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OptiMax 1001
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Mettler Toledo OptiMax 1001 Operating Instructions Manual

OptiMax™ 1001
Synthesis Workstation
Operating Instructions
Content
Content
2 Safety Measures ................................................................................................... 7
2.1 Measures for your protection ................................................................................. 7
2.2 Measures for Operational Safety ........................................................................... 8
3 Installation .......................................................................................................... 11
3.1 Location of the OptiMax™ 1001 .......................................................................... 11
3.2 Connections ......................................................................................................... 11
3.2.2 The Relay for visual or acoustical signalization ................................................... 13
3.2.3 Connecting a Coolant ......................................................................................... 14
3.4 Installing the 1000 mL Two-Piece Reactor .......................................................... 19
3.4.3 Installing Accessories ..........................................................................................22
3.5.1 Installing the Receptacle for the 500 mL Reactors ..............................................26
3.5.2 Openings of the 500 mL Two-Piece Reactor Cover ............................................. 26
3.6 Installing the 250 mL Two-Piece Reactor
3.6.1 Installing the Receptacle for the 250 mL Reactors ..............................................28
3.6.2 Openings of the 250 mL Two-Piece Reactor Cover ............................................. 28
3.7 Installing the 1000 mL One-Piece Reactor ..........................................................29
3.7.2 Openings of the 1000 mL One-Piece Reactor ..................................................... 30
3.8 Installing the 500 mL One-Piece Reactor ............................................................31
3.8.2 Openings of the 500 mL One-Piece Reactor ....................................................... 32
3.9 Installing the 250 mL One-Piece Reactor ............................................................33
3.9.2 Openings of the 250 mL One-Piece Reactor ....................................................... 34
3.10 InstallingtheBafe ............................................................................................... 35
............................................................. 27
METTLER TOLEDO OptiMax
TM
1001 3
Content
4 Design and Operating Principles ..................................................................... 36
5 Temperature Control Modes ............................................................................. 37
5.1 Tj Mode ................................................................................................................ 37
5.2 Tr Mode ................................................................................................................ 37
5.3 Distillation Mode (Tj-Tr) ........................................................................................ 37
5.4 Crystallization Mode (Tr-Tj) .................................................................................. 38
6 Using additional instruments together with the OptiMax
1001 .................... 39
7 Safety System of the OptiMax™ 1001 .............................................................. 40
7.2 Measures for Intrinsic Safety ............................................................................... 40
7.3 Temperature Monitoring ....................................................................................... 41
7.4 Emergency Programs of the OptiMax™ 1001 ..................................................... 41
7.4.2 Emergency Program E ......................................................................................... 42
8 Maintenance and Servicing of the OptiMax
1001 .......................................... 43
8.3 Changing the Coolant .......................................................................................... 43
8.6 Disposing of the Instrument ................................................................................. 45
9 Malfunctions of the OptiMax™ 1001 ................................................................ 46
9.3 Heating ................................................................................................................. 46
10 Technical data .................................................................................................... 47
4 METTLER TOLEDO OptiMax
TM
1001
Content
METTLER TOLEDO OptiMax
TM
1001 5
Introduction

1 Introduction

The METTLER TOLEDO OptiMaxTM 1001 is a reactor system for performing synthesis with a 250-mL,
a 500-mL, or a 1000-mL glass reactor. The instrument is operated via the integrated touchscreen.
• The reactor can be heated or cooled and its content stirred and reuxed.
• The temperature of the reactor content can be measured using a Pt100 sensor.
• The integrated pH measurement system equipped with the appropriate electrode allows you to
measure the pH value of the reactor content.
• You can export the acquired data to another program for further processing using the USB Memory
Stick supplied.
We, Mettler-Toledo AG, accept no liability whatsoever if you do not observe the following rules
and measures for safe operation of the OptiMax™ 1001 with the glass reactor!
6 METTLER TOLEDO OptiMax
TM
1001
Safety Measures

2 Safety Measures

The OptiMax™ 1001 has been tested for the experiments and intended purposes documented in these Operating Instructions. However, this does not absolve you from the responsibility of perform­ing your own tests of the product supplied by us regarding its suitability for the methods and purposes you intend to use it for. You should therefore observe the following safety measures.
Please comply with all safety and accident-prevention regulations, as in force for laboratory work!

2.1 Measures for your protection

Grounding of the power supply outlet
– Make sure you plug the power cable supplied into a power supply outlet that is
grounded! A technical fault could otherwise result in death or serious injury.
Risk of an elec-
trical shock
Risk of explosion
Risk of explosion
Risk of explosion
Risk of explosion
Power failure
– Implement appropriate measures like an uninterruptible power systems (UPS)
against possibly fatal consequences of a power failure!
Potentially explosive environment
– Never work in an environment subject to explosion hazards! The OptiMax
TM
1001 housing is not gas tight (explosion hazard due to spark formation, corro­sion caused by ingress of gases).
Critical reactions
– Always perform a safety analysis before starting investigations with a high haz-
ard potential, for example by a Differential Scanning Calorimeter!
Electrostatic charge formation through stirring of the reaction mass
Hazardous charges can build up in the reactor interior under the following condi­tions:
• when nonpolar liquids of high resistivity (>10
8
Ω.m) are stirred at high speed (i.e.
at high ow rates),
• with two-phase systems with suspended solids (e.g. after crystallization pro-
cesses in nonconductive solvents or immiscible liquids).
– We therefore recommend to work under an inert atmosphere (nitrogen or ar-
gon)!
METTLER TOLEDO OptiMax™ 1001 7
Safety Measures
Risk of explosion
Risk of burns
Hand injury
Reactors
– Check the reactor periodically for damage (scratches, formation of cracks)!
Hot parts
– Do not touch the cover plate of the box, the xing ring, reactor cover and attach-
ments of the reactors or the overhead stirrer if you work at temperatures above 50 °C.
– The housing of the stirring motor may become hot.
Overhead stirrer
– Do not hold the rotation stirrer shaft or the coupling by hand when you operate
the stirrer motor! You could injure your ngers.

2.2 Measures for Operational Safety

Connection of cables
– Connect the cables of stirrers or sensors to their respective inputs and outputs
before you switch on the instrument, and do not disconnect a cable while the system is in operation! The printed circuit board of the instrument could other-
Caution
Caution
Caution
wise be damaged.
– Make sure that the power supply is easily accessible at any time.
Ventilation of the instrument
– Make sure the instrument is well ventilated! It dissipates a lot of heat especially
during longer heating periods and if the temperature difference between the temperature of the thermostat (Tj) and the temperature of the coolant (Tc) is large. If the temperature of the instrument is too high, its temperature protection device is activated, i.e. the instrument is switched off. After cooling down, you can switch it on again.
– Leave a free space of at least 10 cm between the ventilation slots at the back
side of the instrument and any other object or the wall.
Condensation of atmospheric moisture
– Purge the instrument with dry air, nitrogen or argon (3 L/min without purging the
reactor)! This prevents the ingress and condensation of atmospheric moisture and therefore possible corrosion of the instrument.
8 METTLER TOLEDO OptiMax™ 1001
Caution
Safety Measures
Cooling
The instrument needs a constant ow of a cooling medium. You can use salt-free
tap water, ethanol, ethylen glycol or silicone oil.
– If the water is polluted or has a high degree of hardness, install a lter in the
inlet line and clean it regularly!
– Do not use the owmeter with any other liquids than water, the owmeter is not
resistant against other liquids than water!
Cooling with cryostats
– Do not use NaCl or CaCl
solutions! The high chloride concentration can lead
2
to corrosion of the heat transfer area of the instrument.
– Do not use the owmeter with any other liquids than water, the owmeter is
not resistant against other liquids than water! Connect any other cooling liquid directly to "Cooling In" without using the owmeter!
Thermal shock
Avoid any thermal shock in conjunction with the glass parts of the instrument.
– Never ll cool liquids into hot glassware and vice versa.
Caution
Caution
Caution
Caution
Service
– Never open the instrument! Have it serviced only by METTLER TOLEDO ser-
vice.
General
– Exclude the following environmental inuences
• powerful vibrations,
• direct sunlight,
• atmospheric humidity greater than 80%,
• temperatures below 5 °C and above 40 °C,
• powerful electric or magnetic eld!
METTLER TOLEDO equipment, accessories, and spare parts
– Only use original METTLER TOLEDO equipment, accessories, and spare
parts in conjunction with the OptiMax™ 1001 - otherwise the instrument or parts of the instrument may get damaged. This especially applies for the reac­tor, its cover, the stirrer and the stirrer shaft.
METTLER TOLEDO OptiMax™ 1001 9
Safety Measures
Caution
Touchscreeen connection
Do not connect/disconnect the touchscreen while the OptiMax™ is switched on.
This may seriously damage the instrument.
10 METTLER TOLEDO OptiMax™ 1001
Installation

3 Installation

3.1 Location of the OptiMax™ 1001

– Set up the instrument in a fume hood according to the general safety requirements.
– Variations in chemical behavior during handling due to factors such as temperature,
pressure and concentration can cause equipment to fail, even though it passed an
Caution

3.2 Connections

On top of the housing you nd the quick connect couplings for the purge and inert gas outlets and the sockets for the overhead stirrer, the Tr sensor, a pH sensor and an additional temperature sensor (T
Front view:
initial test. SERIOUS INJURY MAY RESULT. Use suitable guards and/or per­sonal protection when handling chemicals.
aux
):
Opening of thermostat
Reactor window (with back- and frontlight)
Touchscreen with color display
Power push button
Socket for USB stick
Flow indicators for control of purge gas and cooling water
METTLER TOLEDO OptiMax™ 1001 11
Installation
Rear view
On the right rear side of the instrument you can nd the RS232 interface, the CAN bus (for additional equipment), the network connection, the connector for the touchscreen (Control Unit), two USB con-
nectors and the connector for the emergency relay:
Holder for lab bars
The power supply, the elbow couplings for the coolant in- and outlet, the quick connect couplings
for the purge- and inert gas inlets and the connector for the internal purging can be found on the rear bottom of the instrument. The connector for the emergency stop button is also situated in this place.
12 METTLER TOLEDO OptiMax™ 1001
Installation

3.2.1 Connecting the Instrument, the Touchscreen and the Emergency Button

– Connect the touchscreen to the instrument. (See chapter 3.2 "Connections")
– Connect the emergency button to the "Emergency Stop" connector on the rear bottom of the instru-
ment. (See chapter 3.2 "Connections")
– Connect the instrument to the power supply using the included country-specic cable.
The emergency button will trigger the emergency program E when pressed. (See chapter 8.4.2 "Emergency Program E")
Note
The emergency button is only active during an active ramp! As long as no ramp is running, pressing
the emergency button will have no effect on the system!

3.2.2 The Relay for visual or acoustical signalization

The emergency relay is thought for connecting an optical or visual alarm. In case no emergency
program is triggered, pins 1 and 2 are connected. As soon as an emergency program is triggered, the relay switches and pins 2 and 3 are connected.
Relay switched off: contact between pin 1 and pin 2
Relay switched on: contact
between pin 2 and pin 3 (Meaning an emergency pro-
gram has been triggered.)
3 2 1
3
2
1
Contact load: 30 V / 3 A for ohmic and inductive load
METTLER TOLEDO OptiMax™ 1001 13
Installation

3.2.3 Connecting a Coolant

The instrument requires a constant ow of a cooling medium (see Section 2.2: "Measures for Opera­tional Safety: Cooling" and Chapter 10: "Technical Data").
1. Connection of a coolant
– Push one piece of the fabric tube (No. 51 161 187, ø 8/14 mm) over the cooling inlet of the
coolant owmeter, secure it with a hose clamp, and connect it to the coolant supply.
– Push a second piece of the PVC tube over the elbow coupling of the cooling outlet on the
back side of the instrument, secure it with a hose clamp and connect it to the waste water system.
Note:
Never use the ow indicator for the coolant nor the coolant owmeter for any other liquids than
water!
2. Connection of a cryostat
– Screw the insulated connection tubes directly onto the inlet/outlet connectors on the back
side of the instrument.
Caution:
Never use the owmeter for the coolant when using a cryostat, the owmeter is not resistant
against other liquids than water!

3.2.4 Connecting a Purge Gas

Caution Operation without purging the instrument can damage the instrument and will void
the warranty!
To prevent corrosion by condensed atmospheric moisture in the instrument, the instrument must be
purged with a dry gas, e.g. dried air, dried nitrogen or dried argon (see Chapter 11: Technical data).
– Install a PVC tube (No. 51 192 239, ø 4/10 mm ) on the purge gas inlet of the purge gas owmeter,
secure it with a hose clamp and connect it to the gas supply.
Note:
The "Purge In" and "Inert In" inlets on the back side of the instrument are directly connected to
the outlets on top of the housing via seperate lines and are thought for purging the stirrer housing
(Purge Out) or to feed the reactor with inert gas (Inert Out).
14 METTLER TOLEDO OptiMax™ 1001
Installation
Inert gas for reactor
Gas regulation valve
Inert Out
2
6
4
8
10
1
3
5
7
9
600
540
480
420
360
300
60
240
180
120
LPM
LPH
2
6
4
8
10
LPM AIR
From coolant supply
Cooling Out (to “Cooling In” on the back side of the OptiMax)
Purge gas flowmeter
Coolant flowmeter
Purge gas In
Purge gas Out (to “Purge Internal” on the back side of the OptiMax)
Purge Out (to stirrer Purge In)
Coolant In
Purge Internal
Purging the reactor with inert gas
If you want to perform reactions under nitrogen (or any other inert gas),
– Install a quick connect coupling (No. 51 190 324, ø 4/6 mm, red) with the PVC tube (No. 51 161
186) on the "Inert In" inlet connector on the back side of the instrument and secure it with a hose
clamp.
– Connect the PVC tube to the gas supply.
– Install a quick connect coupling on the "Inert Out" connector on top of the instrument and push a
piece of the PVC tube (No. 51 161 186) over the quick connect coupling.
– Integrate a bubble counter with a gas regulation valve (51 161 802, optional available as set) and
the wye piece (51 191 373) into the tubing as shown in the drawing. Proceed, depending on the type of the used reactor. (The use of the wye piece guarantees an uncritical pressure for the reac­tor while the gas ow can be monitored with the bubble counter.)
– Always leave a small opening in the reactor to allow a ow of the puge gas.
green line: purge- / inert gas
blue line: coolant dashed line: tubing inside of the instrument
Internal
purging of the
Instrument
Cooling In
METTLER TOLEDO OptiMax™ 1001 15
Purge In
Inert In
Cooling Out
Installation
With the 500 mL/ 1000 mL reactor
– Use the glass adapter ST19/26 GL14,
– First slide the end of the PVC tube (a) through the screw cap (ME 51 190 317, b),
– then through the silicone rubber sealing ring (ME 51 103 947, c),
– and nally screw the cap onto an ST 19/26 GL14 glass adapter (ME 51 192 208, d).
c abd
– Place the adapter in an ST 19 ground glass opening.

3.3 Installing the Overhead Stirrer

The overhead stirrer consists of
• the stirrer motor with already mounted chuck and clamping nut for fastening the stirrer shaft,
• a Alloy 22 stirrer shaft with pitched-blade stirrer elements in Alloy 22 for two-piece reactors or
• a borosilicate glass stirrer shaft with a PTFE half-moon stirrer blade for one-piece reactors,
• a PTFE adapter with sealing sleeve, compession spring and adapter loosening device,
(the loosening device is already mounted on the adapter)
• the locking device which secures the stirrer shaft.
PTFE Sealing rings
In case the stirrer adapter gets
stuck on the reactor cover, turn the loosening ring counterclockwise
until it pushes slightly against the ground joint. While carefully turn­ing it further, the stirrer adapter
wil come loose and can be taken
away.
Note:
In case you are using PTFE seal­ing rings between stirrer adapter
and ground joint, make sure you
always use two of them on differ­ent heights of the adapter to avoid tumbling of the stirrer!
16 METTLER TOLEDO OptiMax™ 1001
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