CEM Discover SP-D Operation Manual

600857 Rev. 1 8/17

Operation Manual

This manual 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 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

Table of Contents

Operating Precautions ............................................................................................................................................................. 1

Warnings and Cautions ........................................................................................................................................................... 1

Introduction ............................................................................................................................................................................... 2

Instrument Description ............................................................................................................................................... 3

Front View .......................................................................................................................................................................... 3

User Interface .................................................................................................................................................................... 3

Keypad ............................................................................................................................................................................... 4

Method Status Bar ............................................................................................................................................................ 4

Rear View .......................................................................................................................................................................... 5

Side Views ......................................................................................................................................................................... 5

Sample Stirrer .................................................................................................................................................................... 6

Cooling ............................................................................................................................................................................... 6

System Installation ................................................................................................................................................................... 7

Installation Site .................................................................................................................................................................. 7

Unpacking .......................................................................................................................................................................... 7

Discover SP Installation .................................................................................................................................................... 8

Computer Installation (optional) ........................................................................................................................................ 9

User Login .................................................................................................................................................................. 11

User Logout ................................................................................................................................................................ 11

Microwave Tips........................................................................................................................................................... 12

Closed Vessel 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 Setup .................................................................................................................................................................... 26

User Setup ......................................................................................................................................................................... 27

Temperature Type ............................................................................................................................................................. 27

Release Limiits .................................................................................................................................................................. 27

User Profiles ................................................................................................................

Clear Password ................................................................................................................................................................. 28

Change Password ............................................................................................................................................................. 28

User Profile Defaults -1 ..................................................................................................................................................... 28

Hold Time .......................................................................................................................................................................... 28

Ramp Time ........................................................................................................................................................................ 29

Temperature ...................................................................................................................................................................... 29

µ Power ........................................................................................................................................................................... 29

...................................................... 28

iii

User Profile Defaults- 2 ............................................................................................................................................................ 29

Stirring ................................................................................................................................................................................ 29

Pre-Mix Time ..................................................................................................................................................................... 30

Pressure ............................................................................................................................................................................. 30

Pressure Units .................................................................................................................................................................. 30

User Profile Defaults- 3 ............................................................................................................................................................ 30

Key Beep ........................................................................................................................................................................... 30

Clock Format ..................................................................................................................................................................... 30

Cooling Time ..................................................................................................................................................................... 31

Backup Methods ................................................................................................................................................................ 31

Restore Methods ............................................................................................................................................................... 31

Calibration Setup ............................................................................................................................................................... 31

Temperature ...................................................................................................................................................................... 32

Infrared ............................................................................................................................................................................... 32

Slope .................................................................................................................................................................................. 32

Fiber Optic ......................................................................................................................................................................... 33

Slope .................................................................................................................................................................................. 33

Pressure (10mL APM) ...................................................................................................................................................... 34

Network Setup ................................................................................................................................................................... 34

IP Address ......................................................................................................................................................................... 34

Sub Net Mask .................................................................................................................................................................... 35

Serial Number .................................................................................................................................................................... 35

Peripheral 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 leakage Measurement ................................................................................................................................... 47

Power Test ......................................................................................................................................................................... 48

Manual Power Test ........................................................................................................................................................... 48

Auto Power Test ................................................................................................................................................................ 49

Vessel Failure Cleanup Procedure .................................................................................................................................. 52

Troubleshooting Guide ...................................................................................................................................................... 54

Specifications .................................................................................................................................................................... 55

Warranty ............................................................................................................................................................................ 56

Operating Precautions

The Discover® SP-D Clinical System must be grounded. In the event of an electrical short circuit, grounding reduces the risk of electric shock by providing an escape wire for electrical current. This instrument is equipped with a cord having a grounding wire with a grounding plug. The plug must be installed into an electrical outlet that is properly installed and grounded. Consult a qualified electrician or service technician if the grounding instructions are not completely understood or if doubt exists as to whether the instrument is properly grounded. If it is necessary to use an extension cord, use only a 3-wire extension cord that has a 3-blade grounding plug and a 3-slot receptacle that will accept the plug from the instrument. The marked rating of the extension cord must be equal to or greater than the electrical rating of the instrument.

The possibility of instrument-induced electromagnetic interference (EMI) is minimal if the instrument is operated as outlined in this manual. The instrument should not be placed close to any electrical device susceptible to EMI. The manufacturer suggests that the user post a sign warning pacemaker wearers that a microwave device is in operation. If the instrument is suspected of inducing EMI, a microwave leakage measurement should be performed as outlined in this manual. Any leakage above the legal limit of 5 mW/cm

Cardiac pacemakers require magnets to control their operation during checkout. Because the instrument is equipped with 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 microwave radiation. Only those trained in repair and maintenance of

high voltage and microwave power systems should perform instrument service and repair.

Use of the Discover instrument in any manner not specified by CEM Corporation could render the instrument operation unsafe for the operator.

This instrument complies with United States Code of Federal Regulations 21CFR Part 1030.10 (C) for microwave leakage. A verification report is on file. This instrument complies with FCC Requirements in the United States Code of Federal Regulations (47CFR Part 18) Industrial, Scientific and Medical (ISM) Equipment emissions requirements. A verification report is on file.

2 should be reported to the CEM Service Department.

Warnings and Cautions

Warnings, cautions and notes are included throughout this manual and should be read thoroughly and strictly followed.

WARNING

A warning is inserted for essential information used to emphasize dangerous or hazardous conditions to the operation, cleaning and maintenance of the instrument which may result in personal injury.

CAUTION

A caution is inserted for essential information used to emphasize procedures which, if not strictly followed, may result in damage or destruction to the instrument or improper instrument operation.

NOTE

A note is inserted for emphasis of procedures or conditions that may otherwise be misinterpreted or overlooked and to clarify possible confusing situations.

Introduction

The CEM Focused Microwave Discover® SP-D Clinical System is designed to enhance the ability to perform acid digestions under controlled conditions on a laboratory scale. It accommodates 4 mL and 10 mL vessels for reactions performed at elevated temperatures and pressures.

The SP-D Clinical system also incorporates ActiVent Technology that 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.

Microwave energy is applied to the vessel contents (reactants, catalysts, salts, solvents and/or solid supports) to accelerate the chemical reaction. The microwave absorption properties of some liquid and solid materials, due to their polar and ionic characteristics, have the capability to significantly enhance chemical reactions relative to traditional energy application (heating) techniques. The microwave interaction properties with the reactants, intermediates, catalysts, solid supports and salts provide unique opportunities for the synthetic chemist.

The Discover SP-D Clinical Sy stem consi sts of:

• A continuous microwave power delivery system with operator selectable power output from 0 - 300 watts (+/- 30

watts) programmable in 1-watt increments.

• A self-adjusting, 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 232).

• Two (2) ethernet ports for computer interface and network connection (optional configuration).

• One RJ-11 port for peripheral connection.

• An accessory kit.

• Two (2) USB ports..

• Infrared Temperature Control System - This temperature control system uses a non-contact, infrared sensor to

measure temperature. It is located below the microwave cavity floor and measures the temperature on the bottom of

the vessel. The sensor is vessel volume independent and is used in a feedback loop with the on-board computer to

control the temperature rise rate and control point of the vessel contents. Temperature is programmable from

C to 220oC.

• Stirring Option - The stirring option consists of an electromagnetic plate located below the floor of the microwave

cavity. Stirring occurs when the magnetic field couples with a stir bar in the vessel. The method setup enables

the stirring feature and the stirring speed. Standard stir bars appropriate to the vessel size are used.

• Cooling Option - The cooling option consists of necessary valves and ports to direct a cooling gas (either

nitrogen or clean air) onto the vessel in the system cavity. This option will decrease the temperature of a 2mL

solution in a 4 mL or 10 mL Pyrex reaction vessel from ~150ºC to ~50ºC in less than 120 seconds. Method setup

enables the cooling feature.

Instrument Description

Front View

User Interface

The user interface consists of the keypad and display which provide the means for the user to input information into and output information from the Discover System.

The input functions are performed with the keypad and provide the ability to

● create new methods and edit existing methods,

● recall and delete methods,

● change operating parameters during method operation in real time,

● start, pause and stop operation,

● set up a computer (optional),

● configure the sensor options and system options,

● create and edit user profiles.

The output functions are obtained from the display and computer/ethernet port. The display provides visual information of the keypad entry and permanently stored instrument information. The computer/ethernet port provides the option 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 operation.

The attenuator can be installed or removed with a twist-lock action (no tools required).

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 SP-D Clinical is electrically grounded to the microwave cavity and is designed to prevent leakage of microwave energy.

● Interlock Assembly - monitors mating of the attenuator to the cavity. If the attenuator is not properly installed,

the instrument will not deliver microwave power nor permit the system to operate.

WARNING

Keypad

• HOME - Press to return to the main screen from any menu in the software. Within the System Setup portion of

the software, press this key to return to the previous menu.

• START/PAUSE - Press to start the current method or press during method operation to pause or suspend

operation. Pressing the key again will restart the method from the paused point.

• ENTER - Press to accept entries while editing or creating a method or in System Setup.

• DISCOVER - Press to load, save and create methods and review data. Pressing this key permits navigation

through and selection of program options.

• STOP - Press to stop any process. Pressing this key when performing a method will stop microwave radiation

and launch the cooling function. Pressing this key during the cooling cycle will abort the cooling cycle and return

the system to the home screen.

• ARROW - Press to navigate through method programming or System Setup steps.

• +/- Press to increase or decrease highlighted method parameters or to navigate through System Setup steps.

• POWER - Press this key to change the maximum applied microwave power setting prior to or during a method.

Use the +/- keys to increase or decrease the setting. If this key is pressed during a method, this does not stop or pause the method but updates the setting in real time. The updated setting is not captured as part of the saved method file in the method library.

• STIRRING - Press this key to change the stirring setting prior to or during 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 key

is pressed during a method, it does not stop or pause the method but updates the setting in real time. The updated setting is not captured as part of the saved method file in the method library. If this key is pressed while the instrument is idle, the PowerMax option appears.

• TEMPERATURE - Press this key to change the temperature setpoint before or during a method. Use the +/- keys

to increase or decrease the setting. If this key is pressed during a method, this does not stop or pause a method but

updates the setting in real time. The updated setting is not captured as part of the saved method file in the

method library.

• PRESSURE - Press this key to change the pressure set point prior to or during a method. Use the +/- keys to

increase or decrease the setting. If this key is pressed during a method, this does not stop or pause a method but

updates the setting in real time. The updated setting is not captured as part of the saved method file in the

method library.

• TIME - Press this key to change the time value during or after a method. Use the +/- keys to increase or decrease

the time setting. Pressing this key allows for real time changes to this value. This does not stop or pause a

method but updates the setting in real time.

Method Status Bar

Rear View

Power Cord Receptacle - Receives the female end of the power cord. Magnetron Cooling Fan - Draws room air past the magnetron for cooling purposes. Power Supply Cooling Fan - Draws room air past the power supply for cooling purposes. Fuses - Prevent electrical power overload. Electrical Connector - Connects autosampler or other peripheral accessory to the reactor

module.

RS232 Port - Allows additional connection and communication. Spill Tray - Removable collection tray for cavity 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 connection for the cooling gas source. 7-Pin Connector - Connects pressure measurement device to the main controller board. USB Ports - Permit installation of USB flash drive to import, export, backup and/or save instrument data. RJ 11 Port - Permits connection and use of additional accessories.

Sample Stirrer

The sample stirrer is a plate containing electromagnetic coils positioned beneath the instrument cavity floor. The electromagnetic stirring plate works in conjunction with stirring bars placed in the reaction vessel to affect stirring and ensure a homogeneous sample. An initial supply of magnetic stir bars are provided with the system. Additional stir bars are available from CEM Corporation. Commercial Teflon® coated magnetic stir bars can be used.

NOTE: The stir bars are Teflon®-coated iron oxide bars. When placed in the microwave field, the iron oxide bars will reflect the microwave energy without damaging the instrument.

WARNING

Cardiac pacemakers require magnets to control operation during checkout. If the Discover System is equipped with a 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.

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 off and is part of the method. The feature consists of:

• plumbing to direct the gas from the inlet point of the Discover to the reaction vessel in the cavity, a solenoid valve connected to the CPU (controller) board to turn the gas flow on and off,

• A hose fitting to connect the Discover to the gas source via hose, and

• 8 feet (2.44 meters) of 1/4 inch (6.35 mm) inside diameter air hose.

The gas source is user supplied. CEM Corporation recommends either nitrogen or clean air at a minimum pressure of 25 psi (~ 1.5 bar). This will provide a flow rate of 20 liters per minute and will cool a 5mL volume of ethylene glycol in a 10mL reaction vessel from 150°C to less than 50°C in less than 2 minutes.

System Installation

Installation Site

The Discover System is designed for installation 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. (46 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 or 240 VAC outlet. The Discover System should be

operated on a stabilized, constant voltage AC power supply. To operate properly, the voltage must be within 10% of specified level.

Unpacking

Carefully remove the system from its shipping carton and place it in an appropriate location in the fume hood or on a laboratory bench.

Note: Retain all packing material for use if returning the system to the manufacturer, subsidiary or distributor for service.

Inspect the instrument 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 insert metallic objects such as wire into the port. Serious microwave leakage and/or electrical shock may result. The access port of the instrument 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 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.

Disconnect the instrument from the AC power source prior to performing any service procedure.

If the instrument has been damaged in shipping, contact the freight carrier to report the damage and to file a damage report. Contact the CEM Service Department or the local subsidiary or distributor to report damage and to request service information.

Discover SP-D Clinical Installation

1. Place the Discover in a hood or on bench.

2. Plug the power cord into the back of the instrument.

3. Remove the vent tubing from the accessory kit and connect to the rear of 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 the regulator.

NOTE: The regulator has an arrow printed on it to show the direction that the air must flow. Set up the regulator according to

the arrow.

ir Flow Arrow

d. Place the second length of tubing into the opposite end of the regulator.

e. Connect the opposite end of the tubing to the air source. f. To change the amount of air flow from the regulator:

Pull the knob on the regulator outward. Rotate the knob clockwise to increase the amount of air flow. Rotate the knob counterclockwise to decrease the amount of air flow. The minimum compressed gas requirement is 25 PSI (20L/min flow). The maximum flow rate is 60 PSI.

Note: The air flow should remain on at all times when a reaction is being performed.

7. Check the cavity for debris.

8. Using the power switch 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 Ethernet ports located at the rear of the Discover.

2. Connect the opposite end of the Ethernet cable extending from the Discover to the computer.

3. Ensure that the computer is turned on and the desktop is visible. Select the Synergy icon to activate the Synergy software. If the Synergy icon is not visible on the desktop, insert the Synergy CD and follow the on-screen instructions.

Note: If this is the first time the software has been activated on the computer, the user will be prompted to create a new

account.

4. Using the pull-down menu, select the proper name and enter the appropriate password. Select “OK.” Synergy will automatically load the user’s preferences and connect to the Discover and Explorer modules during the login process.

5. Select “Network Setup.” The following screen will appear.

6. Select the Discover icon.

7. The IP Address should read “192.168.1.60.” If the IP Address does not read as shown, highlight the IP Address, and using the computer keyboard, enter the correct IP Address.

8. Select “OK.” The icons in the status bar will become green and show that the instruments are connected.

9. If the icons are red and the system is not connected, follow the procedure as outlined below to assign a fixed IP Address to the PC/Laptop:

a. Right click the “My Network Places” icon on the desktop and select “Properties.” This will open the “Network

Connections” window.

b. Right click “Local Area Connection” and select “Properties.” This will open the “Local Area Connections

Properties” window.

c. Select the “General” 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 up to 3 numeric

characters per set. Each set is separated by a period (.). In the Discover System, the first character after a period can be a zero (0). However the first numeric character cannot be a zero when entered into the PC/Laptop IP Address box. The first two sets of Fixed IP Address numbers for the PC/Laptop must match the first two sets of numbers in the Discover IP Address. However, the PC/Laptop’s Fixed IP Address must be unique, thus the reason to decrement the last set of numbers.

g. Press the “OK” button. This will close the Internet Protocol (TCP/IP) Properties window and return the user to the

“Local Area Connections Properties” window. h. Select the “close” button to return to the “Network Connections” window. i. Close this window to return to the Desktop. j. Follow the above steps 1 – 8.

User Login

Before system operation can begin, the user is required to log into the Discover system. The Discover software is designed to permit use by three types of users: Standard, Administrator and Guest. The Discover is originally equipped with an “Administrator,” “User” and “Guest”. The “Administrator” login cannot be deleted. Refer to instrument setup for instructions to create administrative, guest and standard user profiles.

Administrator- can add, modify, or delete users; perform tasks related to the maintenance of the

system; modify all system settings and perform methods.

Standard- can perform methods and modify all system settings. Guest- can perform methods.

1. When the instrument is turned on, the “Login” screen will appear. Use the “+/-” keys to select 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 password has been entered. d. Once the password is entered, use the ARROW and “+/-” keys to highlight “OK.” e. Press ENTER to log in.

User Logout

Once system operation is complete, the user can log out of the system. If the system is idle for 20 minutes or longer, the system will automatically go into an idle mode and the user will be required to log in to continue operation.

1. To log out, press HOME until the “Discover Home” screen appears.

2. Use the “+/-” keys to highlight “XXX-Logout.”

NOTE: The user name will appear where the “XXX” are located.

3. Press ENTER to log out.

Microwave Tips

Cover all solids in the reaction vessel with liquid. Never exceed the maximum working volume of the vial. Always use a stir bar that adequately mixes the reaction contents in the microwave. Reactions can be performed under an inert atmosphere. 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

4 mL 0.200 – 2.0 mL Sealed

10 mL 0.200 – 5.0 mL Sealed

Working Volume Sealed/Pressurized or

Open/Atmospheric

Closed Vessel Extraction

Items Required:

4mL/10mL Attenuator 4mL/10mL mL Vial Stir bar appropriate for vial size 4mL/10mL Cap

Prepare the Vial

1. Select the vial based on the volume of solvents being used.

NOTE: The working volume for the 10mL vial is 0.2mL to 5mL. The working volume for the 4mL vial is 0.2mL to

2mL.

2. Place an appropriate stir bar into the vessel.

3. Place the reaction components into the vessel.

Proper precautions must be taken to avoid contact with acids or acid vapors. Protective gear should be worn as outlined in the user’s safety program for hazardous materials and the reagent manufacturer’s material safety data sheet. Refer to these guidelines for proper decontamination, handling and disposal of reagents or any hazardous materials.

4. Place the cap onto the vial.

The Discover SP-D Clinical is usable only with CEM supplied 4mL or 10mL reaction vessels and caps for sealed reactions.

5. Install the appropriate attenuator 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 software “Help” text for creating a method).

2. Press the START/PAUSE key. The ActiVent will close and lock onto the vessel. The “Waiting” screen appears prior to irradiation initiation. Once the method begins, the system ramps to set-point temperature. The system continues to meet method parameters to perform the complete method.

NOTE: The information across the bottom of the screen displays the parameter status as follows:

Pressure (Bar or PSI) Power (W) Stirring (H {High}, M {Medium}, L {Low} or Off (X) Temperature Control (IR {Infrared} or FO {Fiber Optic)} Vessel Type - If the vessel is a sealed vessel, the size will be displayed beside the picture of the vessel. Cooling (Off or On) - If Cooling is “on,” a snowflake is displayed. Microwaves (Off, On) System accessories (D {Discover}, or E {Explorer})

WARNING

Remove the Vessel

1. Once the vessel is properly cooled, the ActiVent will release the vessel and “Complete” will appear on the Display. If the ActiVent does not automatically release the reaction vessel, the pressure (or temperature) is above the release limit. A message will appear indicating the current temperature and pressure value. Cool the reaction vessel completely and manually release the ActiVent.

2. Rotate 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 the septa to vent the pressure.

4. Remove the cap from the vessel by pressing upward on one side of the cap.

WARNING

Vessels and caps are designed for only one use. Do not use vessels and/or caps more than one time.

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-toTemperature. 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.

+ 42 hidden pages

CEM Discover SP-D Operation Manual

Specifications and Main Features

Frequently Asked Questions

User Manual