CG-4600-01 - Chemglass Life Sciences
Contents
1. Ne 236 42 g 272 7 ml Ne 3 5 Vacuum Requirements The type of vacuum source 1 e a high vacuum pump aspirator or in house vacuum system has no affect on the regulators operation or performance The only requirement is that the vacuum source be lower in pressure than the pressure you want to regulate the equipment at That is to achieve a vacuum or 40 torr in the attached equipment the vacuum source must be at least 40 torr The Digital Vacuum Regulator doesn t create a vacuum it only regulates the vacuum from an external vacuum source 3 6 3 7 Using the Regulator for Vacuum Distillations This version of the vacuum regulator is intended for medium accuracy vacuum applications such as rotary evaporators We say medium accuracy applications because the regulator usually regulates pressure from 0 5 to 2 torr as opposed to a high accuracy regulator that controls pressure to better than 0 1 torr Some vacuum distillations are not affected by changes in pressure of 0 5 torr but many are This regulator is not recommended for small laboratory scale vacuum distillations Having said that we at J KEM know you re going to try it anyway so let us help you set the distillation up to deliver the best performance possible Points to follow 1 Use a precision needle valve available from J KEM between the vacuum pump and the vacuum regulator Adjust the opening of the valve after reaching the set point pressure of the distillat2. A keys until the pressure appears in the display and release both keys Deactivatine the Ramp to Setpoint Feature l Press and hold in both the V and A keys on the front of the meter until the word tunE appears in the display then release both keys A Press the A key 9 times until the word SPrn appears in the display This function turns the ramping feature ON and OFF First hold in the key then while holding in the key press the V or A key until OFF appears in the display then let go of all the keys 3 To exit programming mode press and hold in both the V and A keys until the pressure appears in the display and release both keys 3 4 Use with Rotary Evaporators Your vacuum regulator is ideally suited for use with rotary evaporators To demonstrate the simplicity of the regulator the following example is given 1 Set the Regulator Selection Switch 6 to the OFF position and then turn on power to the DVR Turn on the vacuum pump 2 Enter a set point into the regulator appropriate for the solvent being removed for example 300 torr for CH 2Cl2 3 Place the flask on the rotovap and move the regulator switch from the OFF to the METER position When in the OFF position the regulator isolates the rotovap from the vacuum pump so the rotovap can be open to the atmosphere while the pump is running When placed in the METER position the regulator evacuates the rotovap to the pressure entered into
3. if the unit shows evidence of having been tampered with or shows evidence of being damaged as a result of excessive vibration corrosive materials or misuse Components which wear or are damaged by misuse are not warranted This includes valves and fuses THERE ARE NO WARRANTIES EXCEPT AS STATED HEREIN THERE ARE NO OTHER WARRANTIES EXPRESSED OR IMPLIED INCLUDING BUT NOT LIMITED TO THE IMPLIED WARRANTIES OF MERCHANTABILITY AND OF FITNESS FOR A PARTICULAR PURPOSE IN NO EVENT SHALL J KEM SCIENTIFIC INC BE LIABLE FOR CONSEQUENTIAL INCIDENTAL OR SPECIAL DAMAGES THE BUYER S SOLE REMEDY FOR ANY BREACH OF THIS AGREEMENT BY J KEM SCIENTIFIC INC OR ANY BREACH OF ANY WARRANTY BY J KEM SCIENTIFIC INC SHALL NOT EXCEED THE PURCHASE PRICE PAID BY THE PURCHASER TO J KEM SCIENTIFIC INC FOR THE UNIT OR UNITS OF EQUIPMENT DIRECTLY AFFECTED BY SUCH BREACH Returns requests for service and inquires should be directed to J KEM Scientific Inc 6970 Olive Blvd St Louis MO 63130 314 863 5536 Fax 314 863 6070 Internet Catalog http www jkem com E mail jkem911 jkem com Section 1 Quick Operating Instructions Connect the Regulator to the Equipment Connect the vacuum pump or the vacuum source to the tube marked Inlet Note When the Digital Vacuum Regulator DVR is used on equipment smaller than a Rotovap a needle valve is needed for accurate regulation of pressure Place the valve on the inlet port see Section 3 2 Co
4. the meter 4 When the majority of the solvent is removed move the regulator switch from the METER to the FULL VACUUM position When in the FULL VACUUM position the regulator ignores the set point pressure and fully evacuates the rotovap removing the last amount of solvent 5 When all the solvent is removed place the regulator switch to the OFF position and remove the flask Place the next flask on the rotovap and move the regulator switch to the METER position to begin the process again For the entire rotary evaporation process the only action needed is to change the position of the regulator switch The pump can run continuously and there s no need to change the set point pressure Solvent recoveries from a typical rotary evaporator are shown in the table below Solvent Recovery from Rotary Evaporators using J KEM s Digital Vacuum Regulator Bath Weight of Solvent Weight of Solvent Percent Time To Regulator Temperature Placed on Rotary Recovered from Solvent Evaporate Flask Solvent Set Point C Evaporator Rotary Recovered to Dryness Evaporator ae o a d a i 0 2 s s 2 239 68 g 338 5 ml Ne 466 68 g 352 2 ml Ne J No 100 torr CH2C12 338 23 g 255 3 ml 336 42 g 99 5 Vacuum pump ultimate pressure 0 01 torr Test Conditions Buchi RE 111 evaporator equipped with a dry ice condenser All tests were conducted using a 500 ml round bottomed flask at the pressure shown 285 41 g 316 4 ml
5. In this position the equipment can be opened to the atmosphere while the vacuum pump is running Full Vacuum Opens the regulator continuously to the vacuum pump independent of set point pressure The pressure in the attached equipment is lowered to the limit achievable by the vacuum pump Optional serial port for remote PC control and data acquisition Warning J KEM s Model 200 Digital Vacuum Regulator should only be used with vacuums It is not designed to regulate pressures above atmospheric pressure Exposure to pressures above atmospheric pressure may result in damage to the regulator Section 3 3 1 How the Regulator Works The vacuum regulator consists of 3 important pieces The pressure transducer measures the pressure in the piece of equipment being regulated The process controller compares the pressure reading from the transducer with the set point pressure i e the desired pressure entered If the pressure in the equipment is greater than the set point the process controller opens the control valve allowing the vacuum pump to decrease the pressure in the equipment When the pressure in the equipment equals the set point pressure the process controller shuts the control valve preventing the vacuum pump from lowering the pressure any further The basic method of operation is very simple When the pressure in the equipment is above the set point the controller opens the control valve connecting the equipment to the vac
6. Temperature Control for Research and Industry Digital Vacuum Regulator User s Manual Model 200 M Scientific Inc Instruments for Science from Scientists T O T SSCS CPPS S SPST PSST EEEE TEETE RESP LELT EELL ELLELE ELLEELLE TELEL ELLECEI LRP Pe eer e eee eet eeree ieee eee TPP PCE CULE CPT eee CPR C CORT COP TTT ee DO TTRRU TCE Tee Teer TC errr reer err Terie eri teri INDEX SECTION PAGE 1 QUICK OPERATING INSTRUCTIONS _ 0 eee 3 2 REGULATOR DESCRIPTION eee 4 3 OPERATIONS GUIDE g252255088545 944052528 930 805454655525 2884 5 31 HowtheReg lator Works 25404 seseeiee veers ai eee A EE ts 5 3 2 Factors Affecting Vacuum Regulation Accuracy 5 3 3 Ramp to Setpoint amp Soak Feature 6 ee eee 6 3 4 Use with Rotary Evaporators eee 8 3 Nacom Requirements i24 s4e 32060 iaraa aaa a me evho vane faa 8 3 6 Using the Regulator for Vacuum Distillations 9 3 7 Correcting Offset in the Displayed Pressure 005 9 Warranty J KEM Scientific Inc warrants this unit to be free of defects in materials and workmanship and to give satisfactory service for a period of 6 months from date of purchase If the unit should malfunction it must be returned to the factory for evaluation Ifthe unit is found to be defective upon examination by J KEM it will be repaired or replaced at no charge However this WARRANTY is VOID
7. activated in programming mode Ramp to Setpoint feature remains active even if power is turned off to the controller Activating amp Programming the Ramp to Setpoint Feature Press the A key 8 times until the word SPrr appears in the display This is where you set the ramp rate in units of torr hour First hold in the key then while holding in the key press the V or A key until the desired ramp rate appears in the display then let go of all the keys Units are in torr hour 1 e mmHg hour Press the A key once and the word SPrn will appear in the display This function turns the ramping feature ON OFF or to Hold First hold in the key then while holding in the key press the V or A key until the desired setting appears in the display then let go of all the keys Press the A key once and the word SoaK will appear in the display This is where the soak time is set in units of Minutes A soak time of means to soak forever this setting is one below 0 First hold in the key then while holding in the key press the V or A key until the desired time appears in the display then let go of all the keys If a soak time is set the controller display will alternate between showing the current reactor pressure and the word StoP when the soak time has expired to indicate that power has been turned off 5 To exit programming mode press and hold in both the V and
8. acuation rate Note this parameter specifies the desired rate of evacuation Extremely high evacuation rates will not be maintained if the rate exceeds the capacity of the vacuum pump To minimize fluctuations around the setpoint a needle valve may be needed between the Digital Vacuum Regulator and the vacuum pump SPrn SetPoint Ramp Run Allowable Values ON OFF Hold This parameter turns the ramping feature ON or OFF During an active run if this parameter is set to Hold the setpoint ramp stops and holds at its current value This continues until the parameter is set to ON or OFF When set to OFF the values in SetPoint Ramp Rate and Soak Time are ignored SOAK Soak Time Allowable Values 0 to 1440 min This specifies the amount of time to soak at the setpoint after the setpoint vacuum ramp is complete A setting of causes the controller to remain at the final setpoint indefinitely A numeric value causes the controller to stay at the setpoint for the entered time and then turn power off to the vacuum valve The pressure in the vessel will increase depending on the number of leaks in the system Important Points to Know 1 While the Ramp to Setpoint feature in activated the display alternates between the current reaction pressure and the word SPr to indicate that a SetPoint Ramp is active 2 Once the Ramp to Setpoint feature is activated in programming mode it will remain active until it s de
9. em using a manometer The regulator must be evacuated to as close to 0 torr as possible before the adjustment in step 5 is performed 5 Adjust the Zero pot until the reading on the meter matches the actual pressure 6 Turn the vacuum pump off and unplug the OUTLET port Adjust the Span pot until the Trans meter reads the actual barometric pressure in the former lab 7 Turn the controller off and replace the cover Looking in from the top of the vacuum regulato
10. ion to minimize fluctuations Use a cold trap between the distillation set up and the vacuum regulator The pressure reading begins to lose linearity below 12 torr The pressure reading will be consistent but its absolute value may be off by as much as 2 torr 4 Good luck and give us a call if you need additional assistance NOTE J KEM does manufacture a precision computer controlled high accuracy vacuum controller our DVR 1000 Correcting Offset in the Displayed Pressure A small amount of error can develop in the displayed pressure 2 torr of the vacuum regulator This is due to the wide pressure range of the transducer used and accuracy better than this is usually not possible For display errors larger than 2mm the controller can be calibrated using the procedure below For users experienced with J KEM s meter do not correct pressure using the ZEro function This introduces an error not a correction Before beginning this procedure you will need to know the correct barometric pressure inside your lab This procedure should only be performed by a qualified electrician Remove the controller s cover 2 Plug the OUTLET port of the regulator and set the regulator selection switch to the FULL VACUUM position 3 Let the controller warm up for 10 minutes 4 Connect a vacuum pump to the INLET port turn it on and let it evacuate the controller to as close to 0 torr as possible Measure the pressure in the syst
11. l the equipment is evacuated at a reasonable rate When at the set point adjust the valve for stable pressure regulation Leave the needle valve in this position for future use Once the valve is set for a reasonable evacuation rate it doesn t require further adjustment Section 2 Regulator Description 7 Serial Comm Port on back J KEM Scientific Instruments for Science from Scientists Meter Off Pressure Display The default display is the pressure in the attached piece of equipment in units of mm of Hg torr The set point pressure can be seen any time by holding in the button Control Key Pressing and holding this button causes the regulator to display the set point pressure as a blinking number in the display The set point pressure is entered by holding in the control key and simultaneously pressing the A button to increase or the W button to decrease the displayed value 66399 Decreases V or increases A the set point pressure when the button is simultaneously held in Regulators Power Switch Indicates the position of the regulator selection switch 6 Regulator Selection Switch A three position switch that determines the pressure in the attached equipment see Section 3 6 The different switch positions have the following effects Meter Evacuates the attached equipment to the set point pressure entered in the controller Off Isolates the vacuum pump from the attached equipment
12. ne dry ice trap should be placed between the OUTLET of the digital vacuum regulator and the equipment being regulated This prolongs the life of both the regulator and the vacuum pump The dry ice trap available from J KEM catalog RCE1000 is highly recommended because of its high condensation efficiency large reservoir and ease of solvent removal 3 3 Ramp to Setpoint amp Soak Feature A new feature of J KEM s controllers called Ramp To Setpoint allows a specific rate for evacuation to be entered e g reduce the pressure to 20 torr at a rate of 10 torr Hour A second feature called Soak then lets you specify how long to stay at that pressure before turning off Example of Program Ramps Power Off Nn a ao z 5 Pressure Power Off NY Q ge oe 5 Pressure Time Time The controller is shipped with the Ramp to Setpoint feature OFF the user must specifically turn Ramp to Setpoint ON When Ramp to Setpoint is OFF the controller evacuates to the entered setpoint at the fastest rate possible 1 e the rate that results from fully opening the vacuum valve When Ramp to Setpoint is ON the controller evacuates at the user entered ramp rate The Ramp to Setpoint feature and its associated parameters are turned on and set in the controller s programming mode The parameters of importance are SPrr SetPoint Ramp Rate Allowable Values 0 to 9990 torr Hr This specifies the desired ev
13. nnect the instrument in which the vacuum is to be regulated 1 e rotary evaporator distillation setup etc to the tube marked Outlet There should be no restrictions 1 e valves stopcocks between the Outlet port and the equipment you re regulating Best results are obtained when large diameter tubing is used to make this connection Turn the Regulator On 8 J KEM Scientific we Meter T itr friemen frum Scars _ F FE a 1 Set the regulator selection switch to the of ia Off position Full 7 a Vacuum 2 Ifthe unitis fit with a needle valve turn a he valve until it s fully closed a the va M Ramp to Setpoint i d Digital Vacuum Regulator 3 Turn the regulator and vacuum pump on whe u Regulator Selection Switch Enter the Desired Pressure The default display of the meter is the pressure in the equipment it s attached to The desired pressure or set point is entered by holding in the button on the front of the meter and simultaneously pressing either the W button to decrease or the A button to increase the set point The set point which appears as a blinking number can be seen at any time by holding in the button Move the Regulator Selection Switch to the METER Position When set to the Meter position the regulator maintains the attached equipment at the set point pressure entered in step 3 For Controllers Equipped with Needle Valves open the valve unti
14. uum pump and when the equipment is at or below the set point the controller shuts the control valve isolating the vacuum pump from the equipment 3 2 Factors Affecting Vacuum Regulation Accuracy Operations Guide Outlet Inlet from equipment to pump Control Valve Pressure ransducer a The rate of evacuation An important factor affecting stability is the rate the vacuum pump evacuates the attached equipment In some cases the rate of evacuation must be manually limited by using a needle valve A needle valve is used because many vacuum pumps have such high pumping capacities that they evacuate equipment faster than the controller can respond to changes in pressure the controller needs 1 10 of a second to respond to pressure changes Particularly in small 800 equipment pressure can be lower more Pressure Regulation in a Rotary Evaporator 700 Without valve than desired in 1 10 of a second without a needle valve limiting the ge 000 evacuation rate Regulating the With valve evacuation rate becomes more oe important the smaller the piece of A 400 equipment being evacuated since it s evacuated faster for example consider am a 50 ml flask compared to a rotary evaporator The diagram at the right shows the result of using a needle valve 100 to limit evacuation rate Sy aata Oa a SOS NYY 5 20 30 40 Time Sec 0 60 Use a cold trap to condense volatile solvents At least o
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