CEM PETwave Operating instructions

Brand: CEM

Model: PETwave

Type: Operating instructions

PETwaveTM

Microwave-Assisted Radiosynthesis

Manual

Contents

Instrument Overview

PETwave 1

Microwave 1

Stirring 1

Temperature 1

Cooling 1

Pressure 1

Safety instructions

Safety Notations 2

Operating Precautions 2

Instrument Parts & Accessories

Standard Parts 3

Optional Parts 4

Instrument Components

Microwave Controller 5

Remote Microwave Cavity 6

Instrument Installation

Location 7

Unpacking 8

Attach Cables/tubing 8

Turn instrument On/Off 10

System Verication 10

Instrument Operation

PETwave display and Keypad with onboard software 11

Synergy Software (Optional) 12

Synergy Software Connection (Optional)

Download Synergy Software 14

IP Address 14

Synergy 18

Perform a Reaction

Prepare Sample 19

Microwave 20

Remove Sample 21

General Settings

Integrated PETwave Software 22

Synergy 23

Instrument Calibration and Verification

Temperature Calibration 28

Temperature Verication 29

Stirring Verication 29

Methods

Method Types 31

Integrated PETwave software 32

Synergy Software 37

Data Review

Integrated PETwave software 41

Synergy Software 41

Routine Maintenance & Cleaning

Infrared Sensor 43

Microwave cable 43

Service Utilities

Firmware Update 44

PETwave Information 45

Technical Data

Dimensions (Overall) 46

Troubleshooting

Troubleshooting 48

Warranty

Limited Warranty Information 49

Technical Assistance

Requested Information 50

Contact Information 50

Instrument overview / 1

Instrument Overview

PETwave

The CEM PETwave™ is designed to enhance the ability to perform chemical reactions under controlled conditions

on a small scale inside a ‘hot’ cell or glove box. The system facilitates solution phase chemistry, solvent

evaporation to concentrate reactants and hydrolysis to remove protecting groups. It accommodates conical shaped

vessels ranging in working volume from 50 µL to 2.5 mL. Primary uses of the PETwave™ are for radiolabeling

chemistry in a ‘hot’ cell or chemistry in the controlled environment of a glove box.

Microwave

Microwave energy is applied to the vessel contents (reactants, catalysts, salts, solvents) 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 signicantly enhance chemical reactions relative to traditional energy

application (heating) techniques. The microwave interaction properties with the reactants, intermediates, catalysts,

and salts provide unique opportunities for the synthetic chemist. Power is programmable in 1 watt increments from

0 to 100 watts.

Stirring

Stirring is accomplished using electromagnetic stirring plates located beneath the cavity in conjunction with stir

bars placed in the reaction vessel; ensuring a homogeneous sample. The stir bars must be Teon® coated iron

oxide bars. When placed in the microwave eld, the iron oxide bars will reect the microwave energy without

damaging the instrument. Stirring can be programed as off, low medium or high.

WARNING

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.

Temperature

Temperature is measured by an Infrared Control System. This temperature control system uses a non-contact,

infrared sensor located below the microwave cavity oor. 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 room temperature to 300oC.

Cooling

Cooling – The cooling feature consists of necessary solenoid valves and ports to direct a cooling gas (either

nitrogen or “clean” air) onto the outside wall of the reaction vessel. This provides the ability to rapidly cool

(quench) a reaction after the application of microwave energy. Cooling is programmable as on or off and may be

adjusted using the regulator up to 60 psi.

Pressure

Reactions are performed at or below boiling point of the solvent; therefore, reactions may only performed at

ambient/atmospheric pressure.

2 / Safety instructions

Safety instructions

Safety Notations

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

followed. The following conventions for safety messages are used in this Operations Guide:

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 use 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.

Operating Precautions

The PETwave™ 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 electric current. This instrument is equipped with a cord having

a grounding wire with a grounding plug. The plug must be plugged into an outlet that is properly installed and

grounded. Consult a qualied 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.

If the instrument is suspected of interfering with the operation of a cardiac 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 PETwave in any manner not specied by CEM Corporation could render the instrument operation unsafe

for the operator.

Instrument parts & accessories / 3

Instrument Parts & Accessories

• Retain all packing material for use if returning the system to the manufacturer, subsidiary or distributor for

service.

• If a part is missing, contact your CEM representative.

• 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 le a

damage report. Contact the CEM Service Department or the local subsidiary or distributor to report damage and

to request service information.

WARNING

If damage to the instrument is noted upon receipt, do not attempt to operate the instrument.

Standard Parts

Image Qty Item Part Number

1 Microwave Controller with Microwave transmission cable connected N/A

1 Remote Microwave Cavity N/A

2 4 mL vial (50 µL-0.5 mL working volume) 186400

2 2 mL vial (100 µL-1.0 mL working volume) 186410

2 1 mL vial (250 µL-2.5 mL working volume) 186405

Multi-port Cap (7 ports for reagent addition, vacuum drying, gas

purging, and sample removal)

bottom piece

Silicone o-ring

Top head

186420

186435

186425

4 / Instrument parts & accessories

20 Cap SP-1547

1Regulator

1/4" brass tting adapter

541455-M

BR163380

Cooling Line assembly

Tubing, PFA, 3/16"

Nut 3/16"

Ferrule, 3/16”

BR199117

167315

167320

1 Temperature Cable, 8 pin N/A

1 Stirring Cable, 6 pin N/A

Power cord

USA (120 V)

Export (230 V)

119635

119645

1 Operations Guide 600864

10' Tubing 1/4" BR22122

Optional Parts

Item Description Part Number

Synergy Software Option

The Synergy Software Option is a PC-based software package that allows the

user to program, monitor, and control all PETwave system functions. The option

includes a laptop computer with Synergy software loaded and both Ethernet

and serial cables to communicate directly to the PETwave. The package creates,

and allows for the full management of a database for all system reaction data.

When placed on a network, the current instrument status is visible from a

remote location.

909105

Synergy Laptop Option The laptop option includes the Synergy software along with a laptop computer . 909110

Instrument components / 5

Instrument Components

Microwave Controller

Front

• Display - 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.

• Keypad - allows the operator to create, edit, store and recall methods, start and stop methods and change

programmed parameters during operation.

Right

• USB Ports (2) - Permit installation of USB memory stick to import, export, backup, and/or save instrument data.

• Ethernet port - The PETwave does not utilize this feature.

• 7 Pin Connector - The PETwave does not utilize this feature.

Rear

• Fuses/Fuse holder - Prevent electrical power overload.

• Power inlet - 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.

• Electrical Connector - The PETwave does not utilize this feature.

• RS232 Port - Allows additional connection and communication.

• Ethernet Port (2) - 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.

• 6 pin Stirrer Connector - Connects the electromagnetic plate located in the Remote Microwave Cavity to the

control board located in the Microwave Controller.

• 8 pin Temperature Connector - Connects the infrared temperature sensor located in the bottom of the Remote

Microwave Cavity to the Microwave Controller.

• Cooling Gas Line - Provides a hose connection for the cooling gas source.

6 / Instrument components

Left

• Power switch - Turns AC power on and off to the instrument.

• Cooling Gas Line – Provides a hose connection for the cooling gas source. The cooling feature consists of

necessary solenoid valves and ports to direct a cooling gas (either nitrogen or “clean” air) onto the vessel in the

system cavity.

• Microwave Transmission Cable - Connects the microwave generation component within the Microwave Controller

to the Remote Microwave Cavity. This is the larger blue cable extending from the left side of the microwave cavity.

Use caution when bending/moving this cable.

Remote Microwave Cavity

• Microwave Transmission Port - Connects the Remote Microwave Cavity to the Microwave Controller. Safety

interlock and an interlock monitoring system to prevent microwave emission when the microwave transmission

cable is not properly installed.

• 6 Pin Stirrer Port - Connects the electromagnetic plate located in the Remote Microwave Cavity to the control

board located in the Microwave Controller.

• 8 Pin Temperature Port – Connects the infrared temperature sensor located in the bottom of the Remote

Microwave Cavity to the Microwave Controller.

• Cooling Inlet – Supplies compressed gas from Microwave Controller to the Remote Microwave Cavity.

• Multi-port Cap Holder Pin – Keeps multi-port cap in position during reaction.

Instrument installation / 7

Instrument Installation

WARNING

If damage to the instrument is noted upon receipt, 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 PETwave 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 PETwave 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.

CAUTION

Before connecting power cord to PETwave, ensure proper line voltage is available (120V vs 240V). If large

voltage uctuations are expected, a constant voltage source (UPS) is required.

Location

• Choose a location for the Microwave Controller that is in close proximity, less than 10 feet, to the ‘hot’ cell

or glove box.

• Provides enough space for Microwave Controller: 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 31 in. (77 cm) wide

by 23 in. (59 cm) deep with a height clearance of at least 10 in. (89 cm).

• Provides enough space in hot cell for Remote Microwave Cavity: At least 10 in. (25 cm) wide by 10 in. (25 cm)

deep with a height clearance of at least 15 in (38.1 cm).

• Is free from vibration of large equipment and/or excessive walk-through trafc.

• 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), and

• Permits the system to be connected to a dedicated, grounded 120 or 240 VAC outlet. The PETwave System

should be operated on a stabilized, constant voltage AC power supply.

8 / Instrument installation

Unpacking

1. Verify all parts and accessories are available. View “Instrument Parts and Accessories” for the list.

2. Carefully remove the Microwave Controller from its shipping carton and place on an appropriate location near

the ‘hot’ cell or glove box.

CAUTION

Do NOT use force to bend microwave transmission cable (blue cable extending from left side of

instrument). Extreme bending of the microwave transmission cable will render the PETwave inoperative.

3. Place the Remote Microwave Cavity inside the hot cell or glove box.

Attach Cables/tubing

1. Insert the power cord into the power inlet receptacle located on the back of the instrument and the opposite

end into the electrical outlet.

2. Connect the 8 pin temperature cable and 6 pin stirrer cable to the Microwave Controller.

3. Connect the cooling line tube to the tube extending from the back of the Microwave Controller.

Instrument installation / 9

4. Connect the cooling line tube to the Remote Microwave Cavity.

5. Connect the 8 pin temperature cable to the Remote Microwave Cavity.

6. Connect the 6 pin stirrer cable to the Remote Microwave Cavity.

7. Install blue microwave transmission cable extending from the left side of the Microwave Controller to the Re-

mote Microwave Cavity. Turn nut until nger tight.

CAUTION

Do NOT use force to bend microwave transmission cable. Extreme bending of the microwave transmission

cable will render the PETwave inoperative.

Over tightening the nut can damage the microwave transmission cable. Under tightening the microwave

transmission cable will cause a “door open” error on the Microwave Controller.

8. Connect the pressure regulator to either a nitrogen or clean air supply.

8.1. Cut the ¼" tubing in half.

8.2. Install one length of the tubing into the left side of the Microwave Controller by pushing in on the

tubing until resistance is felt.

8.3. Place the opposite end of the tubing into the regulator.

10 / Instrument installation

NOTE

The regulator has an arrow printed on it to show the direction that the air must ow. Set up the regulator

according to the arrow.

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

8.5. Connect the opposite end of the tubing to the air source.

8.6. To change the amount of air ow from the regulator

8.6.1. Pull the knob out.

8.6.2. Rotate the knob on the regulator clockwise to increase the amount of air ow.

8.6.3. Rotate the knob on the regulator counter clockwise to decrease the amount of air ow.

8.6.4. The minimum compressed gas requirement is 25 psi (20 L/min ow).

8.6.5. The maximum ow rate is 60 psi.

Turn instrument On/Off

1. Position Microwave Controller on bench top and Remote Microwave Cavity in hot cell or glove bag.

2. Turn the instrument on using the power switch on the left side of the Microwave Controller. The software will

take up to a minute to load. While in the reaction programming screen, If a round bottom ask does not appear

in the lower right corner of the software, then the blue microwave transmission cable has not been securely

fastened and a “Door Open” message will appear. See section “Attach cables/tubing” for instructions on how

to install the blue microwave transmission cable.

3. To switch the instrument off, use the power switch. The PETwave system can be turned off or left on when not

in use. The system is ready to run once the software has completely loaded.

System Verification

See section “Instrument Calibration and Verication.”

Instrument operation / 11

Instrument Operation

There are two interfaces for operating the PETwave; the integrated software using the keypad and display or

Synergy software. Synergy is an optional data management software.

PETwave display and Keypad with onboard software

Keypad

HOME

STIRRING

POWER

START/PAUSE

COOLING

ENTER DISCOVER

TEMPERATURE

+/- STOP

TIME

PRESSURE

ARROWS

• HOME – Press this key to return to the previous menu or home screen.

• START/PAUSE – Press to start the current method or pause during method operation.

• 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.

• 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.

If this key is pressed during a method, this does not stop or pause the method but updates the setting in real

time.

• 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.

• COOLING – Press this during a method to perform the cooling function.

• 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.

• PRESSURE – The PETwave does not utilize this feature.

• 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.

12 / Instrument operation

Display

Shows menus, method parameters and instrument status on a 256 x 128 graphics display.

Rxn Programming Discover Home Load, Save, Create Method

Synergy Software (Optional)

The Synergy Software is a PC-based software package that allows the user to program, monitor, and control all

PETwave system functions. The package creates and allows for the full management of a database for all system

reaction data.

Menu Bar

File

• New Folder - The “New Folder” function allows a user to create a new folder to store methods under. To create

a new folder, select “New Folder” from the “File” drop-down menu, enter the name you wish to use for the new

folder, and then click “OK”. Click “Cancel” to exit without creating a new folder. A new folder can only be created

within an existing folder.

• Rename Folder - The “Rename Folder” function allows the user to change the name of the currently highlighted

folder. After selecting the “Rename Folder” option from the “File” drop-down menu, the user must enter the new

folder name, then click “OK”. Clicking “Cancel” will exit without renaming the folder.

• Delete Folder - The “Delete Folder” function allows the user to permanently erase the highlighted folder. After

selecting the “Delete Folder” option from the “File” drop-down menu, the user must click “OK” to conrm the

deletion. Clicking “Cancel” will exit without deleting the folder.

• Log Off - The “Log Off” function allows the current user to be logged out and takes the user to the log-in screen.

• Change Password - The “Change Password” function allows the user to change the password used to log into

the current user’s prole. The user must enter their current password, then enter the new password twice for

conrmation.

• Exit - The “Exit” function closes the Synergy software and returns the user to the desktop.

Instrument operation / 13

Method

• See “Methods” section for details.

Mode

• Explorer -The PETwave does not utilize this feature.

Instrument Keys

• Start - The “Start” function initiates the method operation. To run a method, the user must select a method from

your user prole, then select “Start” from the “Instrument Keys” drop-down menu. A method can also be started

by selecting the START button.

• Pause - The “Pause” function interrupts the currently processing method. To pause a method, the user may

select “Pause” from the “Instrument Keys” drop-down menu. A method can also be paused by using the PAUSE

button. To restart the method, press the START button.

• Stop - The “Stop” function immediately stops the currently running method and initiates the quenching function.

To stop a method, the user may select “Stop” from the “Instrument Keys” drop-down menu. A method can also

be stopped by using the STOP button.

Data

• See Section “View Data” for details.

Options

• Network Setup - The “Network Setup” function allows the user to connect the Synergy software to a PETwave® or

Explorer™. To connect a unit, the user must select “Network Setup” from the “Options” drop-down menu.

• Manage Users - The “Manage Users” function is only available to users with Administrator access to the Synergy

software. Anyone with an Administrator account can add, alter, and delete other users’ accounts. It is advised to

reserve Administrator accounts to a select few users. To manage user accounts, select “Manage Users” from

the “Options” drop-down menu.

• Convert ChemDriver Database - The PETwave does not utilize this feature.

• Open Vessel - The PETwave does not utilize this feature

• Temperature - The PETwave does not utilize this feature.

• Preferences - The “Preferences” function allows the user to alter their personal settings within the Synergy

software. To adjust their preferences, the user must select “Preferences” from the “Options” drop-down menu.

To save their adjustments after the program is closed, the user must check “Save As Defaults” at the bottom of

the dialogue box before clicking “OK” or “Apply”.

Help

• Contents - Allows the user to view the help topics of the Synergy software.

• About - The “About” function allows the user to view the current version of Synergy software, PETwave Firmware

and serial number.

14 / Synergy software connection (optional)

Synergy Software Connection (Optional)

Download Synergy Software

1. Access the CEM website www.cem.com.

2. Select “PETwave” from the “Products” menu.

3. Select “Resource Library.” Scroll to the “Software” section. The current version of Synergy will be available for

download.

4. Log-in or create a CEM user account.

NOTE

If the serial number cannot be located, contact the CEM Corporation Synthesis Department

800-726-3331 or 704-821-7015.

5. Download the Synergy software onto a USB memory stick.

6. Locate a computer designated for the PETwave and place near Microwave Controller. The Synergy Software

requires a computer with Windows XP, Windows 7, Windows 8, Windows 8.1 or Windows 10. Minimum system

requirements are a Pentium 4 class processor running at 2.80 GHz with 1G of RAM and at least 40GB of avail-

able disk space.

7. Turn the computer on.

8. If any applications or dialogue boxes are open, close them.

9. Install the USB memory stick containing the Synergy software and open the Synergy folder.

10. Follow the instructions displayed on the computer screen for installation. A short cut will be automatically cre-

ated with the Synergy icon and placed on the computer desktop when installation is complete.

IP Address

The computer and Synergy software require a Fixed IP address for operation.

Computer

1. Connect an Ethernet cable from the PETwave system to the computer.

2. Turn the PETwave (Microwave Controller) on.

3. Enter the “Local Area Connection Properties screen.” Follow either “Windows XP” or “Windows 7” for IP ad-

dress setup.

Windows XP

3.1. From the computer’s desktop, select “Start” (located in the lower left corner of the screen).

3.2. Select “Control Panel.”

3.3. If using the “Classic View,” select “Network Connections.” If using the “Category view,” select

“Network and Internet Connections” and then select “Network Connections.” The following screen

will appear.

Synergy software connection (optional) / 15

3.4. Select “Local Area Connection.” The following screen will appear.

Windows 7, Windows 8, Windows 8.1 and Windows 10

3.1. From the computer’s desktop, select “Start” (located in the lower left hand corner of the screen).

3.2. Select “Control Panel.”

3.3. If using “Category View,” select “View network status and tasks” within the “Network and Internet”

section. If using “large icons” or “small icons” view, select “Network and Sharing Center.” The

following screen will appear.

16 / Synergy software connection (optional)

3.4. Select “Change adapter settings” located in the upper left corner of the window. The following

screen will appear.

3.5. Select “Local Area Connection.

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CEM PETwave Operating instructions

CEM PETwave Operating instructions

CEM PETwave Operating instructions

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