Corporation Issued: 5/09 P/N: 600104 Rev. 2 Instructions for Assembly, Installation, and Operation of the Gas Addition Kit Accessory with the CEM Discover Systems The Gas Addition Accessory permits the addition of a gaseous reagent into the 10 ml microwave reaction vessel. The vessel has a working volume of 2 ml to 7 ml. Note: This accessory includes a fiber optic probe; therefore, the minimum volume is the amount required to cover the fiber optic probe. The maximum operating conditions are 200 C and 200 psi (14 bar). Note: Assembly instructions vary for the Discover and Discover S-Class instruments. Refer to instructions for the appropriate instrument as outlined in these instructions. Contents Recommended Gas Addition Accessory Operating Parameters... 2 Discover S-Class Installation of Gas Addition Accessory... 3 Reaction Setup... 7 Discover Legacy Systems (BenchMate or LabMate)... 10 Installation of Gas Addition Accessory... 10 Reaction Setup... 15 Maintenance Guide Cleaning Kit... 18 O-ring Replacement... 21 1
WARNING Refer to the user s safety practices for safe handling and operation of compressed gas cylinders. WARNING This system is NOT designed for use with corrosive gases such as ammonia, hydrogen chloride, chlorine, and methylamine. Recommended Gas Addition Kit Operating Parameters Volume: Do not fill the vessel with more than 7 ml nor less than 2 ml. Solid Reagents: If using a heterogeneous reaction mixture, prior to beginning the reaction, ensure that all solids have been washed from the surface of the glass. Rinse all solids from the walls of the reaction vessel Ready for Microwave Gas Pressure: Using the ideal gas law (PV = nrt), calculate the minimum amount of gas needed for the reaction. Typically, this is a good starting point. If a higher gas pressure is required, keep in mind the maximum allowed pressure is 200 psi. Warning The microwave CANNOT be operated with the reaction vessel open to the gas source. Note: If more than 200 psi of gas is required for the chemistry, additional gas can be added after the consumption of the initial 200 psi of gas (refer to the Operating Instructions for further information). Temperature: The maximum suggested operating temperature is the boiling point of the solvent. As the temperature of the reaction mixture increases above the boiling point, the gas may be driven out of the solution, resulting in a decrease in yield. For example, see Vanier, G. S. Synlett 2007, 131-135. The maximum operating temperature is 200 C. 2
Discover S-Class Installation of Gas Addition Accessory Note: Only users with Administrative Privileges may operate the gas addition accessory on the Discover S-Class System. 1. Remove the cover from the right side of the Discover to expose tow (2) USB ports, 1 8-pin port, and 1 RJ-11 port (Figure 1). USB Ports 8-pin connector RJ-11 Port Figure 1 2. Verify the firmware version installed in the Discover S-Class instrument. a. Log into the Discover using the USER login. b. Press the Home key once to return to the Discover Home Screen. c. Using the down arrow key, select System Setup. Press ENTER. d. Using the right arrow key toggle over to the 4 th menu screen Information. e. The firmware version will be displayed at the top of the screen. If the firmware version displayed is 2.05 or greater, skip to step 4. If the firmware version is 2.04 or lower, follow the instructions in step 3. 3. To update the firmware in the Discover, the firmware must be loaded onto the USB stick that is supplied in the Discover accessory kit. a. Install the CEM jump drive into the USB port of a computer and create a folder named cem on the jump drive. CAUTION Only the CEM jump drive supplied with the Discover S-Class instrument can be read by the USB slot. b. Copy the supplied firmware file(s) into the cem folder on the jump drive. Note: bootloader files will follow the CEMLoader_X.X format and firmware files will follow the Evolution_DSCAXX.XX format). c. Place the USB jump drive into one of the USB ports on the side of the Discover and turn the Discover off and back on. The instrument software will begin to boot. d. A screen will appear with the file names listed. Using the arrow key, select (highlight) CEMLoader_1.12.bin (or latest version). Press the ENTER to load the bootloader. e. The file will automatically be installed in the instrument, and the progress will be noted with a progress bar at the bottom of the screen. Once the installation is complete, a screen will appear listing the installed files. f. Select Evolution_DSCA02.05 (or latest version of firmware) and press ENTER to load the firmware on the Discover S-Class. The progress bars will appear to indicate that the file is being loaded. Once the installation is complete, the Discover Home Screen will appear. Wait 30 seconds, and then remove the USB jump drive and continue as normal. CAUTION Wait at least 30 seconds prior to removing the jump drive. Removal of the jump drive prior to completion of the firmware update will corrupt the data on the jump drive as well as the system firmware. 3
4. Install the 8-pin adaptor from the back of the gas addition accessory into the 8-pin connector on the side of the instrument (Figure 2). Note: If necessary, remove the cover from the right side of the Discover S-Class to access the 8-pin connector. Figure 2 5. Install the vent line tubing: a. Locate the spare tubing located in the accessory kit (bag). b. Locate the front and back ferrules from the accessory kit. c. Install the nut and ferrules on the tubing as outlined below (Figure 3). Figure 3 d. Install the tubing into the Vent port located on the back of the Gas Addition Kit. 6. Place the vent tubing from the back of the gas addition accessory into a beaker in back of a fume hood (Figure 4). Vent line Vacuum Line Figure 4 7. If desired, connect the vacuum line to a vacuum source (Figure 4). Do not exceed 25 in Hg. 4
8. Ensure that the pressure line from the 10 ml gas addition vessel top is attached to the gas addition accessory (Figures 5 and 6). WARNING Prior to each use of the gas addition accessory, ensure that the fittings on the vessel top are properly tightened. Failure to tighten these fittings may allow the vessel to leak. Over tightening may disturb the flow of gas within the pressure line. Vessel Gas Source Figure 5 Figure 6 9. Connect the desired gas source to the port on top of the gas addition accessory (Figure 6). 10. If applicable, remove the the standard 10 ml vial attenuator from the instrument by rotating it counterclockwise and lifting the attenuator. 11. Install the attenuator supplied with the gas addition accessory into the instrument cavity. Position the attenuator so that the slots fit into the cutouts of the cavity. Once the attenuator is properly seated, rotate the attenuator clockwise until it locks into position (Figure 7). Figure 7 12. Position the toggle switch of the gas addition accessory to Gas (Figure 8). Figure 8 5
13. Enter the calibration for the gas addition accessory. a. Login with the USER login name or other login name with Administrative Privileges. b. From the Discover Home screen, press the down arrow to highlight System Setup. Press ENTER. c. Press the right arrow key once to access the Calibration Screen. d. Press the down arrow key to highlight Pressure Gas Addition. Press ENTER. Note: The gas addition attenuator must be locked into position, the toggle switch positioned to Gas, and the cable connected from the gas addition accessory to the Discover. e. Press the down arrow key to highlight Slope. Press ENTER. f. Select the Clr button the display to clear the existing value. g. The slope is recorded on the calibration data sheets or on the plug extending from the gas addition accessory to the Discover. Using the arrow keys, select the appropriate values on the instrument keypad. Highlight OK and press ENTER. h. Press the Home key to return to the Discover Home screen. 14. Connect the white communication cable with the RJ-adapter to the gas addition accessory (Figure 9). Figure 9 15. Connect the communication cable into the RJ-11 port on the side of the Discover (Figure 10). Figure 10 16. Insert the temperature sensor into the top of the gas addition accessory. The sensor is attached to the module with a locking collar on the sensor. Push the collar in, twist it clockwise, and then release it to lock the sensor module (Figure 11). Figure 11 6
17. Enter the temperature constant (GF number) for the fiber optic probe as follows. The GF number is recorded on the label attached to the fiber optic probe as well as the label on the case in which the probe is shipped. a. From the Discover Home screen, press the down arrow until System Setup is selected. Press ENTER. Note: If System Setup is not an option, logout and log back in using login name USER or other login name with Administrative Privileges. b. Once in System Setup, press the right arrow key once to access the Calibration Screen. c. The Temperature option should be selected. Press ENTER. d. Press the down arrow to highlight Fiber Optic Probe. Press ENTER. e. If a value exists, highlight the Clr button to delete the value. f. Using the arrow keys, select the appropriate GF number. g. Highlight OK. Press ENTER. h. Press the Home key to return to the Home screen. 18. Select Fiber Optic as the temperature option. a. From the Discover Home screen, select System Setup and press ENTER. b. Select Temperature Type and press ENTER. c. Using the up/down arrow, highlight Fiber Optic. Press ENTER. d. Press the Home key and return to the Home screen. 19. Prior to performing a reaction, place the fiber optic probe into the thermowell, as shown in Figure 12, and verify that Fiber Optic is selected as the temperature option in the System Setup screen. Figure 12 Reaction Setup 1. Place the reaction components into a 10 ml vessel using the appropriate safety precautions based on the components used. CAUTION A stir bar is required. Ensure adequate stirring prior to performing a reaction. 2. Gently place the vessel into the attenuator (Figure 13). Figure 13 7
3. Install the assembled locking cover on the attenuator assembly. Rotate the cover clockwise until it is tightened. CAUTION Over tightening the locking cover can cause vessel failure. WARNING Prior to each use of the gas addition accessory, ensure that the fittings on the vessel top are properly tightened. Failure to tighten these fittings may allow the vessel to leak. Over tightening may disturb the flow of gas within the pressure line. 4. Set the regulator on the gas tank to the desired pressure. Note: The maximum pressure allowed is 200 psi. 5. If installed, turn on the vacuum source. Position the valve to the Vacuum position (Figure 14). Figure 14 6. Rotate the valve to the Fill position to add gas to the reaction vessel (Figure 15). Toggle between Fill and Vacuum at least three times to purge the reaction. Note: Slowly turn the valve from Fill to Vacuum to prevent the reaction mixture from escaping into the pressure line. Figure 15 7. After the final purge, position the valve to Fill to fully charge the vessel, and then position the valve to the Run position (Figure 16). Figure 16 8
WARNING The microwave CANNOT be operated with the reaction vessel open to the gas source. Note: The pressure in the reaction vessel can be observed on both the valve panel (located on the Gas Addition Accessory) and the Discover run screen (located on the Discover S-Class instrument). 8. Refer to the Discover S-Class Operation Manual and enter a method. Press the Start key. A screen confirming the security of the gas addition accessory will appear. 9. Verify that the vessel is securely locked into the attenuator, the valve is positioned to Run, and the fiber optic probe is in place. Using the arrow keys, toggle to select Yes to continue. 10. Press ENTER. The method will begin. WARNING Do not attempt to remove and open a vessel prior to venting the pressure inside the vessel. To prevent injury, prior to venting a gas addition vessel, ensure that the vent tubing is positioned in a fume hood and that the end of the tubing is not pointing toward the operator or instrument. Note: If more than 200 psi of gas is required for the chemistry, additional gas can be added after the consumption of the initial 200 psi of gas. Position the valve to Fill to recharge the vessel. This will pause the instrument. Rotate the valve back to Run and press Start to continue the reaction. 11. Once the reaction is complete, the cooling process will begin. Once the cooling is complete and the system is idle, the valve can be positioned to Vent. (Figure 17). Figure 17 12. Once the pressure is vented, remove the locking cover assembly. Remove the vessel and work up the reaction using standard procedures. 9
Discover Legacy Systems (BenchMate or LabMate): Installation of Gas Addition Accessory 1. Turn off the instrument. 2. Turn the instrument on and observe the instrument screen for display of the Clock Frequency, Firmware Version, and CPU Version. Record the firmware version. If the firmware version displayed is 201A11 or greater, proceed to step 4. If the firmware version is 201A11 or lower, follow the instructions outlined in step 3. 3. Replace the firmware: a. From the instrument main menu, press EDIT to access the System Setup screen. b. Press ENTER to access the Calibrate Temperature screen. c. Press ENTER to display the temperature calibration slope value. Record the slope value for re-entry. d. Turn the instrument off and disconnect the power cord from the electrical source. e. Remove the top cover lid by pressing lightly on the secure tab at the rear center of the lid while slightly lifting and pulling backward on the lid to disengage the front tabs (Figure 1). Figure 1 Figure 2 f. Remove the five (5) screws securing the top cover assembly (Figure 2). g. If a pressure sensor is currently installed in the back of the instrument, unplug it. h. If a cable is connected to RS 232, remove it. i. Lift the top cover from the instrument by lifting the front upward, leaving the electrical wiring connected. j. Remove the E-PROM from the CPU board. Note the notch in the end of the E-PROM for proper positioning of the new E-PROM. k. Install the new E-PROM on the CPU board, ensuring that the pins are positioned to prevent bending or breaking any pins during installation on the connector. Ensure that the notch of the E-PROM is positioned in the proper position (same as removed E-PROM). l. Secure the top cover assembly with the five (5) screws. Install the top cover lid. 4. Install the 8-pin adaptor from the back of the gas addition accessory into the back of the instrument (Figure 3). Figure 3 10
5. If an additional pressure module is used (such as an Explorer 24 or IntelliVent pressure device), it can utilized by placing the pressure line into the auxiliary port (Figure 4) in the gas addition accessory and using the toggle switch (moved to Standard ) to select the additional pressure device. Vent Vacuum Figure 4 6. Install the vent line tubing: a. Locate the spare tubing in the accessory kit (bag). b. Locate the front and back ferrules in the accessory kit. c. Install the nut and ferrules on the tubing as outlined below (Figure 5). Figure 5 d. Install the tubing into the Vent port located on the back of the Gas Addition Accessory. 7. Place the vent tubing from the back of the gas addition accessory into a beaker in the back of a fume hood (Figure 4). 8. If desired, connect the vacuum line to a vacuum source (Figure 4). Do not exceed 25 in Hg. 9. Ensure that the pressure line from the 10 ml gas addition vessel top is attached to the gas addition accessory (Figures 6 and 7). WARNING Prior to each use of the gas addition accessory, ensure that the fittings on the vessel top are properly tightened. Failure to tighten these fittings may allow the vessel to leak. Over tightening may disturb the flow of gas within the pressure line. Gas Figure 6 Figure 7 11
10. Connect the desired gas source to the port on top of the gas addition accessory (Figure 7). 11. If applicable, remove the standard 10 ml vial attenuator port from the instrument by rotating it counterclockwise and lifting it upward. 12. Install the attenuator for the gas addition accessory into the instrument. Position the attenuator so that the slots fit into the cutouts of the cavity. Once the attenuator is properly seated, rotate it clockwise until it locks into position (Figure 8). Figure 8 13. Enter the calibration constants for the pressure sensor: a. Plug the instrument into a dedicated electrical outlet. Turn the instrument on. Note: Ensure that the toggle switch on the gas addition accessory is position to Gas. b. Press the EDIT key. c. Press the right arrow key. d. Once Pressure appears, press ENTER. e. Use the arrow key(s) and select Enter Calibration. Press ENTER. f. Press EDIT to highlight the slope calibration data. Using the instrument numeric keypad, enter the value for the slope of the pressure curve. Press ENTER. Note: Calibration constants are recorded on the label attached to the 8-pin connector of the gas addition accessory and on the calibration certificate that is shipped with the Gas Addition Accessory Kit. g. Using the instrument numeric keypad, enter the value for the intercept of the pressure curve. Press ENTER. h. Press the HOME key until the Discover main screen appears. 14. Connect the gray communication cable to the gas addition accessory (Figure 9). Gray Communication Cable Pressure line cable attached to Discover in step #4 Figure 9 12
15. Insert the temperature sensor into the top of the gas addition accessory. The sensor is attached to the module with a locking collar on the sensor. Push the collar in, twist it clockwise, and release it to lock the sensor (Figure 10). Figure 10 16. Connect the communication cable into the COM 2 port on the back of the Discover (Figure 11). Figure 11 17. Enter the temperature constant (GF number) for the fiber optic probe as follows. The GF number is recorded on the label attached to the fiber optic probe as well as the label on the case in which the probe is shipped. a. From the Discover Home screen, press EDIT to access the System Setup screen. System Setup Temperature b. Press ENTER. Calibrate Temp Enter Calibration Calibrate Device Select Alternate c. Press the down arrow key until Select Alternate is selected. d. Press ENTER. Select Temp Device Device: INFRARED 13
e. Press the right arrow key until Fiber Optic Probe is selected. Select Temp Device Device: FIBER OPTIC f. Press ENTER. g. The main screen will appear. Press the EDIT key to enter in the fiber optic calibration. System Setup Temperature h. Press ENTER. Calibrate Temp Enter Calibration Calibrate Device Select Alternate i. Press ENTER to select Enter Calibration. Calibration XXXXXXX Press EDIT to change NOTE: If the fiber optic calibration number is correct, proceed to step 18. j. Press EDIT to highlight the GF number. Using the instrument numeric keypad, enter the GF number from the label attached to the fiber optic probe or the label on the plastic case in which the probe was shipped. k. Press ENTER. l. Press HOME to return to the Discover Home Screen. 18. Prior to performing a reaction, place the fiber optic probe into the thermowell, as illustrated in Figure 12, and verify that Fiber Optic is selected as the temperature option in the System Setup screen. Figure 12 14
Reaction Setup 1. Place the reaction components into a 10 ml vessel using the appropriate safety precautions based on the components used. CAUTION A stir bar is required. Ensure adequate stirring prior to performing reaction. 2. Gently place the vessel into the attenuator (Figure 13). Figure 13 3. Install the assembled locking cover on the attenuator assembly. Rotate the cover clockwise until it is tightened. CAUTION Over tightening the locking cover can cause vessel failure. WARNING Prior to each use of the gas addition accessory, ensure that the fittings (thermowell and pressure line) on the vessel top are properly tightened. Failure to tighten or over tightening these fittings may allow the vessel to leak. 4. Position the toggle switch of the gas addition accessory to Gas (Figure 14). Figure 14 5. Set the regulator on the gas tank to the desired pressure. Note: The maximum pressure allowed is 200 psi. 15
6. If installed, turn on the vacuum source. Position the valve to the Vacuum position (Figure 15). Figure 15 7. Position the valve to the Fill position to add gas to the reaction vessel (Figure 16). Toggle between Fill and Vacuum at least three times to purge the reaction. Note: Slowly position the valve from Fill to Vacuum to prevent the reaction mixture from escaping into the pressure line. Figure 16 8. After the final purge, rotate the valve to Fill to fully charge the vessel, and then to the Run position (Figure 17). Figure 17 WARNING The instrument CANNOT be operated with the reaction vessel open to the gas source. Note: The pressure in the reaction vessel can be observed on both the valve panel (located on the Gas Addition Accessory) and the Discover run screen (located on the Discover). 9. Refer to the Discover Operation Manual and enter a method. Press the Start key. A screen confirming the security of the gas addition accessory will appear. 10. Verify that the vessel is securely locked into the attenuator, the valve is positioned to Run, and the fiber optic probe is in place. Using the arrow keys, toggle to select Yes to proceed. 11. Press ENTER. The method will begin. 16
WARNING Do not attempt to remove and open a vessel prior to venting the pressure inside the vessel. To prevent injury, prior to venting the gas addition vessel, ensure that the vent tubing is positioned in a fume hood and that the end of the tubing is not pointing toward the operator or instrument. Note: If more than 200 psi of gas is required for the chemistry, additional gas can be added after the consumption of the initial 200 psi. Position the valve to Fill to recharge the vessel. This will pause the instrument. Rotate the valve back to Run and press Start to continue the reaction. 12. Once the reaction is complete, the cooling process will begin. Once cooling is complete and the system is idle, the valve can be rotated to Vent. (Figure 18). Figure 18 13. Once the pressure is vented, remove the locking cover assembly. Remove the vessel and work up the reaction using standard procedures. 17
Maintenance guide Cleaning Kit The cleaning kit (908665) is required to clean the pressure line tubing. 1. Connect the small diameter vent tubing that extends from the back of the Gas Addition Kit to the syringe as outlined below: Vent Line Figure 1 Note: If the tubing does not extend from the Vent port on the Gas Addition Accessory (Figure 1), view the sections in this manual titled Installation of Gas Addition Accessory. a. Slide the white nut (164331) onto the vent tubing, followed by the yellow ferrule (164315) ( Figure 2&3). Note: The yellow ferrule should be positioned so the narrow end of the ferrule is pointed toward the white nut. Figure 2 18
Figure 3 b. Place the red luer lock (164830) onto the end of the tubing so that the threading connect to the nut and ferrule (Figure 4). Figure 4 2. Fill the syringe with a low boiling point solvent that will dissolve any material in the tubing (such as acetone or methanol) (Figure 5). Figure 5 3. Attach the syringe to the luer lock (Figure 6). Figure 6 4. Position the valve on the pressure accessory so that Vent is selected (Figure 7). Figure 7 19
5. Position the vessel top over a waste container such as a beaker to collect the solvent as it flows from the syringe through the tubing (Figure 8). 6. Use the syringe to push the solvent through the tubing until it flows out into the waste container (Figure 8 & 9). Figure 8 Figure 9 Note: Due to the inner diameter of the tubing, extra force might be needed to flush the line. Please contact CEM Service if the liquid does not flow through the system. 7. Repeat steps 2 through 6 until the tubing is clean and free of debris. 8. Once the tubing has been completely flushed with a solvent, remove the syringe from the luer lock and fill it with air. 9. Flush the tubing with air to remove any residual solvent. 10. Remove the luer lock, ferrule, and nut from the tubing. 11. Use previous instructions to connect the Gas Addition Accessory. 20
O-ring Replacement: The O-ring should be replaced if degradation occurs or if the vessel is leaking. Prior to replacing the O-ring, ensure that all fittings, including the thermowell nut fitting, are tight. 1. Use a spatula to remove the current O-ring. 2. Discard the old O-ring. 3. Replace it with a new O-ring by pressing the new O-ring uniformly into place. Note: Check all fittings for leaks if the O-ring replacement does not resolve the problem. 21