MARS 6 Synthes is - CEM...

MARS 6 Synthesis™ Open Vessel Option 601155 • Revision 2 • March 2016

MARS 6 Synthesis

Open Vessel Option

Corporation

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Contents Safety Information 2

Safety Notations 2

Operation Precautions 2

Fume Ventilation 2

Contacting CEM 2

Open Vessel Option Overview 3

Synthesis Features 4

Standard Temperature Control System 4

Optional Internal Printer 4

Turntable Drive System 4

Exhaust Blower 4

Optional Sample Stirrer 4

Overhead Stirring Integration 4

Optional Inlet/Outlet Ports 5

Fiber Optic Operation 6

Temperature Setup 6

Verify Fiber Optic Temperature 7

Create a Method 8

Run and Open Vessel Reaction 12

System Specifications 13

Warranty Information 14

Copyright 2016 by CEM Corporation

All Rights Reserved

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

MARS 6 Synthesis™ is a trademark of CEM Corporation

Teflon® is a registered trademark of DuPont.

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Safety Information

Safety Notations

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

personnel hazards, equipment dangers or important information. 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 of 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 which, if not strictly followed, may result in improper instrument operation.

WARNING A WARNING is intended to emphasize dangerous or hazardous conditions which may result in personal injury to the user

and/or damage or destruction of the instrument.

Operation Precautions

The MARS 6 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 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. It is suggested by the manufacturer 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. Leakage measured above the legal limit of 5 mW/cm2 should be reported to the CEM Service Department. Cardiac pacemakers require magnets to control their operation during checkout. If the instrument is equipped with an optional magnetic sample stirrer which contains very high static magnetic fields, some danger exists if a pacemaker is positioned in close proximity of the instrument cavity (such as placing the head into the instrument cavity to perform a visual inspection). 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.

Fume Ventilation

The MARS 6 Synthesis™ instrument operates as either an open or semi-closed system with venting of any hazardous solvent fumes through the elephant trunk vent hose coming from the back of the instrument. Before beginning operation, the rear vent line must be vented into a proper chemical fume hood or exhaust line no farther than six feet

(6’)/two meters (2 m) from the instrument.

Contacting CEM CEM provides technical and applications support for the MARS 6 Synthesis option. For applications support, call (800)

726-3331 (inside the US) or (704) 821-7015 and ask for “MARS 6 Synthesis Applications,” or email CEM Synthesis

applications at [email protected]. For technical support questions, call (800) 726-5551 (inside the US) or

(704) 821-7015 and ask for CEM Service or email [email protected].

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Open Vessel Option Overview (P/N 925626) The Microwave Accelerated Reaction System, Model MARS 6, is designed for laboratory use in digestion, extraction, and synthesis.

The multiple mode cavity enables the parallel processing of multiple samples in a single run or large batch reactions. The large format of the cavity also allows the user to perform larger scale reactions than those possible with a smaller, single mode system, either in a single batch format or when run in parallel. 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 (P/N 925626 for 230 V and P/N 925628 for 240 V) includes an I/O Port located in the top center of the microwave cavity. This opening permits the attachment of a reflux condenser to the reaction vessel inside the microwave cavity. Any type of round bottom flask may be used with the system with volumes ranging from 250 mL to 5L. The Open Vessel Accessory kit (P/N 907545) includes:

11.5-inch connector adaptor with 24/40 ground glass joint (P/N 135030)

14.75-inch connector adaptor with 24/40 ground glass joint (P/N 135035)

3-liter round-bottom flask with a 40/35 ground glass joint neck (P/N 322045)

5-liter round-bottom flask with a 40/35 ground glass joint neck (P/N 322040)

Ground glass joint reducing adaptor 40/35-24/40 (P/N 135020)

Single neck temperature probe adaptor (P/N 135025)

Double neck temperature probe adaptor to allow for overhead stirring (P/N 135040)

Temperature probe plug adapter (P/N 325216)

Two (2) oval rare earth stir bars 40 x 20 mm (P/N 151060)



All manuals and instruction booklets accompanying vessel sets and instruments should be read and understood prior to

performing microwave reactions.

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Synthesis Features Standard Temperature Control System The standard temperature control system for MARS 6 Synthesis™ Option is the RTP-300 Plus (Resonance Temperature Probe) which monitors and controls temperature conditions inside sample vessels. A microwave transparent fiber optic probe (P/N 314307) is connected to the bayonet connector located to the right of the I/O port on the top outside cover of the MARS 6™. The fiber optic probe is then inserted into the reaction vessel through the small side arm of the single neck temperature probe adaptor. The temperature probe adaptor fits into the glassware extension extruding from the top of the I/O port. A reflux condenser can then be placed into the top joint of the single neck temperature probe adaptor. A feedback signal from the RTP-300 Plus probe to the magnetron of the system regulates microwave power output to maintain the selected temperature parameter. When using sealed vessels, the fiber optic probe is inserted into the vessel via thermowell.

Optional Internal Printer The optional internal thermal printer permits printing of method parameters, graphs and/or method data at any time that the “print” icon is displayed on the screen during method performance or when viewing method information and previous method performance data.

Turntable Drive System The MARS 6 is furnished with an alternating and/or continuous turntable drive system. Rotational configuration is automatically selected by the vessel choice. During sample heating in alternating style, the turntable rotates 355º, then reverses direction to prevent pressure sensing or fiber optic temperature sensors from becoming entangled and damaged. The turntable always operates when the microwave power is on. The turntable stops rotating when the microwave sample preparation cooling cycle ends, when “Stop” is selected, or when the instrument door is opened.

Exhaust Blower The MARS 6 is equipped with an exhaust blower to remove cor4rosive or harmful fumes and flammable vapors from the cavity. The blower moves air at the rate of 3.6 m3/minute (125 ft/minute).

Optional Sample Stirrer The optional sample stirrer is a rotating magnetic field in the bottom of the instrument which works in conjunction with stirring bars placed in the vessel liners to ensure a homogeneous sample.

Overhead Stirring Integration When viscous materials or samples with high solids content need to be stirred, and the sample stirrer along with a stirring bar do not provide adequate stirring, overhead stirring can be used. When using overhead stirring, a double neck temperature probe adaptor must be used. The stir shaft is inserted through the straight section of the adaptor into the reaction vessel, and the adaptor is fitted to the extension extruding through the I/O port. A reflux condenser is attached to the curved section of the adaptor, and the fiber optic probe is inserted through the smaller side arm. Due to different sizes of stirring paddles or blades, the stir shaft may need to be inserted into the reaction flask prior to placing the extension glassware and double neck temperature probe adaptor into place. The stir shaft and paddle must be composed of a non-metallic material, such as glass or Teflon®.

WARNING Because cardiac pacemakers require magnets to control operation during checkout, if the MLARS 6 instrument is equipped with an optional 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.

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Optional Inlet/Outlet Ports Two inlet/outlet ports, located on the right side of the instrument, permit access to the interior of the cavity for optional pressure and temperature control.

CAUTION

When using overhead stirring, the fiber optic probe must be inserted into the reaction material, but away from the stirring paddle or blades. Failure to do so can cause the fiber optic probe to break.

WARNING Never insert metallic objects such as wire into the inlet/outlet ports nor modify the ports. Serious microwave leakage and/or electrical shock may result. The inlet/outlet ports of the MARS 6 are electrically grounded to the

microwave cavity and are designed to prevent leakage of microwave energy.

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Fiber Optic Operation

Temperature Setup

1. Select the icon located in the lower right corner of the Home screen.

2. Select “Settings”.

3. Select “Sensors”.

4. Select “GF Number”. A keyboard will appear on the screen. 5. Using the Keyboard, enter the GF Number of the Fiber Optic Probe installed in the instrument.

6. Once the number is properly entered, select “hide” to close the keyboard.

7. Save the GF number by selecting the icon located at the top right corner of the screen to save the value that was entered. Once the GF number has saved the icon will turn gray.

8. Press the key in the lower left corner of the screen to return to the Home page.

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Verify Fiber Optic Temperature

1. Select the key located in the lower right corner of the Home screen.

2. Select “Tools”. The “FISO Temperature” will be displayed.

NOTE If “---” appears as the temperature, then the MARS 6 does not recognize the Fiber Optic Probe. The probe is either not installed or has been broken.

3. The probe can be inserted into a beaker of warm water for temperature verification.

4. Press the key in the lower left corner of the screen to return to the Home page.

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Create a Method Creation of a method for use in the MARS 6 requires knowledge and selection of the method control type. This section outlines method development for a round-bottom flask reaction.

NOTE Throughout the text of this manual, the word “select” is used to indicate “touch”.

1. From the MARS 6 home screen, select “Classic Methods”.

2. To create a method, select “+” at the top of the screen.

3. Select “Name” to name the method being created. The keypad will appear on the screen.

4. Using the keypad, select the name of the method being created.

NOTE To toggle between upper and lower case letters for the method name, touch the “shift” key on the keypad. To toggle to the numbers and symbols for the method name, select “alt” on the bottom of the keypad. Use the backspace “del” (delete) key to delete unwanted letters and/or numbers. Use the space bar to enter a space in the method name.

5. Once the name is properly entered, select “Hide” to close the keypad.

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6. Touch “Select Control Type” to select the desired control type for the method (Ramp to Temperature, Ramp to Pressure, Standard, or Power Time).

7. Select and highlight the desired control type.

NOTE: “Ramp to Temperature” is the most commonly used control type.

8. Select “OK.”

9. Select “Vessel Type” to select the desired vessel to be used with the method.

10. Scroll through the list until “Beaker” is displayed.

NOTE: Beaker is only selected for the open vessel setup. If using a vessel set, select the appropriate vessel type.

11. Select “Beaker”.

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12. Select “OK.”

13. Select the scroll bar on “Temp Guard” and set to “Off”.

14. Select “Add/Edit Stages->” in the lower right corner of the screen. A new screen will appear.

15. Select “+” to add a stage to the method.

16. Based on the control type selected, enter method parameters as follows: a. Touch the “down” arrow key to scroll and select the desired ramp time (0-59 minutes). b. Touch the “down” arrow key to scroll and select the desired hold time (0-59 minutes).

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c. Touch the “down” arrow key to scroll and select the desired Temperature (0-300oC in increments of 1). d. Touch the “down” arrow key to scroll and select the desired Pressure (0-300oC in increments of 1). e. Touch the “down” arrow key to scroll and select the desired Power (0-1800 watts in increments of 10). f. Toggle the stirring option to the desired setting (on or off).

17. Once all parameters are properly selected, select the icon to save the entered data. Once the method has saved, the disk icon will become gray and the method name will be added to the top left corner of the screen.

NOTE

To add additional stages, repeat steps 15 & 16. To delete a stage, select the stage to delete and then select the “X” on the screen. To edit the method parameters, highlight the stage and select “Edit Method”.

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Run an Open Vessel Reaction

Items Required: Round bottom flask (250mL or larger)

Stir bar appropriate to flask size

Teflon Vessel Stand

Prepare the Vial 1. Place all reagents into a round-bottom flask with a stir bar. 2. Ensure the cavity is clean. 3. Place the Teflon® stand over the turntable drive lug, in the center of the cavity. 4. Place the round bottom flask with the reaction on to the vessel stand in the

cavity. 5. Attach extension glassware and a condenser, if necessary. 6. Insert the fiber optic probe in to the round bottom flask.

If the adapter with the temperature probe port is being used, insert the probe through the I/O port.

If the reflux condenser without the temperature probe port is being used, feed the probe through the top of the condenser down in to the round bottom.

NOTE

Do not program temperature any higher than the boiling point of the lowest boiling solvent being utilized.

Microwave Irradiation 1. Load or create the appropriate method into the instrument. See section “Create Method” for creating a

method.

2. Press the key. Once the method begins the system will ramp to the set-point. The system will maintain the programmed parameters to perform the complete method.

NOTE: If desired, during the method the user can alternate between the thumbnails located on the left side of the screen.

Removing the Vessel 1. Upon completion of the reaction, wait until the temperature setpoint has been obtained and the cool-down

cycle has terminated. 2. Open the door of the MARS 6 Instrument. 3. Remove the fiber optic probe. 4. If applicable, remove the condenser. 5. Remove the round bottom flask.

6. Remove the vessel stand from the cavity.

Maximum Working Volume: 70% of

reaction vial

Minimum Working Volume: 50mL

Maximum Control Temperature: 300 °C

General guidelines for 100% power:

50mL-500 mL: 500 W

500mL-1.5L: 1000 W

1.5L-3.5L : 1800 W

Total Minimum Load: (Total volume of

solvent in the MARS 6 cavity)

50 mL with low and medium absorbing

solvents

WARNING

To prevent the possibility of severe burns, ensure that insulated gloves and protective gear as outlined in the user’s safety program are worn.

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System Specifications

Overall Instrument Dimensions

63.5 cm (25 in.) height x 53.3 cm (21 in.) width X 63.5 cm (25 in.) depth

Weight 63.6 kg (140 lbs.)

Touchscreen 7” (800 x 480) TFT-LED glass capacitive touchscreen display

Ports 5 USB, 1 USB-B, 2 Ethernet, 1 RS-232

Languages Software available in English, German, French, Italian, Spanish, Chinese, and Japanese

Turntable Design PerfectCircle™ design provides absolute radial symmetry. Turntable operates in alternating or continuous mode.

Microwave Cavity Heavy-duty 316 solid steel cavity with multi-layer Teflon® coating

Electrical Requirements 200/208/230 VAC (200-253 VAC), 60 Hz, 15A @ 230 VAC 220/240 VAC (202-250 VAC), 50 Hz, 15A @ 240 VAC

Magnetron Frequency 2455 MHz

Power Output 1800 W – Continuous power available at all power levels to provide more control for reactions

Magnetron Protection Solid-state isolator (US patent 4,835,354) to protect magnetron from reflected energy, ensuring constant power output

Speakers 8 Ω, 2 W, 86 dB

Printer Onboard thermal printer and USB-B compatible printer port

Safety Features Three independent door safety interlocks, including an interlock monitoring system plus three independent thermal switches, are used in each instrument to prevent instrument operation and microwave emissions in case of improper door closure or misalignment. The instrument complies with HHS standards under 21 CFR, Part 1030.10, Subparts (C)(1), (C)(2) and (C)(3). Reactiguard continuously monitors the cavity and disables the magnetron if disturbances occur inside the cavity.

Emissions and Safety Approvals

Conforms to Globally Harmonized EN61010-1 Standard for Safety Requirements for Electric Equipment for Measurement, Control, and Laboratory Use Part 1: General Requirements (CAN/CSA-C22.2 No. 1010.1-1992).

Patents CEM microwave systems and vessel designs may be covered by any one of the following US patents: 5,443,795 5,620,659 6,281,484 6,307,190 6,373,040 6,084,226 6,288,379 5,988,877 8,480,981 6,136,276 6,287,526 6,863,871 7,144,739 7,829,040

Other patents pending

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Warranty Information

What Is Covered: CEM Corporation warrants that the instrument will be free of any defect in parts or workmanship and will, at its option, replace or repair any defective part (excluding consumables) or instrument.

For How Long: This warranty remains in effect for 365 days from date of delivery to the original purchaser.

What Is Not Covered: This warranty does not cover parts or workmanship damaged due to:

Neglect, abuse, misuse or theft,

Damage caused by or to test samples,

Damage incurred during instrument relocation,

Damage caused by or to any attached equipment,

Use of incorrect line voltages or fuses,

Fire, flood, "acts of God" or other contingencies beyond the control of CEM Corporation,

Improper or unauthorized repair, or

Any other damage caused by purchaser or its agents.

Responsibilities of Purchaser: To ensure warranty coverage, the purchaser must:

Use the instrument according to directions,

Connect the instrument properly to a power supply of proper voltage,

Replace blown fuses,

Replace consumables and

Clean the instrument as required.

How to Get Service: Purchaser should contact the Service Department of CEM Corporation or the nearest CEM subsidiary or distributor for return authorization and for proper crating and shipping instructions to return instrument, freight prepaid, for service. On-site repairs by an authorized service technician are available through the CEM Service Department. Travel costs will be charged to the purchaser for onsite repairs.

Within the U.S. Outside the U.S. CEM Corporation CEM Corporation 3100 Smith Farm Rd. 3100 Smith Farm Rd. Matthews, NC 28105-5044 Matthews, NC 28105-5044 (800) 726-5551 (704) 821-7015 Fax: (704) 821-4368 Fax: (704) 821-4368

Warranty Disclaimer: CEM Corporation hereby excludes and disclaims any warranty of merchantability or fitness for any particular purpose. No warranty, express or implied, extends beyond the face hereof. CEM Corporation shall not be liable for loss of use of instrument or other incidental or consequential costs, expenses or damages incurred by the purchaser or any other user. This warranty is not transferable.

Purchaser's Rights under State Law: This warranty gives the purchaser specific legal rights, and the purchaser may also have other rights that vary from state to state.

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