microactivity Reference as well as plotting the control graphs This process may be paused or stopped whenever the user wishes using the respective keys IL and on the functions bar The frequency of acquisition of the system s parameters may be established by modifying the sampling period time elapsed between two successive data acquisitions which is accessed by 78 PID EngaTech clicking on the tab Acquisition on the functions bar and selecting the function Sample Rate as shown in Figure 5 13 000039_ Catalyst Name _ Assay Name MicroactivityReference Experiment MwA Sessions Profiles Data Help Start gt e iy ai a Fa zsa P HE F Stop Sample Rate Figure 5 13 The following screen will be displayed Figure 5 14 in which the desired sampling period can be set in milliseconds It is advisable to use sampling periods of 5 10 seconds 5000 10000 ms Changes made to this parameter will not
52. by 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 assessed by the controller whereby its output signal 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 3 Out 1 and 2 Process value Alarm 1and2 j eds d Set point control output Cursor displacement ALI AL COM ROY Di Digital signals by the digits in each function Y Decrement pulser Access level selector Elaea Increment pulser TOHO Figure 4 3 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 keys The Mode button is used to access the different control parameters configured in the controller e Process value e _ P Proportional band e _ E Integral action s e _ d Derivative action s 20 PID Engatech e _ nd Control mode Select with the AandV keys o R
53. ch 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 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 separator with level sensor incorporated is featured in Figure 4 26 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 27 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 Mic
54. chieved 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 to a value of P 8 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 25 PID EngaTech 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 buffered solution etc to 200 600
55. chromatograph in the Sessions Setting Panel of Process software This cycle actuates closing the electrical circuit that connects with the GC during 1 second The user can configure the cycle time time between 2 closings in the fill CyTime Figure 5 24 Visualization In the process screen is configured the device for checking the status of the chromatography cycle Figure 5 25 Control Panel and Sessions Setting gt ii a Run Session 1 100 1 Initial Run k a No Session Running Session 1 Session 2 Session 3 Session 4 Session 5 Session6 Session 7 Session 8 Session 9 Session 10 Session 11 Session 12 Name Initial Temp Incr Reaction Reaction Stopi End SessionName SessionName SessionName SessionName SessionName SessionName Alias Initial Inert Reacl Reac2 Stop End SessionAlias SessionAlias Session4lias SessionAlias Session4lias Session4lias Description initial Incr Reac1 Reac2 Stop End ssionDescripti ssionDescripti ssionDescripti ssionDescripti ssionDescripti ssionDescripti Time sec 30 1800 900 1800 600 10 0 0 0 0 0 0 Condition x x x x x x x x x x x Variable Oper gt lt gt lt Value Jump to Session 2 3 4 5 6 End End End End End End End Device Property ValueS1 ValueS2 ValueS3 ValueS4 ValueS5 ValueS6 ValueS7 ValueS8 ValueS9 ValueS10 ValueS11 Value 12 Micro3 Peltier I 0 Micto3 Door Micro3 ByPass Micto3 MFC SP1 Micto3
56. ct by an increase of the pressure of the system In this case the user must contact with the Process Integral 92 PID Engatech 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 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 3 disconnect the control cable unscrewing the unit s lower panel and releasing the end connections Figure 7 3 4 The MFC that are installed
57. ction 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 given 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 Reduction element VV I ZR21L 62 PID EngaTech 1 8 VICI pipe thread reduction connection to 1 16 pipe thread 9316 type stainless steel Bushing GY 2BU 316 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 Hoke 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 Non return valve GY 6133M2Y Kalrez 316 stainless steel Joint in chemically compatible Kalrez elastomer Teflon As per Standards ASTM A 182 ASTM A 479 and CMTR certificate Maximum operating pressure of 6000 psig at 70 C 423 Kg cm at 21 C Cy 0 3 In order to
58. ctivity 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 a reactor operating at atmospheric pressure the removal of condensed liquids in the separator has to be performed manually by an operator But this procedure is not possible in equipment that is operating at a pressure that is higher than the atmospheric one as 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 is to have a control loop whereby as of the recording of a specific level of liquid a control valve is operated to maintain the liquid level constant or what is tantamount to the same thing continuously remove 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 t
59. d 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 reactor APPEARANCE OF THE DEVICE 1 Display It shows the value of the pressure measurement adjustments error messages and the keyboard 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 5 SPECIFICATIONS OF MODEL DP2 21 Range of read out 0 100 kPa O 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
60. diate 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 procedure desirable values may be D 0 07 Tc 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 2 PID EngaTech 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 4 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 4 The separator consists of a solid piece
61. e Figure 6 1 4 Hold the reactor with a clamp on the upper part B and loosen 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 inside 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 the passage 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 switch on the equipment again 10 Perform a Leaks 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 Performing an experiment In general terms the sessions that constitute the experiment should be configured as follows An initial session corresponds to the secure
62. e These systems do not allow for heating 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
63. e select Copy all data to clipboard Now these data can be pasted in any data sheet Excel Origin Txt etc The format of the Excel columns must have the same format for each cell number with without decimals date time etc as the data that have been imported Date Time N2 200 ml min lene 150 ml aane 200 ml RC TEMP a 1 27 2006 8 06 34 AM 200 1 ica 1 27 2006 8 06 42 4M 199 9 175 8 1 27 2006 8 06 47 AM 198 8 164 8 1 27 2006 8 06 52 4M 193 5 153 7 1 27 2006 8 06 57 4M 184 143 1 27 2006 8 07 01 AM 172 9 132 7 1 27 2006 8 07 06 AM 104 9 1220 1 27 2006 8 07 11 AM 1 27 2006 8 07 15 AM 138 6 104 5 1 27 2006 8 07 22 AM 124 1 93 4 1 27 2006 8 07 27 AM 149 7 130 5 1 27 2006 8 07 32 4M 162 2 150 1 1 27 2006 8 07 36 4M 180 7 174 6 1 27 2006 8 07 41 AM 190 2 187 2 1 27 2006 8 07 46 AM 195 2 193 7 1 27 2006 8 07 51 AM 197 7 196 9 1 27 2006 8 07 58 4M 199 3 199 1 27 2006 8 08 02 AM 199 7 199 6 1 27 2006 8 08 16 4M 200 2 200 3 1 27 2006 8 08 20 4M 200 3 200 3 1 27 2006 8 08 25 4M 200 3 200 4 1 27 2006 8 08 30 4M 200 3 200 4 1 27 2006 8 08 34 4M 200 3 200 4 1 27 2006 8 08 48 4M 200 3 200 4 AIAN Omer Ake AA A am a Figure 5 19 Peltier Peltier Door Door ByPass ByPass N2 200 ml min N2 MFC SP N2 200 ml min SPN2 Ethylene 150 ml min Ethylene MFC SP Ethylene 150 ml min SPEthylene Methane 200 ml min Methane MFC SP Methane 200 ml min SPMethane Valvel Valve2 RC TEMP Output RC TEMP HB TEMP Output HB TEMP PUMPO1 Purga2 MFC S
64. e are discrepancies notify Process Integral Development Eng amp 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 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 AN 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 only be possible if they have been chosen as a configuration option of the Microactivity Reference reactor 12 PID Engatech 1 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 of the reactors hot box as shown in Figure 3 1 3 NZ Figure 3 1 2 Installation of the liquids pump Before installing the pump make sure the on off switch to be found on the rear of the pump is in
65. e 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 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 2 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 91 PID Eng amp Tech 3 A FUSE Figure 7 2 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 porous plate of the reactor could get blocked identifying this fa
66. e devices represented by displays of this kind is as follows DEVICE dda BY PASS PELTIER DOOR INHIBITION F By pass reactor E Activated The programmed sequence of isolated sessions is interrupted Condenser without Deactivated The programmed sequence of No by pass i Closed i cooling sessions is followed Table 5 1 The process screen displays the process status at any given moment and therefore it is not possible to modify the parameters of the devices on it in the version Process 1 0 To do so either carry out the modification on the Session Configuration Panel or directly modify the hardware directly via the TOHO controllers or by means of the touch screen that is part of the Microactivity Reference unit 5 For opening a new process screen click on the button is 5 4 4 THE PROCESS CONTROL GRAPHS The process control graphs are graphic windows in which the current process values acquired by the control software are plotted in real time When a new experiment is created two graphs will automatically appear in the upper right hand corner of the PC screen In these the x axis represents the relative time elapsed since the start of data acquisition and the y axis represents The process values of the controlled variables upper graph The control outlet of the controlled variables lower graph 14 PID Eng amp Tech 000001 Nombre Catalizador Nombre Ensayo MicroactivityReference Proceso m i Ga
67. e 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 instruments 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 O600 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 16 stainless steel Valcon T rotor material 9 actuator valve separation with AT60 high temperature actuator 65 PID EngaTech 4 8 CONTROL OF PROCESSES AND AUTOMATION 4 8 1 CONTROL LOOPS FOR THE MICROACTIVITY REFERENCE The Microactivity Reference reactor uses closed loop controllers with propor
68. eactor is housed in an oven built without insulation consisting of a 304 stainless steel chassis with the inside housing the resistance together with a refractory material 800 W 220 VAC Maximum operating 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 whose interior holds an electric convection heater Its maximum recommended operating temperature is 190 C 19 PID EngaTech 4 2 THE CONTROLLERS 4 2 1 THE REGULATION PARAMETERS The Microactivity Reference unit uses P I D controllers for the following control loops Control of reaction temperature The signal from the thermocouple located in the catalyst bed is assessed 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 0 and 200 VAC typically between O and 140 VAC proportional to the control signal Control of hot box temperature The signal from the thermocouple located inside the hot box is assessed 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 assessed by the controller where
69. ed in the Check the alarm and reset it providing the system that has shutdown the system s situation that triggered it has been liquid inlet resolved Verify all the liquid inlet lines on the system A blockage of solid deposits has formed in the evaporator Replace the evaporator No liquid is entering the reactor Pressure of the head significantly above operating pressure Faulty operation of the liquid non return Verify the status of the non return valves valve and if necessary replace An alarm has been triggered in the Check the alarm and reset it providing the system that has shutdown the system s situation that triggered it has been liquid inlet resolved 100 PID EngaTech 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 TOHO reaction temperature Introduce the factory set default parameters The reactor s temperature reading l ne controller has been configured in the controller If
70. en or Close the valve s new zero setting point at which the system s gas outlet ceases to bubble If the buttons 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 on memory S8 N turns selector 2 Z switch Valve zero point 1 P switch Potentiometer zero point Micro switch Close 1 gt Ve ve gt 1e te Ve Pe Pe Pe Fe re Pe e i gt Fe gt gt Micro switch Open IM481H Figure 4 24 To return to the initial default zero setting 2 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 49 PID Engatech e Selecting the number of turns S8 This parameter represents the number of turns that the valve is going to do from the 0 to the 100 of output control from totally closed to totally opened By defau
71. enser refrigeration Peltier 0 OFF e 1 ON Hot box door Door 0 Closed 1 Opened By pass valve position ByPass e 0 Reactor position 1 Reactor by passed Gas 3 flow ml min MicroS S Micro3 o MicroS S MicroS S MicroS o Micro3CCSCSC d MMFC SPG Gas 6 flow ml min Actuator Switch S1 S1 0 Deactivated e 1 Activated Actuator Switch S1 S2 0 Deactivated e 1 Activated Actuator Switch S1 3 0 Deactivated e 1 Activated Chromatography cycle ChromOn e 0 Deactivated 1 Activated Time for chromatography cycle time between two analysis Cytime in seconds S SV1 Ramping Time Set Point Control mode REACTOR Auto Manual 0 Automatic Run 1 Manual Man Control mode 1 Manual Man PRESSURE SetPoit o Pressure set point C S CCid Control mode 1 Manual Man PRESSURE Outbut C O utput control in manual mode PRESSURE Proportional Band Proportional band _ _ o PRESSURE integralTime _ Integraltime S O PRESSURE DerivateTime _ Dervatetime S PRESSURE WHlmt Upper limit of the output control o PRESSURE MWhLllmt Ss Lower limit of the output control S Control mode LEVEL Auto Manual e 0 Automatic Run 1 Manual Man Output control in manual mode PUMP __ o d SetPoint Liquid flow mminy o PPUMPO Ro Tumne pump ta o PUMP o Sdo Tumoff the pump put 1 o Table 5 1
72. eptacle grounding should be verified Make sure the unit is connected to a dedicated receptacle 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 appropriated voltage option for the unit The voltage requirements for the equipment are printed near the power cord attachment Voltage 220 VAC 5 Frequency 50 Hz 1 Max power consumption 2000 W 11 PID Engatech 3 1 5 GAS REQUIREMENTS Make sure your lab has the appropriated 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 to the working pressure on the unit and appropriated to the mass flow controllers that the unit incorporates 3 2 EQUIPMENT INSTALLATION Before starting be sure to have available all the tools and pieces necessary 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 Keep all shipping materials for inspection by the carrier Check the items received against the packing lists If ther
73. ess 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 23 PID EngaTech control loops are the trial and error method test error test and the ultimate gain method developed by Ziegler amp Nichols 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 data on the processes 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 It allows for calculating the t
74. f 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 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 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 gap must be configured at O ml min PAS SF WLS bl i eee ee es 2 MAS FLOR UNIT NAME AL Cx MEG CH MET FAs ELOR DELAY TIME ALAR Figure 4 9 Press the Exit key to return to the main menu TEMPERATURE ALARMS Set up menu for the temperature alarms 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 determines the following 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
75. g pressure and backpressure at 21 C of 206 bar 3000 psig Trigger pressure of 25 psi Operating temperature of 23 C at 191 C Cy 0 1 0 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 Long hexagonal male coupling SG SS HLN 2 00 316 Stainless steel Size both NPT male threads 1 8 Length 2 interior diameter 0 19 61 PID EngaTech Operating pressure as per ANSI for 31B 3 pressurised piping of 9400 psig This piece is used for connecting the joint on the liquid check valve SS 2C4 KZ 25 and the hot box and its purpose is to transmit the temperature of the hot box to the non return valve as a result of its relatively high mass solid piece 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 35 CHECK VALVE FOR LIQUID FEEDING LOW DEAD VOLUME SYSTEM SWAGELOK SS HLN 2 00 HOKE 1CF2 316 HOKE 1CM2 316 SWAGELOK SS 2C4 KZ 25 7 5 8 5 82 _ k 25 4 75 8 SS i 1 4 75 ks 6 Figure 4 35 Figure 4 36 shows the Teflon pieces designed to eliminate the liquid non return valve s dead volume Figure 4 36 3 port T conne
76. gure 4 7 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 Pr ArceE lt AL ARM TEMBER ATURERREAS ORs SEE rile TEMPERATURE HOT BOX OFPEM REACTOR PRESSURE JPRES SURE SER LEVEL ee gel toy cee MASS FLOWS IMHIBITION RESET BUZZER RESET ALARM Figure 4 7 32 O PID Engatech Temperature Reactor The reactor temperature exceeds the maximum limit specified in its controller Temperature Hot Box The hot box temperature exceeds the maximum limit specified in its controller By default this limit is set at 40 C with this being the temperature above which forced convection will be 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 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 interrup
77. he Start Menu The installation assistant will take you through the various stages of the installation Finally you will be required to reboot the system The installation assistant will create a shortcut to Process on the Desktop 5 3 COMMUNICATION PARAMETERS CONFIGURATION The Microactivity Reference unit is configured by default with the communication parameters to connect it directly to the control PC The unit user has to check that these parameters are the appropriated ones in both units 5 3 1 COMMUNICATION PARAMETERS OF THE MA REF UNIT These parameters are shown in the screen Communication Setup of the touch screen main menu see section 4 5 2 of this manual By default the unit is configured with these parameters IP ADDRES 192 168 0 5 GATEWAY 192 168 0 1 IP MASK 255 255 255 0 TCP PORT 1234 When the connection is made via Ethernet the user has to modify these parameters to adapt them to the local net 5 3 2 COMMUNICATION PARAMETERS OF THE PERSONAL COMPUTER To check these parameters in Windows operative system proceed as follows Click on the icon Network Connections with the right button of the mouse and select Properties 70 PID Engatech Click on the icon Local Area Connection with the right button of the mouse and select Properties Figure 5 1 s Network Connections File Edit Yiew Favorites Tools Advanced Help p 7 S p Search Key Folders
78. he 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 sensor 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 25 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 a a q 51 Sz Umbral 1 a Wt l Ci t RC Oscillating Circuit Oscillating Circuit behaviour Figure 4 25 This system s output signal is also proportional to the dielectric constant of the substance that acts as 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 51 PID EngaTe
79. his capability Otherwise you need to ask your network administrator for the appropriate IP settings O Obtain an IP address automatically IP address Subnet mask Default gateway Obtain ONS server address automatically Use the following ONS server addresses Preferred OMS server o0 58 0 100 Alternate OMS server oo 58 33 200 Figure 5 3 IP Address 192 168 0 1 Subset mask 255 255 255 0 Default Gateway 192 168 0 1 5 4 USE OF PROCESS 5 4 1 STARTING PROCESS APPLICATION To begin using the application click on the application Figure 5 4 Figure 5 4 The main functions bar will then be displayed This is the starting point for use of the entire application 5 4 2 THE FUNCTIONS BAR The functions bar is the first screen to appear when beginning to use the Process application and it is the tool that provides access to all the other functions for starting and ending acquisition creating experiments session control and so forth Figure 5 5 72 PID Eng amp Tech ProcessA Experiment Acquisition Sessions Profiles Data Help Ss 8 Sga Fala Bas S Not available Y Exit Process available Application configuration Stop acquisition devices Only available for advanced user level Open the process screen Open the control graphs Start acquisition New experiment Figure 5 5 5 4 3 THE PROCESS SCREEN Upon opening the Process application and creating an exper
80. hree 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 with Il 0 and D 0 whilst small disturbances are created until the process begins to oscillate continuously 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 I 60 6
81. ias Alias He Cancelar Units Select from the list Unidades one Decimal OT Aids mentens Limite Alto 1000 Alama Alta al Restaurar Limite Baog MoH Alarma Baja ae Color Figure 5 9 19 PID Engatech Decimal No decimals for the variable Upper Alarm Value of the variable above which the alarm will be triggered Lower Alarm Value of the variable below which the alarm will be triggered Colour Choose the colour of the variable s line in the graph Restore This restores the variable s default setting All changes made to the setting of the variables displays are stored in the memory by clicking on Accept Each one of the variables in the process graphs is depicted by means of a continuous line as per the colour of its corresponding display which shows the evolution of said variable over time The X and Y axes on the graph may be modified as follows gt Y axis this shows the upper and lower limits configured for each one of the variables The axis s numerical scale will at all times feature the colour of the variable whose limits it is featuring To switch from one variable to another simply click the mouse s left button on the display of the variable whose limits are to be called up gt X axis this shows a window of relative time elapsed since the start of data acquisition with the format dd mm yy h min sec The size of this time window may be modified by clicking on the x axis with the mo
82. iment see section Performing an experiment a screen will display a diagram of the Microactivity Reference unit featuring all the virtual devices that make up the control panel and which logically correspond to the real process hardware Two way digital communication takes place between them From the process information to the data acquisition application From the virtual or desired process information held in the computer s virtual devices to the hardware as depicted on the control panel MICROACTI ITY Reference Figure 5 6 73 PID Engatech The plant s different devices are represented by means of the following kind of displays the displays presented on the process screen will depend on the specific configuration of the Microactivity Reference unit 1 Displays that show the variable s current process value Mass flow controllers of the inlet gases Liquid flow pump He Scale for collection of condensable products 2 5 Process value Mass flow meter for outlet gases Pressure transducer DPX 2 Displays that show the variable s process value and set point Reactor temperature Hot box temperature Temp E EEA A System pressure Level in liquid gas separator Output control Evaporator 3 Displays that show the on off status of the device By pass Peltier Door Inhibition function VICI extra valves V1 V2 etc The status of th
83. improve the system s performance 4 7 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 thickness of 0 02 and at a temperature of 316 C The pipes selected that constitute the reactor are Pipe TSS285 1 8 pipe with internal diameter of 2 1 mm 0 085 Declared standards EN 10204 3 1B DIN50049 2 2 Pipe TSS120 1 16 pipe with internal diameter of 0 50 mm 0 020 Declared standards EN 10204 3 1B DIN50049 2 2 4 7 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 operatin
84. ions Ble Help ss 88 RAS hE siai A eini 6 UO Orit Figure 5 22 This list contains all the alarms and events starting sessions devices activation etc that have taken place during the acquisition time Figure 5 23 85 All Event List ony none whe al 1142 2006 9 15 40 AM 11 2 2006 9 15 50 AM 11 2 2006 9 16 01 4M 11 2 2006 9 16 01 4M 1142 2006 9 16 01 AM 11 2 2006 9 16 41 AM 11 2 2006 9 16 44 4M 11 2 2006 9 16 44 4M 11 2 2006 9 16 51 AM 11 2 2006 9 16 51 4M 11 2 2006 9 16 55 4M 11 2 2006 9 16 57 4M 11 2 2006 9 16 57 4M 11 2 2006 9 17 07 AM 11 2 2006 9 17 07 AM 1142 2006 9 17 18 AM 11 2 2006 9 18 18 AM PID Engatech Description Event Session 1 Stop execute Session 1 Stop execute Door Sensor Activate Reactor Sensor Activate Software Inhibition Activate Session 1 Stop execute Reactor Sensor Deactivate Software Inhibition Deactivate Door Sensor Deactivate Software Inhibition Activate Session 2 Start execute Door Sensor Activate Reactor Sensor Activate Reactor Sensor Deactivate Software Inhibition Deactivate Door Sensor Deactivate Hot Box Temperature Alarm Activate Cancel Help Figure 5 23 5 6 CONNECTION TO A GAS CHROMATOGRAPH The Microactivity Reference unit is prepared for connecting to a gas chromatograph actuating the sampling injection valve for starting the analysis Both devices external alarm and chromatography will be connected to the Microactivity Reference using the w
85. iquid outlet a Back Pressure Regulator that generates a outlet pressure of 34 35 bar 44 PID EngaTech 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 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 pulse gas flow inside the reactor several different alternatives that are used commercially in systems like 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 pulse 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 when microdroplets of condensate may accumulate on the control valve s orific
86. ire External Control provided by PID Eng amp Tech with the unit gt Connector EXTERNAL CONTROL BINDER 680 female 6 pin 00000 0 PIN 1 PIN 2 PIN 3 PIN 4 PIN 5 PIN 6 Chromatograph contact BROWN Chromatograph contact WHITE Emergency contact Emergency contact Without cable Without cable YELLOW GREEN 1 CONNECTION TO AN EXTERNAL ALARM The connection to an external alarm gas detectors etc has to be made with the wires yellow and green The contact is normally opened The two wires have to be connected to a relay that is opened normally and closes when the alarm activates The actions that the unit makes when an external alarm appears are the following Reactor Furnace Hot box Heaters Inhibition Session Buzzer OFF OFF ON ON The actions of the external alarm on the MFC and the pump of liquids are the same ones that the configured by the user in the touch screen for a pressure alarm When the external alarm disappears the unit returns to the operation conditions 86 PID Engatech 2 CONNECTION TO A GAS CHROMATOGRAPH The connection to the chromatograph will be made with the cables brown and white The MA Ref unit has to be connected to the Remote Control connector of the GC The contact is normally opened closing itself during 1 second when a pulse is sent to the chromatograph Operation It is possible to activate a cycle to actuate upon a gas
87. istributor 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 94 PID EngaTech MASS FLOW SETUP TEMPERATURE ALARMS PRESSURE ALARMS LEYEL SETUF HIS SETUP COMMUNICATIONS SETUP ABOUT PID ALMIN SE Ter Figure 7 5 Press on the field WASS FLOW SETUP The configuration menu for the mass flow controllers will be displayed MFM MAs FLOR Figure 7 6 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 e
88. ium compressed air etc Place a 1 16 plug in the liquid outlet Switch on the Microactivity Reference unit For a graphic display of the liquid level in the tank during calibration press the key F1 Level Setup and Play on the touch screen LEE es ee oe MAS LEVEL fiREE RE LEVEI 224567 Frequency of oscillation MIN LEVEL PEREIS LEVEL 3 qa on the level sensor Hz FARE E aa a amp LIQUID K Bebe LIQUID K REF 123 PLAY When plotting of the graph starts STOP is then displayed Figure 4 29 55 PID Engatech Calibrating the sensor with deionised water dielectric constant 80 1 O Select the reference liquid liquid used to calibrate the device press the button LIQUID K REF and select the liquid in the list represented in Figure 4 30 If the reference liquid does not appear on the list select the option OTHER and introduce its dielectric constant in the yellow background field LEWEL SENSOR CALIBRATION REF Hexane ss carb tetrachloride Heptane Dichloromethane Hexadecane 1 2 Dichloroethane Acetic acid Deionized water Ethanol Methanol MURUN 25 seers isopropanol othe EE RETURN Figure 4 30 Press the RETURN key to return to the level sensor calibration screen Select the condensed liquid that in this case is the liquid used in the calibration reference liquid Proceed as described before press the LIQUID K button
89. joint between the uncontrollably without responding gas inlet line and the reactor and see to the set point with the 3 port whether the pressure decreases If it does valve in the reaction position 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 through the filter and see whether the pressure decreases If it does replace the filter If it does not continue by verifying the next cause Restore the optimum control parameters for this controller see the section The controllers in this manual The reactor s porous plate is blocked The filter on the reactor gas inlet is blocked The controller s PID parameters have been modified Incorrect operation of the level control Stop feeding liquids into 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 The pressure in the system varies without stabilising at the set point modified Configuration of the Servo Digital V4 0 unit in the manual I
90. key to return to the main menu 34 PID Engatech Sd a Ue S ee a tod ed eee Se F ri MFC CH1 Wee i dele FREE LIaUID PUMP FREE Figure 4 10 m PRESSURE ALARMS Set up menu for the pressure alarms a I I a E a E a MFE CHi BEREE FREE _IGUID PUMP Figure 4 11 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 OFF 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 35 PID Engatech LEVEL SETUP Set up screen for the level sensor for equipment with this option The description of this screen and the procedure for making the level sensor calibration is described in the section 4 6 3 3 of this manual SiS Se e MAX LEVEL FEREHE LEVEL 1234567 MIN LEVEL ERREEN LEVELCH 125 Figure 4 12 Press the Exit key to return to the main menu 7 MISCELLANEOUS SETUP For setting up the following parameters Fea Feed ste eo er aera OUTPUT MANUAL SET Pole Auto AUs2 MANUAL OUTPUT CMANUALS SET POINTCAUT gt Figure 4 13 HEATER Heating of the system s gas outlet line The heater control can be set as o Heater Manual B
91. king 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 Restore the controller to its original parameters Replace the level sensor contact the distributor Disconnect the equipment switch 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 sen
92. l 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 gt INH Inhibition function Whenever the INH function is activated by any one of the system s alarms the Process 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 forthcoming 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 all the MFC the liquid pump triggering the audible alarm buzzer and generating the system s inhibition signal 68 PID Engatech SUMMARY TABLE OF THE ALARM FUNCTIONS ALARM TYPE HOT BOX CONVECTOR REACTANTS MFC s INERTS MFC s LIQUIDS PUMP toa m m h h l x OFF OFF LEVEL SERVO CONTROL O ai TI TI TI O 3 ll OFF
93. 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 controller s _nd parameter to or Rdy instead of to automatic automatic 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 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 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 There is no reading of the connection Verify the status of the source by The power source
94. lp Figure 5 11 This screen allows for setting the following characteristics or parameters of the experiment that is to be carried out Name of the catalyst used Name of the test Equipment in which it is to be performed Name of the head researcher All these parameters may be set by clicking on the icon l that is to the right of each one of them thereby accessing the following screens 77 PID Engatech w Microor mE Microor fC felix w Microor DB Seleccionar Seleccionar Seleccionar MicroactivityReference 10 MicroactivityReference2 SiC Nombre Catalizador Agregar Nuevo Agregar Nuevo Agregar Nuevo Screen for defining the name Screen for defining the name Screen for defining the of the catalyst of the test equipment Figure 5 12 Each one of these screens will call up a list with the different catalyst and test names as well as the different equipment or devices that are controlled by the system 1 2 etc To select each one of these simply use the left button on the mouse to select the desired option and click on the button Select In the event that the desired name is not featured on the list a new one may be created by means of the function Add new Once all the fields have been selected click on Accept on the experiment definition screen This screen includes a space where on an optional basis a description of the experiment or some other further observation m
95. lt 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 operation 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 have to open the 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 the 20 to the 65 for controlling the desired pressure For changing the number of turns proceed as following Localize the dip switch S8 of the driver see Figure 4 24 Check that the switch 4 on dip switch S8 is on the Off position see Figure 4 24 The number of turns is determined with switches 1 2 on 3 on dip switch S8 No OF TURNS _ as o on O z O z off 6 E Turn off the unit With the help of a screwdriver change the position of the switches 1 2 and 3 according with the table above Turn on the unit again Now the valve is configured with the new number of turns 50 PID Engatech 4 6 3 LEVEL CONTROL IN THE LIQUID GAS SEPARATOR 4 6 3 1 Introduction to level control in microa
96. lush 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 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 l 16 Engatech COMPONENTS OF THE MICROACTIVITY REFERENCE UNIT 4 Figure 4 1 shows a diagram of the items that constitute the Microactivity Reference reactor s arrangement of lines and instrumentation 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 agg ee ey tom Te fal frei ey roo TOT Oo Bae E fh re Asi Hane Ines ou tao CTT JEMIMEE re HT ZAJA H TOBLETIETAT Peer a AD ih A Amai ab Fa a A AENDELEE ai Pi pea E APR aE TPA aoe Amea ie A 2 mtia Eie Ena E Ei kne E ALS ENEL Her Lede E Wi Tei Soe To oe Zdr EE Lae ks UL ast ain SISTA AD ethan AD JEO
97. lves 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 PID EngaTech Once the gases 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
98. mportant to be reasonably accurate when setting zero on the instrument and to do so the system must be empty although it will have previously been moistened with the product to be measured Once zero has been set on the instrument it can be verified whether the instrument s output signal is directly proportional to the height of the liquid in the tank In the case of fluids with a low dielectric constant it is important to be reasonably accurate when setting the instrument s zero or baseline To do so the system must be empty although it will have previously been moistened with the product to be measured For control purposes the microprocessor converts the output signal into an analogue signal that can be understood by the control instruments Typically this is a 4 20 mA signal Accordingly all that is required is to indicate to the instrument that 31 000 Hz corresponds to an output of 4 mA and for example 50 000 Hz corresponds to an output of 20 mA As of that moment the instrument provides a 4 20 mA output signal proportional to the height of the liquid in the tank without considering geometric issues in the design of the tank 60 PID EngaTech 4 7 OTHER COMPONENTS ON 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
99. munications via Ethernet by means of the Process control application The equipment s 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 EngaTech 2 2 SPECIFICATIONS Microactivity Reference EN 61326 1997 Ambient temperature range for operating 5 40 C Ambient temperature range for storing 20 70 C Recommended humidity range 5 80 Forced ventilation or convective Refrigeration ae 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 li
100. must have the same format for each cell number with without decimals date time etc as the data that have been imported Once the data are recovered exit this Process session If the user wants to recover another old experiment he has to open a new software session Figure 5 4 5 5 5 SAVING EXPERIMENT TEMPLATES The templates generated for performing an experiment may be stored for subsequent recovery and use Proceed as follows to store a template in the memory 1 Stop acquisition 2 On the functions bar select Experiment 3 Select the option Save Experiment as A window will appear on the screen like the one shown in Figure 5 21 where the user may allocate a name to the template to be saved Complete the saving process by clicking on Accept Template Name Cancel Help Figure 5 21 Saving an experiment template stores the following for subsequent use The session configuration panel The configuration of each one of the devices in the process control graphs The acquisition time To recover a template stored in the memory simply select the name of the required template when creating a new experiment see section 5 4 1 in this manual 5 5 6 CHECKING THE ALARMS All events and alarms are recorded in a list that can be consulted by the user select Data Alatms as is shown in Figure 5 22 000020_ Catalyst Name _ Assay Name MicroactivityReference Experiment Acquisition Sess
101. n installed This value can not be modified manually by the user 1 Additional control options for special configurations of the unit 2 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 Its P I D 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 Fi
102. nce the system is calibrated select in the field LIQUID K on the LEVEL SENSOR SETUP screen the fluid that is going to condense on se liquid gas separator If that liquid is not in the list select OTHER and set the dielectric constant or an estimation on the yellow field Press the RETURN key to return to the level sensor calibration screen In this moment the field MAX LEVEL changes depending on the relation between the dielectric constants of the reference liquid calibration liquid and the actual At this point the level controller gives a REAL reading of the level of liquid K inside the liquid gas separator in ml Table 4 5 lists the dielectric constants at 20 C for different compounds 59 PID EngaTech COMPOUND FORMULA e 20 C Hexane Heptane Hexadecane Carbon tetrachloride Toluene Acetic acid Dichloromethane 1 2 Dichloroethane lsopropanol Ethanol Methanol Glycerol Deionised water Table 4 5 The signal provided by the RC oscillator circuit prior to being converted into an 4 20 mA analogue signal may vary between 31 000 90 000 Hz for water 31 000 50 000 Hz for an alcohol 31 000 32 000 Hz for a hydrocarbon In a situation such as this a zero error on the instrument of for example 50 Hz is insignificant in the case of fluids with a high dielectric constant yet crucial in the case of fluids with a low dielectric constant It is therefore i
103. nearity in the sensor s response to the quantity of liquid present in the system Figure 4 32 and Figure 4 33 show the sensor s response to consecutive additions of 0 5 ml of different substances Oscillation Frequency Hz Vs Volume ml N gt O Cc O 2 LL Cc 2 amp O v O Volume ml Figure 4 32 Oscillation Frequency Hz Vs Volume ml Dichloromethane 1 2 Dichloroethane lsopropanol Ethanol Methanol Glycerol Deionised water Acetic Acid Hexane Heptane Hexadecane Toluene Carbon tetrachloride Oscillation Frequency HZ 1 1 5 Volume ml Figure 4 33 58 PID EngaTech An analysis of the ratio existing between the oscillation frequency of the level sensor difference between the response to the addition of 2 ml of a compound and the threshold and its relative dielectric constant shows that said response is almost perfectly linear for the whole range of dielectric constants see Figure 4 34 N gt O G oO _ LL 2 _ T O e2 O SF 789 94 378 18 R 0 9994 Figure 4 34 This performance by the sensor enables a calculation to be made of the expected response for a specific compound in terms of its dielectric constant without the need to calibrate the system with the new compound and based on the calibration with water that is factory set Accordingly proceed as follows O
104. ning 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 Engatech 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 most 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 It 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 higher than 25 give
105. nsufficient gas pressure is reaching the Make sure the gas inlet pressure on the The pressure in the system does equipment equipment exceeds the operating pressure not reach the set point stabilising 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 102 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 continuously 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 EngaTech 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 The sensor is not wor
106. on the system s touch screen It is self locking in order to avoid a repetitive cycle of the system in 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 gt Level alarm Alarm configured by the parameter _E1H on the level controller It is absolute type and interrupts the operation of the liquids pump 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 Contro
107. ormation of condensates in the orifice Dyna Pak gasket which ensures the tight sealing of the rod without major compression on 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 this 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 major hardness and resistance to distortion Once it has been distorted by continuous use of the valve this disc may be replaced as often as necessary The manufacturer s original Cy curve may be seen in Figure 4 22 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 46 PID EngaTech NUMBER OF TURNS OF VALVE HANDLE 002 004 006 008 010 012 014 016 018 020
108. pressure control optional 10 um filter Figure 2 4 2 4 4 REAR VIEW lt 4 Scale optional lt 4 HPLC liquid pump optional Liquid gas separator with level sensor and micrometric servo controlled valve optional Ethernet remote contro General protection 220 VAC Power supply Figure 2 5 2 4 55 INSIDE VIEW ELECTRONICS Digital Seervo V4 0 for pressure control opt 6 Port Valve Micrometric valve for pressure control opt Pressure sensor opt PID EngaTech 12 V Power Supply 15 15 5V Power Supply 24 V Power Supply Digital servo V4 0 for level control opt Scale communications card opt SSR Furnace SSR Hot Box Heaters SSR GC Heater Electrovalves Gas Mixer Mass Flow Controllers PID Engatech 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 The site is well ventilated and free of corrosive materials and overhanging obstacles O 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 Power receptacle is earth grounded Electrical supply meets all equipment s power requirements Voltage
109. quids 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 A PC 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 EngaTech 2 4 1 GENERAL VIEW Online GC analysis not included HPLC liquid pump optional Control PC Microactivity Reference unit Figure 2 2 2 4 2 FRONT VIEW Hot box door Touch screeen Pressure transductor for atmospheric pressure units 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 10 um filter Liquid evaporator Autoclave Engineers tubular reactor 6 port VICI VALCO valve for reactor by passing Reactor furnace Extra 6 port valve optional Micrometric servo controlled valve for
110. r 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 eS eS OPErati on OF WGW Wrong screen Verify the configuration of the PC s IP address local area network Reboot both systems ETERNO Comndnieaiey Reboot the equipment If the problem between the reactor and the touch Blocking of the microprocessor eae we GEE persists please contact the distributor Check the gas installation and make sure nei en EAE the system s air inlet pressure is 5 bar The door on the reactor does not y p open and on the by pass valve Leaks in the compressed air lines or Disconnect the equipment switch the circuit breaker to OFF unscrew the right and left P eS TO Opra AET a rine pheumaNG hand side panels on the equipment and check the orange polyurethane pipes No communication is established between the reactor and the control PC l Check the gas installation and make sure No gas pressure reaches the equipment the gas cylinders are open The on off stopcocks on the front panel Open the on off stopcocks are off 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
111. reactor Operator Operator that is to be used in the condition gt lt gt lt Value Value of the variable upon which the condition is set e g 500 C Index of next session No of the session with which the link up is to be made 1 2 3 etc The next step is to define the status that is to apply to each variable in the different process sessions The variables with their different options are as shown in Table 5 1 The upper part of the session configuration panels features the session control keys that are detailed below PLAY Launch session no 1 E E PAUSE Pause the sequence of sessions session time continues to run but no jump is made to the next session STOP Stop the sequence of sessions First session Display is made in the window of the experiment s first session no 1 but this is not performed until the button PLAY is pressed E E Prior session Display is made in the window of the experiment s prior session but this is not performed until the button PLAY is pressed 5 a Subsequent session Display is made in the window of the experiment s subsequent session but this is not performed until the button PLAY is pressed E Final session Display is made in the window of the experiments final session no 100 but this is not performed until the button PLAY is pressed E 81 PID EngaTech DISPOSITIVE PROPERTY CHARACTERISTICS Cond
112. rmed 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 singularity that too long will have been spent waiting to undertake 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 I 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 l 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 26 PID EngaTech pilot systems are very high due to the imme
113. roactivity 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 proceed 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 52 Engatech DISENO DEL CONDENSADOR LIQUIDO GAS CON SENSOR DE NIVEL A 6 OC A 3 TEFLON v N D 6 S TEFL N lt A 2 3 NPT 1 4 A s ae es TEFLON Vv Vv Y he NPT 1 4 lt gt 4 KK NPT 1 8 gt BXM3 Nn Tt X 8 5 A 67 5 NPT 1 8 4 2 g B NPT 1 8 PROYECTO MICROACTIVITY REFERENCE y AUTOR PID Eng amp Tech y ESCALA 1 1 MATERIAL AISI 316 Figure 4 26 53 PID Engatech Capaci
114. rogrammed to open and close during a method run They can also be opened and closed manually The default state is open 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 to be introduced and following these steps Adjust the syringe on the upper part of the 3 port valve With the valve in the position load syringe Figure 4 20 position no 1 draw on the syringe s plunger thereby introducing liquid inside removing air bubbles from the feed line Set the valve to the position Injection from syringe Figure 4 20 position no 2 and press the Prime key on the keyboard The pump will then begin to pump liquid at its maximum speed Press the plunger on the syringe until no air bubbles can be seen at the pump inlet and liquid reaches the outlet Set the valve to i
115. rror 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 lf 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 vice versa by pressing the soft key Change 42 PID EngaTech 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 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 p
116. s ie IbIHiAl bd IbiLoAl CI j PMP1 100 IbIHiAl d 5 IbIHiAI d ibiLosl f o IbiLaal CI a 0 6000 400 4 oom 100 inal CO IbIHi o Scroll ibilal Call o ibiLeal CI 320 4 Cursor F 51 W 240 IEY oes Hai 5 50 bIHiAl CI A AICI oO IkiLoAl CI Aan 160 80 F Q l l eaaa itoa sail 2185 DEN MARN ioe ee RE 000001_ Nombre Catalizador Nombre Ensayo MicroactivityReference Control 59 0654 49 0654 39 0654 29 0654 19 0654 9 06542 0 934579 Zoom Cursor 14 12 05 15 36 00 14 12 05 16 48 00 14 12 05 18 00 00 14 12 05 19 12 00 Figure 5 7 As soon as data acquisition starts the graphs will begin to plot the process values of the controlled variables Each one of these variables is represented by a display to the right of the control graphs with the following appearance Variable represented Colour of the variable s line plotted in the graph Upper and lower limits for plotting in the graph Upper and lower alarm limits Activation xf or deactivation X of the Process value variable s plotting in the graph Figure 5 8 By moving the cursor over the display and clicking the right button on the mouse access is gained to the set up window for the chosen variable The set up options are as follows Configuraci n de Yariable Variable Name Nombre MFE PW Micro3 Al
117. 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 also be known As has been noted on several occasions pilot plant operation involves a 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 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 perfo
118. sor 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 controller s _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 liquid The level controller is set to manual fully closed 0 A blockage has formed in the liquid 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 controllers _nd parameter to 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
119. ssure control system Range of operating pressures atmospheric 100 bar Control accuracy 0 1 bar Variations in gas flow at the reactor outlet lt 5 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 47 PID EngaTech 4 6 2 3 Configuration of the Servo Digital V4 0 unit microstep positioner The Servo Digital V4 0 microstep positioner that is part of the pressure and level control systems on the Microactivity Reference units are factory set with the optimum parameters for the equipment s correct operation which means that in principle 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 23 OPEN CLOSE S6 ADDRESS J6 ANALOG INPUTS S1 ZERO J4 ZERO SENSOR POTENCIOMETER LED S J7 RS 485 2 S3 S4 ANALOG J3 MOTOR INPUTS CONFIGURATION S7 TERMINAL RESISTOR 90o00o0o0n0d0 eo00000000 J1 15 VDC INPUT u 1 py R17 MOTOR e Rew CURRENT LIMIT 0 0 0 OL a 7a
120. supply is adequate for oven type 1Gas supplies meet the requirements of the equipment 1Gases 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 Recommended temperature range 18 25 C Temperature range 5 40 C Recommended humidity range 50 60 Humidity range 5 80 Recommended 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 10 PID Eng amp Tech 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 70 cm Height Width 60 cm Depth 55 cm Depth Width 3 1 4 ELECTRICAL REQUIREMENTS 3 1 4 1 Grounding AN 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 rec
121. the condenser Liquid Valve o Sensor for the level of liquids in the condenser Level Sensor 5 Gas outlet on the system Leading to the analysis system A heater is included for this line see Figure 3 5 Gas outlet Heater connector HW Figure 3 5 Heater 6 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 6 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 6 7 The reactors power socket is on the lower rear of the reactor Figure 3 7 WARNING Before connecting the equipment s power supply make sure that the main circuit breaker is in the OFF position Figure 3 8 CEPA Gat POWER SUPPLY Figure 3 7 Figure 3 8 15 3 2 4 GAS INSTALLATION PID Engatech 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 87 line preferably of 316 stainless steel between the pressure reducers on the gas cylinders and the system s gas inlet which is
122. 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 on the Mode button 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 Current surge due to a short circuit Reboot the device ee Pressure is being applied to the device Carry out the adjustment of the zero at during the adjustment of the zero setting setting at atmospheric pressure The pressure applied exceeds the upper limit N of the pressure range that can be shown The pressure applied must be within l 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 EngaTech 4 5 THE TOUCH SCREEN The Microactivity Reference unit has a touch screen which allows for adjusting the various process parameters displa
123. the off position o Figure 3 2 Figure 3 2 The following connections are to be made see Figure 3 3 a Connect the power cable to one of the two 220 VAC power sockets on the rear 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 need to operate separately from the Microactivity Reference unit b Connect the connection terminal stop for system alarm as well as the sub D connector digital communications on the rear of the pump c Connect the round connector on the end of this same cable to the Pump Control on the rear of the Microactivity Reference 13 PID EngaTech Figure 3 3 3 Installation of the liquid scale see Figure 3 4 a Connect the sub D type connector digital communications to the rear of the scale b To the left of the sub D connector connect the JACK type plug power supply c These two connectors are joined in a single round connector that has to be plugged into the corresponding socket on the rear of the hot box Scale Control Figure 3 4 14 PID Engatech 4 Other components On the rear 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 Mass flow meter MFM o Valve for regulating the level of liquids in
124. these are not known is incorrect ae incorrectly please 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 C on the hot box s temperature controller which it starts operating SET 2 menu on the controller Th The hot box s temperature controller has Set the control mode to automatic Run on e electric heater on the hot box i i been set to manual at 0 the controllers _nd parameter doce NOt opetata 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
125. ting 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 Reactor Detection of open oven Pressure Servo Alarm in the Digital Servo of the micrometric valve for pressure regulation in the system 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 reactor s by pass valve Access is 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 ee peep e ey fol bl MASS FLOW SETUP UP gl ee ce Eel Bs Taio b PRESSURE ALARMS SER er ESENS ADMIN SETUP MISC SETUR ABOUT PID COMMUN IT CAT TONS T SETUR FEC TTILIER T CONTEOL Figure 4 8 33 PID EngaTech m 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 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 o Name ofthe gas o o
126. tional 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 manner 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 There is a third zero passage relay for the possible temperature control of a heating pad for heating the 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 rela
127. tive level sensor lt _ Condenser Regulating micrometric valve Condenser amp level sensor RnR Figure 4 27 4 6 3 3 Calibrating the level sensor All Microactivity Reference equipment that includes the level control option in the liquid gas separator is factory supplied with the level sensor calibrated with distilled water which means that the user should not calibrate it again when beginning to operate with the equipment In this state the TOHO level controller that is on the equipment s front panel will display the reading of the ml of water inside the separator at any given moment There is no need to calibrate the level sensor on a regular basis although it is advisable to perform a calibration whenever the user dismanitles any part of the liquid gas separator as well as whenever any anomalies are detected in the reading of the level inside In such cases proceed as follows Switch off the Microactivity Reference unit Loosen and remove the 3 connectors on the tank that are shown in Figure 4 28 in the following manner Gas outlet Gas Inlet Liquid outlet Figure 4 28 54 PID EngaTech o Use a 5 16 spanner to loosen and remove the liquid outlet connection on the tank O o Usea 7 16 spanner to loosen the gas inlet and outlet connections Place a container below the liquid outlet Clean and dry the tank to remove any possible dirt Cleaning may be performed by applying Hel
128. ts normal operating position Figure 4 20 position no 3 When no more air bubbles are observed at the outlet on the liquids pipe press the Stop function key to finish venting the pump Under normal operation plugging the end of the feed line will increase the pressure displayed on the message screen whilst the line is sealed and the pump is running Inlet oe Vassel 1 Syringe in load position y Pump B Liquid 2 Position for loading from syringe Inlet D Vessel For feed calibration seq o o Pump Yo Run position Te ra Pump Liquid 3 Normal operating position inlet filter 10 pm Inlet P Vessel Injection from tank Figure 4 20 43 PID EngaTech 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 will always
129. ue 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 each one of the digits and then use the A and YW keys to increase or decrease the value The standard set up for the Microactivity Reference reactor is detailed in Table 4 1 Control Reactor Hot box Pressure Level parameter temperature temperature es ee ee ee E ee ae Em 70 40 donotmodify Table 4 1 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 Engatech meacIOr PALRO Pressure Level Aux 1 Aux 2 Temperature Temperature Oo o o 2 2 E Table 4 2 P I D values depends on the operation conditions As a example in Table 4 3 are shown the PID parameters for the reactor oven depending on the working temperature Temp Reactor 200 400 500 600 ti rr ae o f 465 ooo 5o M Maij eoo S 5o Table 4 3 There now follows a brief introduction to the different methods that are used for tu
130. un 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 Ady Control start at a given moment When this mode is activated 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 RADY mode the LED RDY on the front is to remain off e _ nut The variable s control output 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 Val
131. use s left button The three function keys that are to be found on the right of the process graphs allows for configuring their display setting yy ZOOM It increases the size of the selected window Keep the left button on the mouse depressed and draw the required box oom scroll p SCROLL It allows for dragging the graph backwards and forwards Keep the left button on Cursor the mouse depressed and drag the graph CURSOR It shows the exact value of the variable at the point selected with the mouse click the mouse s left button on the control graph p DEFAULT To come back to the default display Each one of the functions is activated by clicking the mouse s left button on them and they remain activated until a further click is made whereupon the graphs normal setting is restored For opening a new control graph press the button 76 PID Engatech 5 5 PERFORMING AN EXPERIMENT 5 5 1 CREATING AN EXPERIMENT To create an experiment click on the icon on the process functions bar or select New Experiment ProcessA Seige Acquisition Sessions Data Help New experiment Save experiment 45 Load experiment Figure 5 10 The experiment definition screen will be displayed Define Experiment Catalyst Hame Assay Assay Name Equipment lEquipmert Nam Researche a a Researcher Researcher Namel Description Description Text Ok Cancel He
132. used Flow control adjustabk in mLimin from DOTH 100 of the mammum flow rate of the pump head being used Upto 999 loops with urdimited linking of files Storage for 10 user programs and four emor Ales with a madmum of 25 points ard timed events in each program Flow rate 10 pL min 10 raL rain Coefficient of variation 0 1 940 6 with aqueous solutions or hydro organic polar sovent mixtures 0 3 1 with hydrocarbons or chlorinated wolatile solvents Mamum accuracy error 1 with water over the full flow rate and pressure ranges 01 60 MPa 600 bar S700 pai depending on pump head used Accuracy lt 1 9 or 0 1 MPa 1 bar 15psi Repeatability lt 1 or 0 1 MPa i bar 15 pa Pulsation lt 1hwith water at 1 mLimin and pressure gt 4 MPa _ Dampener volume 0 6 mL at atmosphere pressure 1 6 mL at 60 MPa Mia Gilson UniPoint System Software _ FR 232 oF S100 four inputs and four relay outputs 2x character LOD Keypad and built in hep messages 3 16L stainless st titanium sapphire ruby PTFE PCTFE and HDPE Frequency S460 Hz Voltage 100 120 or 220 2400 mains voltage fluctuations not to enceed 109 ofthe nominal voltage Environmental Operating Temperature Manufacturing Standards Instrument Dimensions w xd x hj Instrument Weight with head mere _ Meets applicable Safety and EME certification standards CE certified 3403392 Semil3e 13x 5ini 11 5 kg 25 4 Ibs Shipping Weight withhead 15 4 kg 34
133. w value for each one of the controllers see the specific documentation for each MFC 99 PID EngaTech These sockets are not energised when the The pump is connected to the 220V equipment is switched off plug the pump sockets on the rear of the equipment into another socket separate from the unit or switch on the equipment The 3A 250V fuse in the fuse box on the Change the fuse PE rear panel has blown or is missing The Gilson liquid pump does not The pump s electrical installation has not See the section Electrical installation in ewitched ork been performed correctly this manual Turn the switch on the rear of the pump to the l position The Gilson liquid pump does not switch on with the Microactivity switched off The on off switch is in the 0 position The Gilson pump does not If a prior manual control has been made register the information or the set on the pump s display it is not possible points relayed to it from the to establish digital communication with Process software 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 Reboot the pump If this is not possible control of the same is to be maintained in manual mode The Gilson pump does not respond to the parameters that are manually entered into the display Reboot the pump If this
134. y default In this mode the user can set the output control of the heater in the Output manual gap 0 No heating 100 Maximum power of heating 36 PID EngaTech In this mode the controller does no attend to the P I parameters or 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 does not attend the output of control CAUTION If the unit does not incorporate this thermocouple the 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 heater must be plugged to the AUX2 connector on the rear panel of the unit The operation with this device is the same as has been described in the previous section HEAT Press the Exit key to return to the main menu n COMMUNICATIONS SETUP Set up parameters for the communications via Ethernet between the devices By default the unit is configured with the appropriated parameters to connecting it directly with the control PC with a crossed cable IP ADDRESS 192 168 0 5 IP MASK 255 255 255 0 GATEWAY 192 168 0 1 TCP PORT 1234 i a i a LM i CoA TT e E SE
135. ying 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 6 Pressing on the different icons and buttons grants access to the different functions Severe Figure 4 6 Buttons could 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 It 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 Engatech 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 bee
136. ys the 0 5 VDC control signals to the MFC The signal recognises the 0 5 VDC output signal from the MFC 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 8 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 66 PID Engatech 4 8 3 SYSTEM SAFETY MANAGEMENT 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

MICROACTIVITY - REFERENCE

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