CEM Mars 6 Owner's manual

MARS 6 Synthesis

Parallel & Scale-Up Microwave Synthesizer

Manual

THIS PAGE INTENTIONALLY LEFT BLANK

Contents

Safety

Safety Notations 1

Introduction

About the Instrument 2

Important Safeguards

Solvent Chart 3

Microwave Safeguards 3

Instrument Safeguards 4

Instrument Overview

Front and Side View 5

Back and Side View 6

Cavity 7

Software Overview

Software Icons 8

Home Screen 9

Methods Screen (One Touch and Classic) 9

System Menu 10

System Installation

Unboxing 13

System Setup 15

Vessels

GlassChem 20 19

EasyPrep & EasyPrep Plus 19

Open Vessel/Beaker 19

Methods

Create a Classic Method 20

Create a One Touch Method 22

Edit Method 22

Delete Method 22

Export Method 23

Import Method 24

Users

Edit/Delete User 26

Auto Login 26

Password Conguration 27

Data Management

View, Print, and Export Data 28

Activity Log 29

Calibrations

Fiber Optic Probe 30

Pressure Control 30

Temperature Verication (IR Sensors) 30

Temperature Calibration (IR Sensors) 31

Pressure Calibration 32

Power Test

Power Test 33

Printer (Optional)

Internal Printer 34

Fiber Optic Temperature Control

Fiber Optic Installation 35

Fiber Optic Temperature Verication 36

Fiber Optic Care 37

Software Update

How to Update Software 38

Routine Maintenance

After Every use 39

Daily 39

Weekly 39

Annually 39

As Needed 39

Troubleshooting

Problems and Possible Solutions 40

System Specifications

Location Requirements 41

Electrical Requirements 41

Environmental Requirements 41

Warranty

Limited Warranty Information 42

Appendix A: GlassChem 20 Vessels

Vessel Components 44

Operating Parameters 45

New Cap and Vent Plug Conditioning 46

Perform a Reaction 47

Vessel Cleaning 53

Appendix B: EasyPrep and EasyPrep Plus Vessels

Vessel Components 54

Operating Parameters 55

New Liner and Cover Conditioning 55

Perform a Reaction 56

Vessel Cleaning 65

Appendix C: Open Vessel Reactions

Vessel Components 67

Operating Parameters 67

Perform a Reaction 68

Glossary

Glossary 71

Technical Assistance

Applications Support 72

Technical Support 72

Contact Information

CEM Corporation Headquarters 73

CEM International Subsidiaries 73

CEM Distributors 74

1

Safety

Safety Notations

This manual uses three safety alert words at points in the documentation where the user should be aware of

potential hazards. The safety alerts are shown in color-coded boxes. The three words – NOTE, CAUTION, and

WARNING – indicate differing levels of observation or action as described below:

NOTE

A NOTE is intended to provide emphasis on procedures that may be misinterpreted or overlooked, or to

clarify confusing situations.

CAUTION

A CAUTION is intended to provide essential information and to emphasize procedures that, if not strictly

followed, may result in improper instrument operation.

WARNING

A WARNING is intended to emphasize dangerous or hazardous conditions that may result in personal

injury to the user and/or damage or destruction of the instrument.

2Introduction

Introduction

About the Instrument

The MARS™ 6 Synthesis is a multi-mode microwave system that provides parallel reaction processing, under

uniform conditions. The power output on this particular system is programmable up to 1800 watts and uses an

advanced feedback system to monitor and control the rate of heating of the sample(s) in the cavity. The MARS 6

Synthesis Open Vessel Option includes an I/O Port located in the top center of the microwave cavity. This opening

permits the attachment of a reux condenser to the reaction vessel inside the microwave cavity. Any type of round

bottom ask may be used with the system with volumes ranging from 250 mL to 5 L. The sample stirrer is a

rotating magnetic eld in the bottom of the instrument which works in conjunction with stirring bars placed in the

vessel liners to ensure a homogeneous sample.

The MARS 6 Synthesis is designed to be operated in accordance with the guidelines outlined in this manual.

The GlassChem, EasyPrep™, and EasyPrep Plus™ are the only approved sealed vessels designed for synthetic

pressurized reactions performed in this system. Conventional laboratory glassware can only be used for microwave

reactions at atmospheric pressure.

This manual refers to MARS 6 software version 1.50 for all software information, including screenshots and

technical information.

This manual contains proprietary information which shall not be reproduced or transferred to other documents or

disclosed to others without prior written permission from CEM Corporation.

Read and fully understand all documentation before operating the instrument.

3

Important Safeguards

General guidelines for safe operation of the MARS 6 Synthesis system are presented below and all specic safety

messages are located throughout the manual.

Proper precautions must be taken to avoid contact with reagents or reagent vapors. Protective gear should be worn

as outlined in the user’s safety program for hazardous materials and the reagent manufacturer’s safety data sheet.

Refer to these guidelines for proper handling and disposal of the reagents. Dispose of all waste in accordance with

all applicable local, state, and federal health and safety recommendations.

Solvent Chart

The below chart provides some representative examples of microwave absorptive properties for a variety of

common synthetic solvents. For solvents not included in this chart, contact your CEM representative.

Microwave Absorbency Solvent

High DMSO, EtOH, MeOH, Propanols, Nitrobenzene, Formic Acid, Ethylene Glycol

Medium Water, DMF, NMP, Butanols, Acetonitrile, HMPA, Methyl Ethyl Ketone, Acetone and other ketones,

o-Dicholorbenzene, 1,2-Dichloroethane, 2-Methoxyethanol, Acetic Acid, Triuoroacetic Acid

Low Chloroform, Dichloromethane, Carbon Tetrachloride, 1,4-Dioxane, THF, Glyme, and other ethers, Ethyl

Acetate, Pyridine, Triethylamine, Toluene, Benzene, Chlorobenzene, Xylenes, Pentane, Hexane and other

hydrocarbons

Minimum Cavity Load

A minimum cavity load must be met before running a microwave method. The minimum cavity load is determined

by the solvent, number of vessels, and vessel type: GlassChem 20, EasyPrep, EasyPrep Plus, and Open Vessel.

Microwave Absorbency GlassChem 20 EasyPrep Plus Open Vessel

Low 50 mL 50 mL 100 mL

Medium 50 mL 50 mL 100 mL

High 10 mL 20 mL 100 mL

Microwave Safeguards

• Never heat liquids in a sealed vessel or container that is not equipped with a pressure relief device.

• Cover all solids in the reaction vessel with liquid

• Metal catalysts can be used, but ensure they are wetted or in solution

• Finely divided (powder) metals are safer than bulk metals for heterogeneous catalysis

• Solid state reactions should not be performed in a Mars 6

• Never exceed the maximum working volume of the vessel

• Always use a stir bar that adequately mixes the reaction contents in the microwave

• When transitioning a conventional, open vessel reaction to a closed vessel reaction, Increase reaction

temperature 25 °C above the highest boiling point solvent in vessel

• Always use the Ramp-to-Temperature control type and allow for sufcient time to heat to temperature, especially

for low absorbing solvents. This will help prolong the life of the magnetron and microwave unit.

• Start with the recommended power based on the number and type of vessels used

• Always prepare the Control (vessel with ber optic probe) the same as the Standard vessels

• The Control vessel must contain the same solvent and reagents as used in the Standard vessels

• Always distribute multiple vessels evenly around the turntable

4Important Safeguards

Instrument Safeguards

• Service can only be performed by an authorized CEM service technician. This instrument utilizes high voltages

and microwave radiation.

• DO NOT tamper with the instrument.

• DO NOT install the MARS 6 instrument inside of a fume hood. The exhaust hose must be connected and draw at

least 125 CFM at the point of connection at all times as it is essential for removing harmful gases away from the

instrument. Vapors should be vented into a fume hood by means of the exhaust hose only.

• If any damage to the instrument is noted, do not attempt instrument operation.

• Use only CEM specied consumables and accessories.

• If installed, remove the ESP-1500 Plus cable connection and clean as outlined in this manual.

• Clean the temperature sensors as outlined in this manual.

5

Instrument Overview

Front and Side View

1

2

3

4

5

6

7

8

9

Item Description

1 Touch Screen Display Shows menus, method parameters, etc. Includes 86 dB speakers

2 Door Handle Permits ease of opening instrument door

3 RTP-300 Connector Connects Fiber Optic probe

4 I/O Port Access to install condenser for open vessel reactions

5 Internal Printer (optional) Permits printing of method parameters, graphs and/or method data

6 High Voltage Cooling Fan Draws room air past the magnetron

7Communication Access Permits access to USB, Ethernet, and RS232 ports

8 Fuses Prevent electrical power overload

9 Power Switch Turns AC power on and off to the instrument

6Instrument Overview

Back and Side View

1

2

3

4

5

6

Item Description

1 Power Cord Receptacle Receives the female end of the power cord

2 Cavity Exhaust Outlet Exhausts fumes from the microwave cavity

3 Cavity Exhaust Blower Directs air from the microwave cavity to the exhaust outlet at the rate of 3.6 m3/minute (125

ft3/minute)

4 External Sensor Port Permits interface of optional instrument features

5 High Voltage Cooling Fan Draws room air past the magnetron

6 Nameplate Lists model, serial number, operating voltage, frequency, and current draw

7

Instrument Overview

Cavity

Fluoropolymer-coated microwave cavity.

1

2

3

4

5

Item Description

1 Door Seal Ensures tight t between door and interior cavity of the MARS 6 to prevent microwave

leakage

2 Waveguide Covers Evenly distribute microwaves into instrument cavity

3 Turntable Drive Lug Allows the turntable drive shaft to pass through the cavity oor and engage the

Turntable

4 Floor Mat Protects the Teon Coating on the Floor of the Mars 6 Cavity

5 Door Lock 3 door safety interlocks and an interlock monitoring system to prevent microwave emission

when the door is open

* IR Sensors (optional) Measures temperature using Infrared Sensors

* Pressure Port connector

(optional)

Provides pressure control utilizing an internal Electronic Sensor for Pressure (ESP)

* Turntable Sensor Detects type of turntable

* Vessel Counting Sensor Counts number of vessels in the turntable

* Not visible in photo.

8Software Overview

Software Overview

Software Icons

Icon Description Icon Description Icon Description

Add Stage Filter Remove Stage

Back Home Run

Blower Import Save

Delete Information System Menu

Done Infrared System Settings

DuoTemp™New Temperature

Edit Power Turntable

Export Pressure

Fiber Optic Print

9

Software Overview

Home Screen

The Home screen is the rst screen that appears when the system is turned on. Three areas are accessible from

this screen: One Touch® Methods, Classic Methods, and System Menu.

• One Touch Methods are methods created and optimized by CEM for digestion applications. These methods

should NOT be used for synthetic chemistry applications

• Classic Methods are created by the user and can be edited at any time. These methods are intended for MARS 6

Synthesis users. Classic can be imported from another instrument.

• The System Menu icon provides access to any functionality that does not directly involve creating or running a

method.

Methods Screen (One Touch and Classic)

After choosing either the One Touch Methods (left) or Classic Methods (right), the method library will appear.

NOTE

A blue avatar will appear for user-created methods.

10 Software Overview

System Menu

The following is a basic review of each section of the System Menu to be used as a quick guide for locating

software items and instrument functions.

• Tools: Calibration and Diagnostic tools to ensure proper system functionality and software update when a new

version is released

• Settings: Adjustable system settings necessary prior to running samples, system information including serial

number, software version, contact information, etc., and users

• Video: Visual display to ensure proper system handling and usage

• Logout: Protects the current user’s access or prevent unauthorized actions on the current login session

Tools

• System: Views hardware stats

• Diagnostics: A listing of real-time readings directly related to unit functionality and the option to manually

maneuver commonly used hardware

• Power: Allows user to verify power output

• IR: Temperature sensor calibration

• Pressure: Zeros false pressure

• Turntable: Allows user to determine alignment

• Activity Log: Audit trail for tracking user movement within software, including system and method editing

• Update Manager: Used for updating software when a new version is released

11

Software Overview

Settings

• General: Views system information, service records and CEM information

• System: Instrument settings for the audio and visual selections for the individual user

• Localization: Regional adjustments, including language and the preferred date and time format

• Date/Time: Location for setting the correct date and time

• Users: Manage users and passwords and log-in preferences

• Run: Adjustments to settings specic to each sample run including: data output, vessel cool down, and turntable

positioning

• Method: Parameter increments for method programming

• Sensors: Calibrations and readings for sensors and exhaust sensor selection

• Printing: Install and view printer

• Networking: Connect instrument to network

Video

• Videos to help with system operation

12 Software Overview

Logout

• Displays the Logout screen

13

System Installation

Unboxing

1. View the Site Preparation Guide (P/N FM0050) and select a location that meets requirements before installing

the MARS 6 Synthesis instrument.

2. Carefully inspect the shipping carton, the instrument and accessories for any damage that may have occurred

during shipping. If the instrument or accessories have damage, contact the freight carrier to report the damage

and le a damage report. Contact your CEM representative to request service information.

WARNING

If any damage to the instrument is noted, do not attempt instrument operation.

3. Pull plastic tab, swing handle open and remove the plastic assembly from box. Repeat process on the remain-

ing handles.

4. Use top handles to pull up and remove outer box.

5. Carefully cut the tape on both sides of the inner box.

14 System Installation

6. Lay the sides of the box at and remove the foam from the top of the system.

7. Lift the system, from the sides, onto bench top near exhaust service (two people required). Do not place the

system in a fume hood.

8. Remove the plastic and discard. Do not leave the plastic under the system.

15

System Installation

remove plastic & lifting

device before using

9. Remove the box from inside of the system cavity. Write down the serial number located on the nameplate on

the back left side of the system.

10. Retain all packing material for use if returning the instrument to the manufacturer for service.

System Setup

1. Connect the exhaust hose to back of the system.

2. Connect the opposite end of the exhaust hose to a fume hood that pulls a minimum of 125 CFM at point of

connection.

3. Plug power cord into the system and a dedicated, grounded outlet. The instrument is supplied with a power

cord, but an adequately rated power cord may be used.

16 System Installation

4. Position the instrument so the door is facing forward and so there is open space to access the power switch.

5. Locate the power switch on the right side of the instrument, and position it in the ON position.

6. When the system is rst powered on during the install, a “Line Voltage” message will appear.

7. Determine the line voltage from outlet:

• 60 Hz, 208 V or 230 V

• 50 Hz, 200 V, 220 V, or 240 V

8. Set the line voltage.

8.1. Select the System Menu icon in the bottom right corner of the screen.

8.2. Select Settings.

8.3. Select System.

Page is loading ...

CEM Mars 6 Owner's manual

This manual is also suitable for

CEM Mars 6 Owner's manual

Related papers

Other documents