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15 

 

Load, Save, and Create a New Method 

 

The “Load, Save, and Create a New Method” screen allows all users to create new methods, save them to the Discover 
data base and Load (recall) the methods at a later time. From this screen, the user can also recall data from a reaction 
previously run on the Discover system. To access this screen press the Discover key on the Discover keypad. 
 

 

 
Create a New Method 
 

The Discover System has three (3) control options for programming a method – Standard, Dynamic and Ramp-to-
Temperature. These options permit the user to control how the system applies the microwave energy to the reaction. 
In all control options, the user inputs control parameters to create the method. The user enters more control information 
as the level of control increases. The Standard control option is the recommended control technique for routine operation. 
 
The Dynamic method allows the user to implement the ActiVent feature. The SP-D Clinical system permits the user to 
release unwanted gaseous byproducts from the reaction to prevent over pressurization and vial failure from gaseous 
buildup. This ensures safe handling of the vial during and at the end of the reaction. The ActiVent safely bleeds the 
solvent/vapor from the reaction vessel and releases it through the vent tube connected to the back of the system and into 
a controlled environment. 
 
If the reaction generates a gaseous byproduct or an extreme amount of pressure during the reaction, the ActiVent will 
vent at a specific set point for a pre-determined number of times. 

  The “Delta Pressure” is the assigned amount of pressure to drop from the pressure set point. A delta of 50 PSI 

(1.7 BAR) is recommended. 

  The “PressureSP” is the pressure set point at which the venting will begin. If the gaseous byproduct that is 

generated is the only pressure in the reaction vial (the reaction temperature does NOT exceed the boiling point of 
the solvent), the ActiVent pressure release can be set below the control point. If a gas is generated, but some of 
the pressure is due to vapor pressure, then the release point for the ActiVent must be set at or above the 
pressure control point. 

  The “Times at SP” is the maximum number of times a reaction will vent during the assigned ramp and hold time. 

However, this parameter can be adjusted based on specific reaction conditions. For a typical reaction, 5 vents 
are recommended. 

 

CAUTION 

 

If the reaction temperature exceeds the acid boiling point and too many venting actions are performed, the vial 
could become dry and superheat. 

 

  The number of stages is the stage at which the PressureSP will be active for a multistage method. A maximum of 

5 stages can be added. 

 

 
 
 
 
 
 
 
 
 

Содержание Discover SP-D

Страница 1: ...i Operation Manual 600857 Rev 1 8 17 ...

Страница 2: ... to others without prior written permission of CEM Corporation CEM is a registered trademark of CEM Corporation Discover is a registered trademark of CEM Corporation Patents Pending CEM Corporation POB 200 3100 Smith Farm Road Matthews North Carolina 28106 0200 704 821 7015 phone 704 821 7894 fax www cem com website Manufactured in the United States of America 600857 Rev 1 8 17 ...

Страница 3: ...l Extraction 13 Items Required 13 Prepare the Vessel 13 Perform a Method 13 Vessel Removal 14 Load Save and Create a New Method 15 Create a New Method 15 Standard Control 16 Dynamic Control 16 Save Method 20 Ramp to Temperature Control 21 Load Method 22 Data Review 22 Delete Method 23 Discover Home 24 Rxn Programming 24 Logout 25 ActiVent Home ActiVent Moving ActiVent Closed APM Recovery 25 System...

Страница 4: ...heral Setup 35 Information 35 Administrative Functions 35 Create New User 35 Create User 35 User Name 36 Permissions 36 User Profile 36 Save User 37 Edit User 37 Permissions 37 User Profile 37 Save User 37 Delete User 38 Administration 38 Maintenance 39 Interlocks 39 Cavity 39 ActiVent 40 APM Cleaning 42 Clean ActiVent using Water 43 Stirring Verification 45 Firmware Update 45 Service 47 Microwave...

Страница 5: ...an electromagnetic sample stirrer which contains very high static magnetic fields some danger exists if a pacemaker is positioned in close proximity of the instrument cavity If the instrument is suspected of interfering with the operation of a pacemaker the instrument should be turned off or the pacemaker wearer should move away from the instrument This instrument utilizes high voltages and microw...

Страница 6: ...djusting single mode microwave cavity that is manually accessed via multiple attenuator ports A 256 x 128 graphics display and on board computer for programming and operational control of the system The memory will store and recall methods 3 safety interlocks and an interlock monitoring system to prevent microwave emission when the attenuator port is not properly installed One 1 serial port 1 RS 2...

Страница 7: ... of using an offboard PC to program the system and to collect data Display displays menus method parameters and instrument status on a 256 x 128 graphics display Keypad allows the operator to create edit store and recall methods start and stop methods and change programmed parameters during operation Attenuator provides access to the instrument cavity while preventing microwave leakage during oper...

Страница 8: ... a method Use the keys to toggle to the appropriate setting High Medium Low Off If this key is pressed during a method this does not stop or pause the method but permits changing the setting in real time The updated setting is not captured as part of the saved method file in the method library COOLING Press this prior to beginning a method or during a method to perform the cooling function If this...

Страница 9: ... contents in case of a vessel failure Ethernet Port Allows communication and connection to an external computer for data collection a local area network LAN or the Internet Optional Nameplate Lists the model serial number Product Tag operating voltage frequency and current of the instrument Side Views Power Switch Turns AC power on and off to the instrument Cooling Gas Line Provides a hose connect...

Страница 10: ...rument is suspected of interfering with the operation of a pacemaker the instrument should be turned off or the pacemaker wearer should move away from the instrument Cooling The cooling feature directs a gas source onto the outside wall of the reaction vessel This provides the ability to rapidly cool quench a reaction after the application of microwave energy The cooling feature is either on or of...

Страница 11: ...t for shipping damage such as cracks dents or warping WARNING Upon receipt if damage to the instrument is noted do not attempt to operate the instrument This instrument utilizes high voltages and microwave radiation Only technicians trained in repair and maintenance of high voltage and microwave power systems should perform instrument service and repair Never modify the attenuator access port or i...

Страница 12: ...the ActiVent 4 Place the other end in the back of the fume hood or other location appropriate for solvent exposure 5 Plug the power cord into the wall outlet 6 To set up the air regulator a Splice the tubing supplied by CEM in half b Install one length of the tubing into the left side of the Discover by pushing in on the tubing until resistance is felt c Place the opposite end of the tubing into t...

Страница 13: ...itch located on the left side of the Discover turn the instrument on 9 The ActiVent pressure device will return to the home position once the Login screen appears Remove the 10mL shipping device Note Do not discard the 10mL shipping device It will be required if returning the system to CEM Corporation for service Computer Installation optional 1 Connect one end of the Ethernet cable to one of the ...

Страница 14: ...al tab highlight the Internet Protocol TCP IP connection and select Properties This will open the Internet Protocol TCP IP Properties 168 1 window d Select Use the following IP Address e Assign 192 168 1 10 to the IP Address f Press the tab button Tthe subnet mask box should populate with 255 255 255 0 NOTE The IP address consists of up to 12 numeric characters The address is broken into 4 sets of...

Страница 15: ...t the appropriate user 2 Press ENTER 3 If the user is prompted to provide a password a Use the ARROW and keys to highlight the first letter or number of the password NOTE The Shift key changes the letters and or symbols to lowercase b Press ENTER to accept the first letter c Continue highlighting the letters or numbers of the password and pressing the ENTER key for each letter number until the pas...

Страница 16: ...ere Try performing the reaction at higher concentrations How to Cautiously Microwave Start with a low power input 200 W or less this can be adjusted as necessary Watch the first minute of the reaction If a gas forms during the reaction Cool the reaction completely Allow the ActiVent to release the excess gas Standard Vessel Total Volume Vessel Name Working Volume Sealed Pressurized or Open Atmosph...

Страница 17: ...nuator assembly with the large slot positioned toward the back of the instrument 6 Rotate the attenuator assembly clockwise until the attenuator locks into position 7 Place the vessel into the attenuator Perform a Method 1 Load or create the appropriate method into the instrument on the Discover SP D Clinical or the Synergy software see section Load Method or Create New Method or the Synergy softw...

Страница 18: ...tate the attenuator assembly counterclockwise and lift it from the instrument WARNING To prevent the possibility of severe burns wear insulated gloves and protective gear as outlined in the user s safety program 3 Carefully remove the vessel from the attenuator NOTE If the cap still holds residual pressure place the cap and vial in a fume hood or other well ventilated area Use a needle to pierce t...

Страница 19: ...he reaction vessel and releases it through the vent tube connected to the back of the system and into a controlled environment If the reaction generates a gaseous byproduct or an extreme amount of pressure during the reaction the ActiVent will vent at a specific set point for a pre determined number of times The Delta Pressure is the assigned amount of pressure to drop from the pressure set point ...

Страница 20: ...t modulates this set power automatically based on the sensor feedback data to ensure the control point is reached rapidly but with limited error temperature or pressure overshooting The user programs the maximum amount of microwave power that can be applied to the method a temperature control point a pressure control point a hold time the time the system maintains the control parameters a stirring...

Страница 21: ...ltiple irradiation steps and is a general control method for maintaining critical control points 1 With the main menu displayed press the DISCOVER key 2 Using the ARROWS and keys highlight Dynamic 3 Press the ENTER key 4 Press one of the hotkeys to modify any of the default parameters 5 Use the ARROW keys to navigate between temperature time power pressure stirring PreMix PowerMAX and number of St...

Страница 22: ... gas is generated but some of the pressure is due to vapor pressure then the release point for the ActiVent must be set at or above the pressure control point The Times at SP is the maximum number of times a reaction will vent during the assigned ramp and hold time However this parameter can be adjusted based on specific reaction conditions For a typical reaction 5 vents are recommended The number...

Страница 23: ... T or P 5 Enter the desired method parameters using the arrow keys to navigate between power time temperature pressure stirring and PreMix Use the keys to increase and decrease the numeric value Ramp Time 1 second to 99 hours 59 minutes and 59 seconds Hold Time 1 second to 99 hours 59 minutes and 59 seconds Power μλ 0 300W Temperature To 15 260 ºC ...

Страница 24: ...hat vent point This parameter should be adjusted based on specific reaction conditions The number of stages is the stage at which the PressureSP will be active for a multistage method A maximum of 5 stages can be added 8 Once all parameters have been entered press the ENTER key to return to the method parameters screen 9 Press the ENTER key again to accept all method parameters Save a Method Savin...

Страница 25: ... The Load Method option gives the user the ability to recall a method previously saved under their user profile or that of another user saved on the same Discover SP D Clinical System Methods can also be transferred from one system to another using the USB flash drive supplied with the Discover SP 1 With the main menu displayed press the DISCOVER key 19 2 Using the ARROWS and keys highlight Load 3...

Страница 26: ... Data Review If the USB drive is in position on the side of the Discover during the reaction the temperature data for each run will automatically be stored This data can be viewed on the Discover screen later as a graph or viewed as individual data points on a computer NOTE Only USB flash drives supplied by CEM Corporation are compatible with the Discover SP D Clinical system 1 Install the USB fla...

Страница 27: ...older 3 Select the appropriate user s folder 4 Select the data folder 5 Select the appropriate data file and open as a CSV or excel document Delete Method The Delete Method function allows the user to delete methods that have been stored within the Discover SP D Clinical database 1 With the main menu displayed press the DISCOVER key 2 Using the ARROWS and keys highlight Load 3 Press the ENTER key ...

Страница 28: ...e users when shipped Administrator includes all administrator privileges and is password protected USER includes all administrator privileges and does not include a password Guest includes Guest privileges If the Discover is not being installed by a CEM representative contact CEM to obtain a password that will permit administrative rights The Discover Home screen will appear differently for users ...

Страница 29: ... user types guest standard and administrator ActiVent Home is displayed when the attenuator is exposed and the APM is near the back of the instrument When ActiVent Home is highlighted and the ENTER key is pressed the ActiVent will move to the closed position If a vessel is not in place when the ENTER key is pressed the Discover SP D Clinical will display a Vessel Not Found message ActiVent Moving ...

Страница 30: ...will raise the ActiVent to the highest position c Use the ARROW and keys to highlight APM Back d Press the ENTER key If the APM appears to be moving backward select APM Back until the ActiVent no longer moves backward The ActiVent should be all the way back away from the attenuator e Use the ARROW and keys to highlight the HOME button f Press the ENTER key The APM should now return to the HOME pos...

Страница 31: ...ption must be connected on the side of the instrument The part number for the fiber optic assembly is 541166 4 Press the ENTER key The User Setup screen will appear again Release limits Temperature and pressure release limits are the temperature and pressure at which the ActiVent will automatically open and release the vessel after cooling The recommended default temperature is 60 C The recommende...

Страница 32: ...rs and or symbols to lowercase 3 Press the ENTER key to accept the first letter 4 Continue highlighting the letters or numbers of the password and press the ENTER key for each letter number until the password has been entered 5 Once the password is entered use the ARROW and keys to highlight OK User Profile Defaults 1 User Profile Default is the 2nd page of the User Profile menu The User Profile D...

Страница 33: ...4 Press the ENTER key to accept the default temperature Power Microwave power is the user defined maximum power used during a method The default microwave power is 150 watts When creating a new method the microwave power can be changed from the default power programmed in the User Profiles 1 Use the keys to highlight Temperature 2 Press the ENTER key 3 Use the keys to increase and decrease the mic...

Страница 34: ...Units Pressure Units is the user defined unit in which the pressure is displayed The instrument default pressure unit is PSI 1 Use the keys to highlight Pressure Units 2 Press the ENTER key 3 Use the keys to change the units between PSI and Bar 4 Press the ENTER key to accept the default pressure unit User Profile Defaults 3 From the 2nd User Profile Default screen press the right arrow key one ti...

Страница 35: ...nstalled in one of the USB ports the software will prompt the user to install a USB flash drive If desired press the Home key to exit the screen CAUTION Do not remove the USB flash drive from the USB port during method backup or restoration Removal of the USB flash drive prior to completion of method backup or restoration will corrupt the data on the USB flash drive and or the system files Wait 15...

Страница 36: ...n Setup screen 1 From the Temperature Calibration screen use the keys to select Infrared 2 Press the ENTER key to enter the IR Calibration screen Slope Slope is used to enter a known slope for the Infrared temperature control 1 Use the keys to highlight Slope 2 Press the ENTER key 3 Use the keys to highlight Clr to delete the current value 4 Use the ARROW and keys to highlight and select the prope...

Страница 37: ...hen pull the cable away from the box 2 Install the white communications cable 277275 to RJ 12 adapter 277225 by pushing in until a click is audible 3 Install the adapter to the fiber optic box and tighten the screws finger tight Refer to the Fiber Optic Instructions for further information c Insert the temperature sensor into the temperature control module The sensor is attached to the module with...

Страница 38: ... Setup from the Discover Home screen This page allows the user to view or enter an IP Address Sub Net Mask or Serial Number The IP Address Sub Net Mask and Serial Number should not be modified except by a technician experienced in Network Setup IP Address The IP Address setting allows the user to set an IP address on the Discover SP D Clinical system to allow connection to the Synergy Software The...

Страница 39: ...erial number should not be altered Information The Information page is the 5th page that appears after selecting System Setup from the Discover Home screen This page allows the user to view the following information Firmware PS Firmware Power Supply ID PC Board Magnetron Time Temperature Temperature Control Pressure Vessel Administrative Functions The Administrative Functions screen consists of tw...

Страница 40: ...TER key 3 Use the keys to highlight User Name 4 Press the ENTER key A new screen will appear 5 Use the ARROW and keys to highlight the first letter or number of the desired user name NOTE The Shift key changes the letters and or symbols to lowercase 6 Press the ENTER key to accept the first letter 7 Continue highlighting the letters or numbers of the name and pressing the ENTER key for each letter...

Страница 41: ... and edit system parameters There are four 4 pages within the User Profiles page Refer to the section titled User Setup for guidance Save User The Save User option saves the user that was created in the previous steps to the Discover SP D Clinical database 1 From the Create New User screen Use the keys to highlight Save User 2 Press the ENTER key 3 Press the ENTER key to save the user NOTE The use...

Страница 42: ...light the user to be deleted 4 Press the ENTER key 5 The user will be given the option to Delete Selected User 6 Use the ARROW keys to toggle between Yes and No 7 Press the ENTER key 8 Press the HOME key to return to the Discover Home screen Administration The Administration page is the 2nd page that appears after selecting Administrative Functions from the Discover Home screen This page allows th...

Страница 43: ...ity The cavity should be cleaned inspected if any of the following occurs vessel Failure material spilled in cavity or the cavity has not been inspected in a week or more The spill cup protects the temperature sensor from debris in case of a vessel failure 1 Turn the instrument off 2 If applicable remove the attenuator by rotating it counterclockwise to expose the cavity 3 Inspect the cavity If it...

Страница 44: ...tion it will reflect an image similar to a mirror If the IR lens appears to be damaged ie scratched contact CEM Service at 800 726 5551 or 704 821 7015 or email service cem com 9 If the spill cup is not damaged install it once it has dried NOTE Replacement of the spill cup will require calibration of the IR as outlined in this manual 10 Replace the attenuator and continue operation ActiVent The Ac...

Страница 45: ...R key A new screen will appear 8 Remove the attenuator from the cavity 9 Press the ENTER key A new screen will appear Clean APM Moves the APM forward and lowers the pressure head APM Home Raises the pressure head and homes the APM 10 Use the keys to highlight Clean APM 11 Press the ENTER key The pressure device will move forward ...

Страница 46: ...e Pressure Head is not fully extended do not select OK 15 Once the pressure device is lowered and an audible noise can no longer be heard remove the back cover of the APM 16 Hold the front cover of the ActiVent and lift it upward The underside of the pressure device will be exposed 17 Use a damp cloth to clean the pressure device inside and out including the o rings ...

Страница 47: ... 00 Pressure 400 PSI Power 150W general starting point Stirring High Pressure SP 150 PSI Times at SP 10 Delta Pressure 50 PSI 5 Perform the venting method allowing the water to be vented through the pressure device and clean the pressure head 6 Once complete stop the reaction and remove the vial once it is completely cooled Note If the temperature decreases suddenly stop the reaction and repeat wi...

Страница 48: ...utlined in the user s safety program for hazardous materials and the reagent manufacturer s material safety data sheet Refer to these guidelines for proper handling and disposal of reagents 8 Press the ENTER key 9 Press the right ARROW key for 4 times to display the Maintenance 5 screen 10 Press the keys to highlight Test Stirring 11 Press the ENTER key The stirring speed will be displayed at the ...

Страница 49: ...s website www cem com Note Bootloader files will follow the CEMLoader_X X format and firmware files will follow the Evolution_DSXAXX XX format 5 Turn the instrument off 6 If applicable remove the small side cover from the right side of the instrument 7 Place the USB flash drive into one of the USB ports on the right side of the instrument 8 Turn the instrument on A screen will appear with the file...

Страница 50: ...that the file is being loaded CAUTION Do not remove the USB flash drive from the USB port during the firmware update Removal of the USB prior to completion of firmware update will corrupt the data on the USB 14 Upon completion the Log In Screen will appear Wait at least 30 seconds and remove the USB flash drive ...

Страница 51: ...r such as the Holaday Model HI 1500 available from CEM Corporation P N 300500 Slowly move the RF probe around the attenuator perimeter and around the fan grills to check for microwave leakage Note CEM does not recommend use of meters available in electronics stores because they are prone to give erroneous readings and lack the necessary sensitivity to properly test an instrument for microwave leak...

Страница 52: ...nce all the letters have been entered highlight OK 16 Press the ENTER key to save the method 17 If applicable remove the attenuator assembly from the instrument cavity 18 Insert the vessel stand in the instrument cavity with the standoffs pointing downward Ensure that the vessel stand is flat against the bottom of the cavity and that the cutout in the stand is positioned over the opening in the ca...

Страница 53: ...wer Output Note The Discover system is designed to apply 300 watts If the current wattage is greater than or less than ten Percent the system is within its operating limits If the system is not within ten percent calibrate the instrument Note If the current wattage is not within ten percent contact CEM Service at 800 726 5551 or 704 821 7015 or email service cem com Auto Power Test Items required ...

Страница 54: ...RROW key three times or until Maintenance 4 appears Note The system requires the fiber optic option to perform an auto power test Refer to the Fiber Optic section to enter the calibration and select the Fiber Optic option 8 Press the keys to highlight Auto Cal PS 9 Press the ENTER key 10 Use the ARROW keys to highlight Power Test 11 Press the ENTER key 12 If applicable remove the attenuator assemb...

Страница 55: ...e vessel 19 Press the START PAUSE key Note If the following screen appears ensure that the Fiber Optic option is assembled correctly Also ensure that Fiber Optic is selected and calibration has been entered 20 Once the START PAUSE key is pressed the following message will appear in the bottom line of the instrument Screen Record start temperature in 10 seconds Once the countdown is complete the bo...

Страница 56: ... If the spill cup contains glass particles or shards ensure that the glass is placed into a proper waste container 6 Rinse the spill cup Once all debris is rinsed from the spill cup check for cracks and or damage Wipe the spill cup with an alcohol wipe or equivalent Note If the spill cup is damaged replace the spill cup 7 Check the cavity walls for debris Remove any debris and wipe down the walls ...

Страница 57: ... Remove the screw securing the spill tray to the back of the instrument cover c Carefully slide the spill tray out of the instrument d Properly dispose of the contents of the tray e Rinse the tray with an appropriate solvent and allow it to dry f Install the spill tray and secure it to the instrument with the thumb screw 11 Allow the cavity liner and spill cup to dry 12 If the spill cup is not dam...

Страница 58: ...ice section of this manual Inoperative vessel stirring Sample viscosity See section titled Stirring Verification within the Maintenance Section Weak stir bar See section titled Stirring Verification within the Maintenance section Erratic Temperature Lens dirty or blocked See section titled Vessel Failure Cleanup Procedure Infrared needs to be calibrated See section titled Temperature within the Sy...

Страница 59: ...erform all functions with or without connection to external PC RS 232 9 Pin IBM PC compatible Internal Diagnostic Software BITS System Built In Test System Checks monitors line voltage magnetron life temperature control status operation safety interlocks Pressure Control System Inboard pressure control system to monitor and control System equilibrium reaction pressure Pressure sensed 200 times per...

Страница 60: ...n fuses Replace consumables and Clean the instrument as required How to Get Service Purchaser should contact the Service Department of CEM Corporation or his distributor for return authorization and for proper crating and shipping instructions to return instrument freight prepaid for service On site repairs by an authorized service technician are available through the CEM Service Department Travel...

Страница 61: ...2842 96440 phone 49 2842 964411 fax info cem de email Ireland Subsidiary CEM Technology Ireland Ltd Sky Business Centre 9a Plato Business Park Demastown Dublin 15 Ireland 353 0 1 885 1752 phone Info ireland cem com email Italy Subsidiary CEM S r l Via Dell Artigianato 6 8 24055 COLOGNO AL SERIO bg Italy 390 35 896224 phone 390 35 891661 fax info srl cem com email Japan Subsidiary CEM Japan K K 2 1...

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