Explorer Hybrid Automated Microwave Synthesizer. Manual

Transcription

1 TM Explorer Hybrid Automated Microwave Synthesizer Manual

2 NOTE Read these instructions carefully and thoroughly before any attempt to operate this instrument and retain them for future reference. A complete Discover SP manual (PN ) and Explorer manual (PN ) with additional information are provided. CEM provides technical and applications support for any synthesis related questions from a team of trained chemists. For applications support, call (800) (inside the US) or (704) and ask for Synthesis Applications, or synthesis.support@cem.com. Instrument Parts Explorer Hybrid Accessory Kit 4' Network/Ethernet Cable PN: Hybrid Rack PN: ' Network Cable PN: Trays (Qty:2) PN: Rack PN: Adapter PN: Ball End Adapter (Qty: 2) PN: x 9.5 MM Stir Bars (Qty: 5) PN: ml Vessel (Qty: 25) PN: ml Caps (Qty: 25) PN: Discover Accessory Kit View Discover Operations Manual, PN , for a complete list of accessories

3 Instrument Installation Installation Site The Discover/Explorer SP System may be installed in a laboratory fume hood or on a laboratory bench with proper ventilation. Choose a location that Provides at least 8 in. (20 cm) of open space on each side and 6 in. (15 cm) of open space in the rear of the instrument for ventilation. The space should be at least 22 in. (56 cm) wide by 25 in. (64 cm) deep with a height clearance of at least 35 in. (89 cm) Is free from vibration of large equipment and/or excessive walk-through traffic Provides a temperature range of 41 F (5 C) to 104 F (40 C) and a humidity range of 10-85% relative humidity Provides adequate space for sample handling and computer placement, if applicable Permits the system to be connected to a dedicated, grounded 120 VAC outlet. The Discover SP System should be operated on a stabilized, constant voltage AC power supply. To operate properly, the voltage must be within ±10 % of the specified level. Tools Required: Razor blade or box cutter. Unpack the System 1. Open the Discover SP and Explorer shipping cartons. 2. Remove the accessory kits & packing materials. 3. Carefully remove the Discover SP and Explorer modules from their shipping cartons. 4. Inspect the instrument for shipping damage such as cracks, dents, or warping. If the instrument has been damaged in shipping, contact the freight carrier to report the damage and to file a damage report. Contact CEM to report damage at Retain all packing materials for return shipment to the manufacturer if the need should arise. WARNING If damage to the instrument is noted upon receipt, do not attempt to operate the instrument. Never modify the attenuator access port or insert metallic objects, such as wire, into the port. Serious microwave leakage and/or electrical shock may result. The access port of the Discover is electrically grounded to the microwave cavity and is designed to prevent leakage of microwave energy. Cardiac pacemakers require magnets to control operation during checkout. Because the Discover SP System is equipped with a variable-speed, electromagnetic sample stirrer, some danger exists if a pacemaker is positioned in close proximity to 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. Instrument installation / 1

4 Position the System Modules 1. Place the Discover SP module on a work bench with the rear of the module facing outward. Install the two ball screws into the back of the Discover. 2. Place the Explorer Hybrid into a fume hood or on a work bench. 3. Position the Discover SP module into the Explorer base using the track in the base as a positioning guide. 4. Slide the Discover SP module back until the ball screw snaps through the Explorer module stand. 5. Place the trays, calibration tool and 10 ml Explorer rack into position. 6. Rotate the system approximately 90 degrees to access the rear of the modules. 2 / Instrument installation

5 Connect the Vent tube (PN ): 1. Remove the nut and ferrule from the end of the white connector that is not connected to the tubing. 2. Place the nut and ferrule on the tubing extending from the back of the instrument and connect it to the vent line. Ensure that the orientation of the nut and ferrule matches the picture below. 3. Place the opposite end of the tubing in the back of the fume hood or other location appropriate for solvent exposure. Connect the Power Cord and Cables 1. Connect the detachable power cord to the Discover SP module. 2. Connect the power cord of the Explorer module to the Discover SP module. 3. Plug the power cord into the electrical outlet. 4. Connect the 1' Ethernet cable to one of the Ethernet ports on the Explorer module. Connect the other end of the cable to one of the Discover module Ethernet ports. 5. Connect the 4' Ethernet cable to the second Ethernet port of the Discover SP module. NOTE The other end of this cable will connect to the computer in a later step. 6. Turn the Explorer so that the rack is facing forward. 7. Turn the Discover SP on. Instrument installation / 3

6 Connect the Air Line 1. Locate the 8' long ¼" tubing (PN BR221221). 2. Cut a perpendicular 1' section off the tubing. 3. Place the 1' section of tubing into the left side of the Discover SP module by pushing on the tubing until resistance is felt. 4. Connect the opposite end of the 1' tubing to the air regulator. The regulator has an arrow printed on it to show the direction that the air must flow. Position the regulator with the arrow pointing toward the Discover SP module. 5. Connect the air line to the opposite end of the tubing connected to the regulator. NOTE There are 2 regulator setup options. The option on the left is set up to connect the Tygon tubing (BR870002) over a barb fitting (PN BR802008). A clamp (PN BR851037) is then used to secure the connection to the barb fitting. The option on the right uses ¼" tubing (PN BR221221) designed for use with most standard NPT connections. 6. Connect the opposite end of the tubing to the air source. 4 / Instrument installation

7 7. To change the amount of air flow from the regulator: 7.1. Pull the knob out Rotate the knob on the regulator clockwise to increase the amount of air flow and counterclockwise to decrease the amount of air flow. The minimum compressed gas pressure requirement is 25 psi (20L/min flow) and the maximum pressure is 60 psi. The air flow should remain on at all times when a reaction is being performed Push the knob in to set the desired pressure. Remove the Shipping Device 1. Remove the attenuator from the cavity by rotating it counterclockwise. 2. Remove the thumb screw and shipping device from the bottom of the attenuator. Install the screw back into the shipping device. NOTE Do not throw the 35 ml shipping device away. It will be needed if the system needs to be returned to CEM for service. 3. Check the cavity for debris. Refer to the Discover SP Operation Manual (PN ) for information relating to removing debris from the cavity. Connect the Instrument to the Synergy Software NOTE If using a computer that was not furnished by CEM Corporation, install the Synergy software package on the computer as follows: 1. Plug the computer into an electrical outlet and turn it on. 2. Connect the loose Ethernet cable from the Discover SP module to the computer. 3. Select the Synergy icon to activate the Synergy software. 4. Log-in or create a new user. 5. If the following screen appears, proceed to step 6. Select Options from the menu bar and select Network Setup from the drop-down menu. Instrument installation / 5

8 6. Select Network for the Discover SP communication type. 7. Select the Explorer icon and check the Active box to activate the Explorer. 8. Select OK to save changes. 9. Select Explorer from the menu bar and select Explorer 12. Calibrate the System 1. Install the 10 ml attenuator into the cavity of the Discover SP module with the large slot positioned toward the back of the instrument. Rotate the attenuator assembly clockwise until the attenuator locks into position. 2. Install the 10 ml rack in the Explorer. Ensure that the CEM logo on each rack is facing the front of the instrument. 3. Select Explorer from the menu bar and select Explorer Calibration. 6 / Calibrate the system

9 4. Follow the steps in the Synergy software for the calibration of the racks and adapter storage, as well as the configuration of the adapter attenuator positions. After the calibration is complete, return the calibration tool to the holder on the front underside of the autosampler for convenient storage. Perform a Reaction Prepare the vessel: 1. Place a stir bar into the vessel. 2. Place all reagents into the vessel. WARNING Proper precautions must be taken to avoid contact with solvents or solvent vapors. Protective gear should be worn as outlined in the user s safety program for hazardous materials and the reagent manufacturer s material safety sheet. Refer to these guidelines for proper handling and disposal of reagents. CAUTION Vessels and caps should be used for only one (1) single reaction. Reuse of vessels and caps can jeopardize the integrity of the vessel or cap, possibly causing substantial damage to the instrument and voiding the instrument warranty. Perform a reaction / 7

10 3. Place the cap on the vessel. Perform a method using the Explorer Autosampler as follows: 1. Install the attenuator 1.1. For a 10mL reaction, install the 10mL attenuator For reactions using both vessel types (10mL and 35mL) install the 35mL attenuator. 2. Select the appropriate rack in the Synergy software Select Explorer from the Synergy toolbar. A drop-down menu will appear Highlight A 35mL Rack, Hybrid Rack: 2 (35mL) and 5 (10mL) or Hybrid Rack: 3 (35mL) and 3 (10mL) If using a Hybrid rack, place the adapter in the number 1 position, A for the Hybrid racks only. 3. Load the vessel(s) into the Explorer racks. 4. Assign the appropriate method(s) to the cell(s) that will become queued or select a sequence. The rack position(s) become highlighted (light green) once a method is loaded into that position. A sequential number will appear in the center of each of the selected rack positions chosen for the method. The number corresponds to the order in which the reaction(s) will be performed. WARNING The high temperature spill cup (162426) is required for reactions exceeding 200 o C for greater than 20 minutes or programmed temperature greater than 250 C. When replacing the spill cup, the IR sensor will require verification and possibly recalibration. 8 / Perform a reaction

11 5. From the top of the Explorer menu, select Play. The active rack position will become yellow. The Explorer will automatically retrieve the vessel from the active rack position and position it in the attenuator. The pressure device will lock into position. The method proceeds through the programmed parameters. Note: During the method operation, the hotkeys can be used to edit method parameters. The hotkeys can be utilized from either the Discover SP System keypad or from the Synergy software. NOTE To stop a reaction prior to completion, select the Stop button. The reaction is stopped and cannot be resumed. Once the method is stopped, cooling begins prior to release of the vessel. Once the vessel is cooled sufficiently, the pressure device will release from the attenuator and move into the idle position. The instrument will then remove the vessel from the attenuator and place it into the proper rack position. In the software, the appropriate rack position is displayed in red, indicating that the user stopped the reaction. Remove the vessel: 1. Once the method is complete, the cooling cycle will begin. Once the cooling is complete, the vessel will be returned from the attenuator to its proper rack position. 2. After the vessel has been returned to the Explorer rack, it may be removed from the rack. CAUTION To prevent the possibility of severe burns, ensure that insulated gloves and protective gear as outlined in the user s safety program are worn. Contents may be under pressure and should be released within a fume hood. 3. If applicable, vent any residual pressure from the vessel using a needle to pierce the septa. 4. With the top of the vessel tilted toward the back of the hood, or otherwise away from the user, carefully remove the cap from the reaction vessel. 5. Discard the cap. 6. Perform the workup. Perform a reaction / 9

12 USA: CEM Corporation (Headquarters) PO Box 200 Matthews, NC United States Fax: France: CEM μwave S.A.S. Immeuble Ariane Domaine Technologique de Saclay 4, rue Rene Razel, ORSAY Cedex 33 (01) Fax: 33 (01) Germany, Austria, Switzerland: CEM GmbH Carl-Friedrich-Gauss-Str.9, Kamp-Lintfort (49) Fax: (49) Ireland: CEM Technology (Ireland) Ltd. Sky Business Centre, 9a Plato Business Park, Damastown, Dublin (0) Fax: +353 (0) info.ireland@cem.com Italy: CEM S.R.L. Via Dell Artigianato, 6/ Cologno al Serio (Bg) (39) Fax: (39) info.srl@cem.com Japan: CEM Japan K.K Takanawa, Minato-ku, Tokyo Fax: info@cemjapan.co.jp United Kingdom: CEM Microwave Technology Ltd. 2 Middle Slade, Buckingham Industrial Estate, Buckingham MK181WA (44) Copyright 2018 by CEM Corporation All Rights Reserved. This guide contains proprietary information which shall not be reproduced or transferred to other documents or disclosed to others without prior written permission of CEM Corporation. CEM and Discover are registered trademarks of CEM Corporation. Part Number February 7, 2018 Rev. 4 Copyright CEM Corporation 2018