102 operating instructions - mettler toledo · mettler toledo easymax® 102 7 2 safety measures the...

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METTLER TOLEDO EasyMax® 102 3

Contents

1 Introduction .......................................................................................................... 6

2 Safety Measures ................................................................................................... 72.1 Measures for your protection ................................................................................. 72.2 Measures for Operational Safety ........................................................................... 8

3 Installation .......................................................................................................... 103.1 Location of the EasyMax® 102 ............................................................................. 103.2 Connections ......................................................................................................... 103.2.1 Connecting the Instrument and the Touchscreen ................................................ 113.2.2 Connecting a Coolant ......................................................................................... 113.2.3 Connecting a Purge Gas ...................................................................................... 113.3 Installing the Overhead Stirrer ............................................................................. 133.4 Installing 100-mL Reactors ................................................................................. 143.4.1 Openings of the 100-mL Reactor Cover .............................................................. 153.4.2 Installing the Tr Sensor in the ST 10 Opening .................................................... 153.4.3 Installing Accessories .......................................................................................... 153.5 Installing 50-mL Reactors ................................................................................... 173.5.1 Openings of the 50-mL Reactor Cover ................................................................ 183.5.2 Installing Pt100 Sensors ...................................................................................... 193.5.3 Installing accessories ........................................................................................... 193.6 Installing One-Piece Reactors ............................................................................. 213.6.1 Installing a stirrer .................................................................................................. 213.6.2 Openings of the 100-mL One-Piece Reactors ..................................................... 223.6.2 Openings of the 50-mL One-Piece Reactor ......................................................... 223.7 Installing 10 mL / 25 mL Reactors ........................................................................ 233.8 Installing PTFE Cover for 100 mL Reactor .......................................................... 243.8.1 Opening of the PTFE Cover for 100 mL Reactor ................................................. 253.9 Installing the Pressure Reactor ............................................................................ 25

4 Design and Operating Principles ..................................................................... 264.1 Thermostat ........................................................................................................... 26

5 Temperature Control Modes ............................................................................. 275.1 Tj Mode ................................................................................................................ 275.2 Tr Mode ................................................................................................................ 275.3 Distillation Mode ................................................................................................... 275.4 Crystallization Mode ............................................................................................. 28

4 METTLER TOLEDO EasyMax® 102

Contents

6 Using additional instruments together with the EasyMax® ............................296.1 Dosing Unit DU SP-50 (ME-51161770) .............................................................. 296.2 pH meter SevenMulti S40 (ME-51302807) ........................................................ 29

7 Safety System of the EasyMax® ...........................................................................317.1 Measures for Chemical Safety ............................................................................. 317.2 Measures for Intrinsic Safety ............................................................................... 317.3 Temperature Monitoring ....................................................................................... 327.4 Emergency Programs of the EasyMax® 102 ........................................................ 327.4.1 Emergency Program A ......................................................................................... 327.4.2 Emergency Program E ......................................................................................... 337.4.3 Warning "Tc < Tc min" .......................................................................................... 33

8 Maintenance and Servicing of the EasyMax® 102 ........................................... 348.2 Changing the Coolant .......................................................................................... 348.3 Cleaning the Interior of a Thermostat .................................................................. 348.4 Replacing the O-Ring and Sealing Ring of the Stirrer Adapter ............................ 358.5 Replacing the Upper Coupling of the Stirrer Motor .............................................. 368.6 Replacing the Clamping and Sealing Rings of Guide Sleeves ............................ 368.7 Cleaning the Instrument ....................................................................................... 378.8 Disposing of the Instrument ................................................................................. 37

9 Malfunctions of the EasyMax® 102 ................................................................... 389.1 Instrument ............................................................................................................ 389.2 Stirrer ................................................................................................................... 389.3 Heating ................................................................................................................. 38

10 Technical data .................................................................................................... 3910.1 Thermostats ......................................................................................................... 4110.2 Reactors ............................................................................................................... 4110.3 Stirrers ................................................................................................................. 4110.4 Cooling of the instrument ..................................................................................... 4210.4.1 Cooling with a cryostat ......................................................................................... 4210.5 Purge gas ............................................................................................................. 42


1 Introduction

The METTLER TOLEDO EasyMax® 102 is a reactor system for performing parallel synthesis, with 10-mL, 25-mL, 50-mL and 100-mL glass reactors and 50mL, 100 mL pressure reactor. The instrument is operated via the integrated Touchscreen. • Eachreactorcanbeindividuallyheatedorcooledanditscontentsindividuallystirredandrefluxed.

The 10-mL and the 25-mL reactors are exceptions.• ThetemperatureofthereactorcontentscanbemeasuredusingaPt100sensor.• ConnectionoftheMETTLERTOLEDOSevenMultiinstrumentequippedwiththeappropriateelec-

trode allows you to measure the pH of the reactor contents.• YoucanexporttheacquireddatatoanotherprogramforfurtherprocessingusingtheUSBMemorySticksupplied.

We, Mettler-Toledo AG, accept no liability whatsoever if you do not observe the following rules and measures for safe operation of the EasyMax® 102 with glass reactors!


2 Safety Measures

The EasyMax® 102 has been tested for the experiments and intended purposes documented in these Operating Instructions. However, this does not absolve you from the responsibility of perform-ing 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.

2.1 Measures for your protection

Risk of an elec-trical shock

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 be otherwise result in death or serious injury.

Risk of explosion

Power failure– Implement appropriate measures against possibly fatal consequences of a

power failure!

Risk of explosion

Potentially explosive environment– Never work in an environment subject to explosion hazards! The EasyMax

housing is not gas tight (explosion hazard due to spark formation, corrosion caused by ingress of gases).

Risk of explosion

Critical reactions– When using the 50-mL and 100-mL reactors, always perform a safety analysis

before starting investigations with a high hazard potential, for example by a Dif-ferential Scanning Calorimeter!

Risk of explosion

Electrostatic charge formation through stirring of the reaction massHazardous charges can build up in the reactor interior under the following condi-tions:• when nonpolar liquids of high resistivity (>108 Ω.m) are stirred at high speed (i.e.

at high flow 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)!


Safety Measures

Risk of explosion

Reactors– Check the reactor periodically for damage (scratches, formation of cracks)!

Risk of burns

Hot parts– Do not touch the cover plate of the box, the fixing rings, reactor covers and at-

tachments of the reactors or the overhead stirrers if you work at temperatures above 50 °C.

– If the overhead stirrer is exposed to a high section modulus, the housing of the stirring motor may become hot.

Hand injury

Stirrer motor– Do not poke your fingers into the slots of the plug-in flange when you operate

the stirrer motor! You could injure your fingers.

2.2 Measures for Operational Safety

Caution

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-wise be damaged.

Caution

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 module 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.

Caution

Overhead stirrer– Do not let the stirrer run with the lower coupling if a stirrer shaft is not mounted!

The coupling touches the plug-in flange and will be damaged if it is not guid-ed.


Safety Measures

Caution

Condensation of atmospheric moisture– Purge the instrument with dry air, nitrogen or argon (3 L/min without purging

the reactor and 5 L/min with purging the reactor)! This prevents the ingress and condensation of atmospheric moisture and therefore possible corrosion of the instrument.

Caution

CoolingThe instrument needs a constant flow of the 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 filter in the

inlet line and clean it regularly!

Cooling with cryostats– Do not use NaCl or CaCl2 solutions! The high chloride concentration can lead

to corrosion of the heat transfer area of the instrument.

Caution

Service– Never open the instrument! Have it serviced only by METTLER TOLEDO ser-

vice.

Caution

General– Please note that certain solvents like Methylene-chloride, DMSO and THF may

cause swelling of PEEK. We recommend to use the PTFE parts to avoid break-age of the glass ports.

Caution

General– Exclude the following environmental influences • powerful vibrationen, • direct sunlight, • atmospheric humidity greater than 80%, • temperatures below 5 °C and above 40 °C, • powerful electric or magnetic field!


3 Installation

3.1 Location of the EasyMax® 102

– Set up the instrument in a fume hood according to the general safety requirements.

3.2 Connections

Front view

Socket for USB stick

Power push button

Window (with backlight)

Holder for lab bars

Fixing ring of thermostat 2

Overhead stirrerTr sensor

Connections (Thermostat 2):

Quick connect coupling for purge gas outlet

Rear view

Elbow coupling of the coolant inlet

Elbow coupling of the coolant outlet

Power supply

RS232 interfaceTouchscreen connection

Network connection

Quick connect couplingfor purge gas inlet

CAN bus (e.g. for DU SP-50)


Installation

3.2.1 Connecting the Instrument and the Touchscreen

– Connecttheinstrumenttothepowersupplyusingtheincludedcountry-specificcable.– Connect the Touchscreen to the instrument.

3.2.2 Connecting a Coolant

Theinstrumentrequiresaconstantflowofacoolingmedium(seeSection2.2:MeasuresforOpera-tional Safety: Cooling and Chapter 11: Technical Data).

1. Connection of a coolant– Push one piece of the PVC tube (No. 51 161 187) over the cooling inlet of the coolant flowmeter, secure it with a hose clamp, and connect it to the outlet of the flow indicator(No. 51 191 915).

– PushasecondpieceofthePVCtubeovertheinletoftheflowindicator(No. 51 191 915) and connect it to the coolant supply.

– PushathirdpieceofthePVCtubeovertheoutletofthecoolantflowmeterandconnectittothe elbow coupling of the cooling inlet on the back side of the instrument. Secure both con-nections with a hose clamp.

– Push another piece of the PVC tube over the elbow coupling of the cooling outlet on the back sideoftheinstrument,secureitwithahoseclampandconnectittothewaste water system.

Note: Neverusetheflowindicatorforthecoolantnorthecoolantflowmeterforanyotherliquidsthanwater!

2. Connection of a cryostat– Screw the insulated connection tubes directly onto the inlet/outlet connectors on the back

side of the instrument.

Caution:Neverusetheflowmeterforthecoolantwhenusingacryostat,theflowmeterisnotresistantagainst other liquids than water!Note:Youcanalsouseonecryostatforcoolingseveralinstrumentsinparallel.Inthiscase,youneedapumpwithhighercapacity,dependingonthenumberofinstrumentsthathavetobecooled.The required cooling capacity at -15 °C increases by 350 W for each EasyMax® 102 connected.

3.2.3 Connecting a Purge Gas

NOTICE Operation without purging the instrument can damage the instrument and will void the warranty!

Topreventcorrosionbycondensedatmosphericmoistureintheinstrument,theinstrumentmustbepurgedwithadrygas,e.g.driedair,driednitrogenordriedargon(seeChapter11:Technicaldata).– Install the quick connect coupling (No. 51 190 342) with the PVC tube (No. 51 161 186) on the gas

inlet connector and secure it with a hose clamp.– Connect the PVC tube to the gas supply.


Installation

Purging reactorsIfyouwanttoperformreactions,forexampleundernitrogen,– install a quick connect coupling on the purge gas connector of the corresponding thermostat and

push a piece of the PVC tube (No. 51 161 186) over the quick connect coupling.– integrateabubblecounterwithagasregulationvalve(51161802,optionalavailableasset)intothetubingasshowninthedrawingonthenextpage.Proceed,dependingonthetypeoftheusedreactor:

With the 100-mL reactor– First slide the end of the PVC tube (a)throughascrewcap(No.51190317,b),– thenthroughthesiliconerubbersealingring(No.51103947,c),– andfinallyscrewthecapontoanST14glassadapter(No.51191267,d).

– Place the adapter in an ST 14 ground glass opening.

c abd

1

2

3

2

6

4

8

10

LPM

AIR

2

6

4

8

10

1

3

5

7

9600

540

480

420

360

300

60

240

180

120

LPM LPH

CoolantPurge gas

Purge gas for reactor 1

Purge gasfor reactor 2

From coolantsupply

Cooling Out(to “cooling In” on the backside of the EasyMax)

Purge gas In

Purge gas Out(to “Purge In” onthe backside ofthe EasyMax)

(With the help of the magnetic holder, the bubble counter set can easily be attached to the housing of the EasyMax.)


Installation

With the 50-mL reactor– FirstslidetheendofthePVCtubethroughascrewcap(No.51190317),– thenthroughthesiliconerubbersealingring(No.51103947),– andfinallyscrewthecapontoaGL14opening.

3.3 Installing the Overhead Stirrer

Theoverheadstirrerconsistsofthestirrermotor,astirrershaftwithpitched-bladestirrerelementsin Alloy 22 for 50-mL and 100-mL reactors or an anchor or pitched-blade stirrer in glass or a stirrer shaft with an anchor blade in Alloy 22 for 100-mL reactors (see EasyMax® Catalog). The speed range is 50 to 1000 rpm.

PEEK adapter

Pitched-blade element

Stirrer motor

Adjustment unit

PA washer

Lower coupling

Upper coupling

Plug-inflange

Stirrer shaft

Locking lever

Assembling the stirrer– Screw the pitched-blade element (or the anchor blade for 100

mL reactors) onto the stirrer shaft. – Push the stirrer shaft or the glass stirrer from below through the

opening of the reactor cover. – Push the PEEK adapter with the height adjustment unit over the

stirrer shaft and insert it into the tapered opening of the cover.– Place the PA washer over the stirrer shaft onto the adjustment

unit.– Push the lower coupling onto the stirrer shaft.– Pushthestirrermotorovertheadjustmentunitinsuchaway,

that it snaps into its three pins. – Secure the adapter on the reactor with a Keck clamp.

You can change the immersion depth of the stirrer with the height adjustment unit: – Pressitslockinglever,lifttheunitandletitsnapintooneofthe

adapter holes.

– Connect the stirrer cable to the connector of the corresponding thermostat.

NOTICEDo not let the stirrer run with the lower coupling if the stirrer shaft isnotmounted!Thecouplingtouchestheplug-inflangeandwillbe damaged if it is not guided.


Installation

3.4 Installing 100-mL Reactors

With a magnetic stir bar Place the magnetic stir bar carefully in the reactor.

With an overhead stirrer – Push the glass stirrer or the stirrer shaft with anchor or pitched-blade element through the central

opening of the reactor cover before you place the cover onto the reactor and connect it to the stirrer motor (see Section 3.3: Installing the Overhead Stirrer).

Reactor cover

BuckleHook

Shoulder for placingthe reactor

100-mL reactor

Reactor holder

O-ring

Clamp chain

– Place the reactor in the reactor holder..– Place the O-ring on the cover rim and

place the cover on the reactor.– Place the clamp chain carefully around the coverandthereactorflanges.

– Screw the hook in or out so that the buckle canbeeasilyclosed(withonefinger).

NoteBefore you place the reactor in the thermo-stat, we recommend that you install theTrsensor and other inserts in order to check their distance from the stirrer or the bottom of the reactor. We also recommend that you add the reagents and solvent for the starting volumeandpossiblycheckthefilllevelofthefirstfill.TheTrsensormustbeimmersedtoadepth of at least 2 cm in the reaction solution in order to give correct measurement values.


Installation

3.4.1 Openings of the 100-mL Reactor Cover

Choose the openings for inserts and attachments so that cable and tubing connections are as neat and tidy as possible.

Opening for overhead stirrer

Openingforrefluxcondenser

Opening for 50-mL dropping funnel

Opening for Tr sensor with ST 10/ST 19 adapter

Opening for pH electrode with ST 14-6 mm guide sleeve

Opening for turbidity probe with ST 10-6 mm guide sleeve

NS 10

NS 10

NS 14

NS 14

NS 14

NS 14

3.4.2 Installing the Tr Sensor in the ST 10 Opening

– FirstslideaUNF1/4"G28nut(b)overthesensor(No.51191515,a),– thenaUNF1/4"G28ferrule(No.51191514,c),– andfinallytheST10/19adapter(No.51161728,d).

– Screw the nut lightly into the adapter: this presses the ferrule into the nut.

Make sure the temperature sensor shows an immersion depth of at least 2 cm into the liquid.

3.4.3 Installing Accessories

1. Ifyouusethemagneticstirbar,youcanmount• eitheradryingtube• ortherefluxcondenser(No.51161029)onthecentralgroundglassopeningof the reactor

cover.

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Installation

2. Whenusingthe"Semi-Micro-L"pHelectrodeorsensorswith6-mmdiameter,in an ST 10 opening,– unscrew the nut of the ST 10/19 guide sleeve slightly and push the electrode through the

sleeve (No. 51 161 515).

in an ST 14 opening,– unscrew the nut of the ST 14/23 guide sleeve slightly and push the electrode through the

sleeve (No. 51 160 680).– Placethesleeveonthecorrespondingopening,setthedesireddistancetothestirrerand

tighten the nut.– Connect the cable of the pH electrode to the SevenMulti instrument.

3. Whenusingtherefluxcondenser– pushtheplastichoseconnectionwithseal(No.51190319)throughtheholeoftheGL14screwcap(No.51190317),push a tube over the hose connection and secure it with a hose clamp.

– Tightentheplastichoseconnectionwiththescrewcapontheglassthreadoftherefluxcon-densor.

–Whenyouhaveinstalledsensorsandaccessories,placethereactorinthethermostat.– IfyouhaveinstalledtheoverheadstirrerandTrsensor,connecttheircablestotheconnectorsthat

correspond to the thermostat.

NoteWhentheexperimentiscompleted,youcanremovethecoverwiththeinsertsfromthereactor,rinse the inserts and place the cover directly on the reactor holder:


Installation

3.5 Installing 50-mL Reactors

With a magnetic stir bar – Place the stir bar carefully in the reactor.

With an overhead stirrer – Pushthestirrerthroughthecentralopeningofthereactorcover,beforeyouplacethereactorcover

on the reactor and screw the pitched-blade element onto the stirrer shaft (see Section 3.3: Install-ing the Overhead Stirrer).

Notch

Reactor cover

Reactor clamp

Reactor holder

50-mL reactor

O-ring

Groove

Knurled screw with washer


Groove

Whiteclawfixingwithcam

– Loosen the knurled screws of the reactor clamp, lift theclawfixingsoutof thegroovesandplacethemoutwardoverthefixingring.

– Place the reactor in the reactor clamp. – Place the reactor with reactor clamp ring on

the reactor holder. – Place the O-ring supplied on the cover rim

(possibly use a little grease). – Place the reactor cover on the reactor so that

its groove locates the cam of the white claw fixing.

– Lift the reactor clamp– Placetheclawfixingsoverthereactorcover,

press them into the corresponding groove and tighten them with the knurled screws.

NoteBeforeyouplace the reactor in the thermostat,we recommend that you install the Tr sensor and other inserts in order to check their distance from the stirrer or the bottom of the reactor. We also recommend that you add the reagents and sol-vent for the starting volume and possibly check thefilllevelofthefirstfill.TheTrsensormustbeimmersed to a depth of at least 2 cm in the re-action solution in order to give correct measure-ment values.


Installation

Fixing ring ofthe thermostat

Window of the thermostat

50-mL receptacle with window

Cylindrical pin

Allen screw

Hole

Fixing ring

– After installing the sensors and in-serts,

– place the 50-mL receptacle in the thermostat with the window facing for-ward. Turn it slightly until it snaps in.

– Placethefixingringonthe50-mLre-ceptaclesothattheholeofthefixingring locates the cylindrical pin.

– Place the reactor with the reactor clamp in the 50-mL receptacle so that thegrooveunderthewhiteclawfittinglocateswiththeAllenscrewofthefix-ing ring.

– If you have installed the overhead stir-rerandTrsensor,connecttheircablesto the connectors that correspond to the thermostat

3.5.1 Openings of the 50-mL Reactor Cover

Choose the openings for inserts and attachments so that cable and tubing connections are as neat as possible.

GL 14NS 14

NS 10

NS 10NS 7

GL 14Opening foroverhead stirrer

Openingforrefluxcondenser(with overhead stirrer)

Opening for- guide sleeve with pH electrode or turbidity probe-refluxcondenser (with overhead stirrer)

Opening for- Tr sensor- dosing tubes

Openings for- glass funnel for dosing solids- dosing tubes- Tr sensor- pH electrode- turbidity sensor


Installation

3.5.2 Installing Pt100 Sensors

1. Pt100 sensor in the ST 7 opening: – FirstslideaUNF1/4"G28nut(No.51191515,b) over the sensor (a),– thenaUNF1/4"G28ferrule(Nr.51191514,c),–andfinallyanST10-UNF1/4"G28adapter(Nr.51160200,d).

– Screw the nut lightly into the adapter: this presses the ferrule into the nut.

2. Pt100sensorintheGL14opening:– FirstslideaGL14screwcap(No.51190317,b) over the sensor (a),– thenaUNF1/4"G28nut(No.51191515,c),– thenaUNF1/4"G28ferrule(No.51191514,d),– andfinallythePTFEGL14-UNF1/4"283.2adapter(No.51161558,e).

– Screw the adapter lightly onto the nut: this presses the ferrule into the nut. – Slideasiliconerubbersealingring(No.51103974,f) over the sensor into the screw cap and screwthecapontotheGL14screwthread.

3.5.3 Installing accessories

1. Ifyouusethemagneticstirbar,youcanmountadryingtubeonthecentralgroundglassope-ning of the reactor cover.

2 ScrewtheGL14screwcapwithPTFEsealing(No.51190318)ontotheglassthreadthatyouare not using.YoucanusetheGL14screwcap(No.51190317)withseptum(No.51191170)for• takingsampleswithasyringe,• dosingtubes,e.g.ifyoumakeasuitableholeintheseptumbeforehand.

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Installation

3a. When using an ST opening for the "InLab1022" pH electrode or sensors with 6 mm diameter:– Unscrew the nut of the ST 10/19 guide sleeve (No. 51 161 515) slightly and push the electrode

through the sleeve. – PlacethesleeveononeoftheST10openings,setthedesireddistancetothestirrerand

tighten the nut.

– Connect the cable of the pH electrode to the SevenMulti instrument.

3b. WhenusingaGL14openingforthe"InLab1022"pHelectrodeorsensorswith6-mmdiameter:– SlidetheGL14screwcap(No.51161037,b) over the sensor (a),– slidethePTFEadapter(No.51161037,c)overthesensorintothecap,and– pushthesiliconerubbersealingring(No.51103947,d) over the sensor into the cap.

– Screw the cap lightly onto the glass thread. – Tooptimizethepositionofthesensor,turntheadapter-itsboreholeisnotcentered-andthen

tighten the screw cap.

– Connect the cable of the sensor to the corresponding instrument.

4. Whenusingtherefluxcondensor,– pushtheplastichoseconnectionwithseal(No.51190319)throughtheholeoftheGL14screwcap(No.51190317),push a tube over the hose connection and secure it with a hose clamp.

– Tightentheplastichoseconnectionwiththescrewcapontheglassthreadoftherefluxcon-densor.

NoteWhentheexperimentiscompleted,youcanremovethecoverwithinsertsfromthereceptacle,rinsethe inserts and place the cover directly on the reactor holder:

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Installation

3.6 Installing One-Piece Reactors

The two 100-mL One-Piece reactors can be inserted directly into the thermostat. For the 50-mL One-Piecereactorthereceptacle(seechapter3.5)hastobeused.Thefillingisdoneviatheopeningsforinsertsandattachements.Ifnotinuse,thereactorscanbestoredintherespectivereactorholder:

NoteBeforeyouplacethereactor inthethermostat,werecommendthatyouinstall theTrsensorandother inserts in order to check their distance from the stirrer or the bottom of the reactor. We also recommend that you add the reagents and solvent for the starting volume and possibly check the filllevelofthefirstfill.TheTrsensormustbeimmersedtoadepthofatleast2cminthereactionsolution in order to give correct measurement values.

3.6.1 Installing a stirrer

With a magnetic stir bar: – Place the stir bar carefully in the reactor.

With an overhead stirrer: – Push the stirrer through the central opening of the reactor. Only use the glass stirrer (ME-51 161 748)

and the corresponding stirrer blade (ME- 51 161 749) in connection with the One-Piece reactors!

4-port reactor(100 mL)


reactor holder



Installation

3.6.2 Openings of the 100-mL One-Piece Reactors


3.6.2 Openings of the 50-mL One-Piece Reactor


ST 19/26 ST 19/26

ST 10/19

ST 19/26 ST 19/26

ST 10/19

ST 14/23

ST 19/26

ST 19/26

4-port reactor(ME- 51 161 786)

5-port reactor(ME- 51 161 747)

ST 19/26ST 19/26

ST 19/26ST 10/19

ST 14/23

5-Port Reaktor(ME- 51 161 792)


Installation

3.7 Installing 10 mL / 25 mL Reactors

– Remove the screw caps with silicone rubber seals (septum) of the reagent tubes. – Put the magnetic stir bars carefully into the reaction tubes and allow them to slide to the bottom. – Place the tubes in the openings of the corresponding receptacle (10 mL or 25 mL).– Place the receptacle on the pin of the desired thermostat with one of the windows facing forward.

Ifyouwanttofollowthereactionsinoneoftheothertubes,– raisethereceptacleslightly,turnittothedesiredreactiontubeandthenlowerit.

10 mL

25 mL


Installation

3.8 Installing PTFE Cover for 100 mL Reactor

The PTFE cover set is developed to combine EasyMax® with IR and FBRM® probes. It is mainly used to run crystallization experiments.

With a magnetic stir bar Place the magnetic stir bar carefully in the reactor.

With an overhead stirrer – Push the glass stirrer or the stirrer shaft with anchor or pitched-blade element through the central

opening of the reactor cover before you place the cover onto the reactor and connect it to the stirrer motor (see Section 3.3: Installing the Overhead Stirrer).

– Place the reactor in the reactor holder.– Place the O-ring on the cover rim and place the

cover on the reactor.– Place the clamp chain carefully around the coverandthereactorflanges.

– Screw the hook in or out so that the buckle can beeasilyclosed(withonefinger).

NoteBeforeyouplacethereactorinthethermostat,werecommend that you install the Tr sensor and oth-er inserts in order to check their distance from the stirrer or the bottom of the reactor. We also recom-mend that you add the reagents and solvent for thestartingvolumeandpossiblycheckthefilllev-elofthefirstfill.TheTrsensormustbeimmersedto a depth of at least 2 cm in the reaction solution in order to give correct measurement values.

PTFE® cover

O-ring

Clamp chain

BuckleHook

100-mL reactor

Reactor holder



Installation

3.8.1 Opening of the PTFE Cover for 100 mL Reactor

3.9 Installing the Pressure Reactor

In order to know how to install the pressure reactor, refer to documentNr.51710880 EasyMax Pressure Reactor.

ST19/26FBRM® probe

ST10/19Turbidity sensor, pH electrode, Tr sensor

ST14/23Overhead stirrer

ST14/23Turbidity sensor, pH electrode, React IR probe,reflux condensor, dropping funnel

ST19/26FBRM® probe

ST14/23Turbidity sensor, pH electrode, React IR probe,reflux condensor, dropping funnel


4 Design and Operating Principles

The EasyMax® 102 comprises four modules:• the electronic control unit• the two thermostats• the measurement system• the Touchscreen

The Touchscreen is used to control the EasyMax®, to perform experiments and manage the related data (store and export experimental data). See document number 30032003 Touchscreen Operating Instructions for detailed information.

The microprocessor control in the instrument acquires a set of the set and actual values every 2 seconds: the temperature of the reaction mass, thermostat, and coolant as well as the stirrer speed. These values are used for controlling the instrument and to trigger warnings and emergency programs.

4.1 Thermostat

Tj sensor

Reactor wall

Tr sensor

Peltier elementTc sensor

Cooling element

Heater Heater

Reactor shell

• TheTrsensormeasuresthetemperatureofthereactorcontents,• theTjsensorthetemperatureofthereactorshell,and• theTcsensorthetemperatureofthecoolingelement.

Overhead stirrer


5 Temperature Control Modes

The EasyMax® 102 has four control modes available:• theTjmode,• theTrmode,• thedistillationmode,thatisalsousedforrefluxing• thecrystallizationmode.

5.1 Tj Mode

Thetemperatureofthethermostatiscontrolled.Tjisheldataspecificvalueorchangedwithatem-peratureramp.

5.2 Tr Mode

Thetemperatureofthereactorcontentsiscontrolled.TherebyTrisheldconstantorchangedwitharamp.Deviationsofthetemperatureofthereactorcontentsfromthesetvalue(throughheatofreaction)arecompensatedbyappropriatecorrectionof the thermostat temperature, i.e. theheatgeneratedisdissipated.

5.3 Distillation Mode

Thevalueenteredforthedesiredtemperaturedifferencebetweenthethermostatandthereactorcontents(Tj-Tr)isaddedtothemeasuredtemperatureofthereactorcontentsandgivesthesetvalueforthecontrolofTj.Forthismode,youhavetoenter• thedesiredtemperaturedifference,Tj-Tr,and• theupperlimitofthejackettemperature,Tjend.Asaresult,duringthetimeinwhichnosolventisdistilled,thetemperatureofthereactorcontents,Tr,risesinaccordancewiththevalueenteredforTj-Tr.Duringtheactualdistillation,TrandhencealsoTjremainapproximatelyconstant.AssoonasTjendisreached,thefinal(end)temperatureisheld.

Tj (Tj-Tr)

Tj end

t

Tr

T


5.4 Crystallization Mode

Thevalueenteredforthedesiredtemperaturedifferencebetweenthethermostatandthereactorcontents(Tr-Tj)issubtractedfromthemeasuredtemperatureofthereactorcontentsandgivesthesetvalueforthecontrolofTj.Forthismode,youhavetoenter• thedesiredtemperaturedifference,Tr-Tj,and• thelowerlimitofthejackettemperature,Tjend.Asaresult,duringthetimeinwhichnocrystallizationoccurs,thetemperatureofthereactorcontents,Tr,dropsinaccordancewiththevalueenteredforTr-Tj.Duringtheactualcrystallization,TrandhencealsoTjremainapproximatelyconstant.AssoonasTjendisreached,thefinal(end)tempera-tureisheld.

Tj

(Tr-Tj)

Tj start

t

Tr

T

Crystallization Mode

Crystallization


6 Using additional instruments together with the EasyMax®

6.1 Dosing Unit DU SP-50 (ME-51161770)

The Dosing Unit SP-50 is a volumetric dosing de-vice which allows highly accurate dosing controlled via the local touchpad of the EasyMax® or via the PC software iControl for EasyMax®.Different from other dosing units the DU SP-50 does not need a power cable when connecting to the EasyMax®. The whole communication and also the power supply is done via a CAN connection cable. • Four different syringe volumes (from 1 mL up

to 50 mL) can be used.• A simple Plug & Play behavior makes it easy

to install and setup the dosing unit.• One dosing unit can be used to dose into both

reactors of an EasyMax® at the same time.

Press the key on the EasyMax® 102 touchscreen to open the Device management menu. Within this menu all connected dosing units can be configured and operated. Please refer to the document number 30032003 Touchscreen Operating Instructions for detailed information.

6.2 pH meter SevenMulti S40 (ME-51302807)

With the SevenMulti S40 pH meter it is possible to measure the pH value simultaneously in both reactors of the EasyMax.Once the pH meter is attached to the EasyMax® with a connecting cable, it will log the measurement values and show them online.

Note: If you want to use a SevenMulti-instrument together with the EasyMax, make sure that it is equipped with two pH-modules.

Note: Do not touch the SevenMulti™ touchpad when it is connected to the device to avoid system crash.

Note: If SevenMulti is connected to the EasyMax®, pH control on both the reactors is not pos-sible with only one dosing unit.

Connect two dosing units, one for each reac-tor.


Connecting Peripherals

Using the EasyMax® together with a SevenMulti:

Connect the SevenMulti with the RS232 cable (ME-51190589) to the RS232 port of the EasyMax.Once the instruments are connected proceed as follows:

On the SevenMulti™

1. Set time and date.2. Select "LabX (bidirectional)" from the interface settings. Keep the default values:

Baud rate 9600Data bit 8Stop bit 1Parity NoHandshake xoff

3. Adapt the calibration settings and perform a calibration, when not connected to the EasyMax®. (Use MTC and enter the temperature of the buffers for temperature correction.)

4. Set the temperature mode to MTC (Manual temperature compensation) and enter the reactor temperature for the adjustment of the slope).

Note: If you want to use both channels of the pH meter, you have to perform steps 3 and 4 for both channels, Left and Right.

5. Switch the SevenMulti™ to Dual mode before starting the measurement. Don't press any keys on the pH meter, once the experiment was started.

For more information please refer to the operating instructions of the SevenMulti (ME-51710416).

On the EasyMax®

The SevenMulti™ is automatically detected by EasyMax®.

In case the SevenMulti™ is not connected to the EasyMax®, the following message appears:

Select OK and connect the SevenMulti™.


7 Safety System of the EasyMax®

The safety system monitors safety with chemical reactions as well as the safe operation of the instru-ment functions.

Safety with chemical reactionsThe safety with chemical reactions is assured by monitoring the limit values of the temperatures.You as the user bear full responsibility for selection of the safe limit values and the reaction control. In the case of chemical reactions with a virtually unknown profile, you are responsible for prevent-ing the reactor reaching a hazardous condition long before the limit values of the intrinsic safety are reached and before the safety system would respond.

Intrinsic safetyThe operation of the instrument is monitored.For every instrument configuration used, you are responsible for ensuring that the entire system is safe if a power failure occurs and that the reaction currently in progress cannot get out of control.

7.1 Measures for Chemical Safety

• Monitoring the limit values for Tr, Tj and Tc defined by you; triggering emergency programs if limit values are exceeded.

• Limitation of the Tj set value to Tj end in the distillation or reflux mode.• The safety temperature Tsafe you defined is used as the set temperature for emergency program

E (see also Section 7.4.3).

7.2 Measures for Intrinsic Safety

The following measures have been implemented for error recognition and for effective intervention when error conditions arise:

Electronics• Monitoring the microprocessor for breakdown (watchdog).• Monitoring of the stirrer motor• 100-Ω resistor as reference for checking the A/D converter.

Software• Self-test of the microprocessor system after switching on.• Restriction of the temperature difference "Tj - Tr" to maximum 60 K in the Tr and distillation modes

to avoid glass breakage.• Monitoring all measured values for plausibility and failure.• Monitoring of the safety limit values.• Plausibility test of parameters.• Error recognition and triggering of emergency programs.


Safety System

7.3 Temperature Monitoring

To ensure the acquisition of reliable values of the measured temperature, the electronics employs a reference value in the form of a precision resistor that corresponds to the resistance of a Pt100 at 266 °C (= 200 Ω).

Tj sensorThe Tj sensor is monitored for a preset measured value range. If values fall outside this range, emer-gency program E is triggered. Emergency program A is triggered if the sensor is defective.

Tr sensorThe Tr sensor is monitored for a preset measured value range. If values fall outside this range, emer-gency program E is triggered. This program is also triggered if the sensor is not attached or defective.

Tc sensorThe Tc sensor is monitored for a preset measured value range. If values fall outside this range, emer-gency program A is triggered.

The electronic system is designed so that if a short circuit or failure occurs, -125 °C is displayed.

7.4 Emergency Programs of the EasyMax® 102

The microprocessor of the instrument can trigger two emergency programs, emergency program A or E.• As long as emergency program A is active, errors which trigger this program cannot be reset, i.e.

you have to switch off the instrument and rectify the error. An exception is the emergency program "Tc higher than Tc max" (program A).

• Errors which trigger emergency program E can be reset, i.e. you can continue the experiment when you have rectified the error.

7.4.1 Emergency Program AIf this emergency program is triggered, the following message is displayed: "Heater and Peltier ele-ment switched off!" followed by the error cause.

Error causes Measures to take

No connection Switch off the instrument and restart it.

A/D converter defective Call METTLER TOLEDO Service.

Power PIC error Call METTLER TOLEDO Service.

Tj sensor defective Call METTLER TOLEDO Service.


Safety System


Tc sensor defective Call METTLER TOLEDO Service.

Tc > Tc max(The temperature of the coolant, Tc, is higher than the defined safety limit value ,Tc max)

Monitor the Tc value in the Safety page and check the flow rate of the coolant Touch Reset, when Tc is lower than Tc max again and continue the inter-rupted experiment.

7.4.2 Emergency Program EIf this emergency program is triggered, the following message is displayed: "Tj is controlled to T safe" followed by the error cause.


Tr sensor defective or not connected. Connect the Tr sensor or connect a new one.

Tr > Tr max(The temperature of the reactor contents, Tr, is higher than the defined safety limit value Tr max)

Touch Reset and wait until Tr is lower than Tr max; then continue the experi-ment.

Tr < Tr min(The temperature of the reactor contents, Tr, is lower than the defined safety limit value Tr min)

Touch Reset and wait until Tr is higher than Tr min; then continue the experi-ment.

Tj > Tj max(The temperature of the thermostat, Tj, is higher than the defined safety limit value Tj max)

Touch Reset and wait until Tj is lower than Tj max; then continue the experi-ment.

Tj < Tj min(The temperature of the thermostat, Tj, is lower than the defined safety limit value Tj min)

Touch Reset and wait until Tj is higher than Tj min; then continue the experi-ment.

NoteIf an emergency program A and E are triggered at the same time, program A is executed.

7.4.3 Warning "Tc < Tc min"


This warning appears if Tc is lower than the defined safety limit Tc min.

Check the temperature of the coolant.


8 Maintenance and Servicing of the EasyMax® 102

Any maintenance or servicing not specifically described in the following must be performed by METTLER TOLEDO service.Any maintenance or service work not performed in strict accordance with the directions given in previous sections and especially the directions mentioned in the following shall ab-solve Mettler-Toledo AG from any liability whatsoever in regard to the consequences of such improper work!We strongly recommend you to have the instrument inspected once a year by a METTLER TOLEDO service engineer.

8.1 Checking the Reactor

To check the reactor vessel for possible damage (scratches and cracks), it must be empty, clean, dry and open. Small hairline cracks can be detected by refraction using an additional light source (focused, not dispersed light).

8.2 Changing the Coolant

If you change the coolant, you must rinse and dry the tubing in the instrument before you use the new coolant.– Remove the connection tube first at the "In" inlet, and then at the "Out" outlet.– Rinse and dry the tubing in the reverse direction (from the "Out" outlet).– Afterward fill the tubing with the new coolant.

8.3 Cleaning the Interior of a Thermostat

If chemicals get into the thermostat,– remove the reactor or receptacle and clean the interior of the thermostat with a solvent suitable for

removing the substance.


Maintenance and Servicing

8.4 Replacing the O-Ring and Sealing Ring of the Stirrer Adapter

If you have to perform reactions under tight system conditions, we recommend that you change the O-ring and the sealing ring at regular intervals:– Press the locking lever of the height adjustment unit (see picture) and pull the adapter completely

down, turn it slightly to the left and remove it from the locking device.- Loosen the O-ring from the groove of the PTFE adapter by applying pressure to the inner circum-

ference of the O-ring with a size 0 screwdriver as shown in the diagram:

right wrong O-ring / PTFE ring

– Afterward also remove the PTFE sealing ring and replace both rings. (The rings are delivered as a unit under No. 51 191 375.)

– Press the ring unit into the adapter.– Push the height adjustment unit over the adapter again:

Locking lever

Pin Groove

– Push down the locking lever and turn the height adjustment unit until its lower pin is in the groove of the adapter; turn it slightly to the right, then push it upward and let go the locking device.



8.5 Replacing the Upper Coupling of the Stirrer Motor

If the upper coupling of the stirrer motor is damaged, for example by chemicals, you can replace it (No. 51 161 360).– Pull the adapter with the height adjustment unit, stirrer shaft and lower coupling out of the stirrer

motor.

Setscrew of the upper coupling

Flat part of the motor shaft

Upper coupling

– Loosen the setscrew using a 2-mm Allen wrench and remove the coupling from the motor shaft

– Push the new coupling over the motor shaft with the round part in front so that its thread is on the flat part of the shaft.

– Push the coupling over the motor shaft until it is flush with it (see diagram above)

– Screw in and tighten the setscrew using the Al-len wrench.

8.6 Replacing the Clamping and Sealing Rings of Guide Sleeves

Nut

Sleeve

Clamping ring

Sealing ring

– Unscrew the nut from the guide sleeve and re-move the sleeve from the sensor.

– Remove the clamping and sealing rings from the sensor and replace them with new rings in the same order as shown in the picture.

– Screw the guide sleeve and nut together again.



8.7 Cleaning the Instrument

The housing of the instrument is not watertight (i.e. splash proof). We therefore recommend that you clean the box with a cloth soaked in ethanol.

Risk of burns

– Do not clean the cover plate of the reactor box until it has reached room tem-perature

8.8 Disposing of the Instrument

In conformance with the European Directive 2002/96/ EC on Waste Electrical and Electronic Equipment (WEEE), this device may not be disposed of in do-mestic waste. This also applies to countries outside the EU, per their specific requirements.Please dispose of this product in accordance with local regulations at the col-lecting point specified for electrical and electronic equipment. If you have any questions, please contact the responsible authority or the dis-tributor from which you purchased this device. Should this device be passed on to other parties (for private or professional use), the content of this regulation must also be related. Thank you for your contribution to environmental protection!


9 Malfunctions of the EasyMax® 102

9.1 Instrument

Instrument inoperativeIf the instrument does not start when you switch it on, you should first check the power supply before calling the METTLER TOLEDO Service.

No display on TouchscreenMake sure the touchscreen cable is connected to the instrument before calling the METTLER TOLEDO Service.

Cooling below Tc not possiblePlease call the METTLER TOLEDO Service

Wrong Tr measurement value1. Check the immersion depth: The Tr sensor must be immersed in the reaction mass to a depth of

at least 2 cm! 2. Check the value with a reference thermometer or with the Tr sensor of the second thermostat: • If their values are correct, the sensor is defective. • If their values are also wrong, please call the METTLER TOLEDO Service.

Window of the thermostat foggedMake sure the thermostat is purged or increase the purge rate.

9.2 Stirrer

Overhead stirrerIf the stirrer does not operate after switching on the instrument, please make sure it is not blocked and try it on the other reactor before calling the METTLER TOLEDO Service.

Magnetic stir barIf the stirrer stops stirring or starts to "bounce" (speed to high!), enter a smaller value for the stirrer speed.

9.3 Heating

Heating failureIf the heater is inoperative, please call the METTLER TOLEDO Service.


10 Technical data

Power supply

• Voltages 100 – 240 VAC

• Permissible voltage fluctuation ±15%

• Frequency 50/60 Hz

• Power consumption max. 1000 VA

Materials

• Cover plate stainless steel coated with PFA/FEP

• Housing material powder-coated stainless steel

• Connectors for purge gas stainless steel, nickel-plated brass

• Purge gas lines PVC, FEP, PP, PVDF, PTFE, aluminum

• Coolant tubing PVC, PVDF, PTFE,copper

• Cooling connectors nickel-plated brass

• Holder for lab bars stainless steel

• LEMO connectors for Tr sensor and overhead stirrer

chrome-plated brass with protection cap in POM

• Reactor windows Borosilicate glass 3.3

• Receptacles for 10- and 50-mL reactors anodized aluminum

• Fixing rings of thermostats PTFE C25

• USB connector stainless steel with protection cap in POM

• On/Off switch stainless steel

• Glass reactors Borosilicate glass 3.3

• Magnetic stirrer PTFE coated

• Overhead stirrer Borosilicate glass 3.3 or Alloy 22

• Touchscreen PA 12, aluminum

• Protective cover for Touchscreen Barex®

Backlight 2 LED per reactor

Weight incl. Touchscreen 16 kg


Technical Data

DimensionsTop view

470

mm

376

mm

195.

4 m

m33

2 m

m

560.4 mm

Side view with 100-mL reactor

624

mm

280.

5 m

m

495

mm

179.

5 m

m58

.5

133.4 mm355 mm46

Ambient conditions

• Temperature 5 °C – 40 °C

• Max. relative atmospheric humidity 80% for temperatures up to 31 °C, decreasing linearly to 50% relative atmospheric humidity at 40 °C

• Altitude up to 2000 m

• Use indoors

• Overvoltage category ll

• Pollution degree 2


Technical Data

10.1 Thermostats

Power

• Heating

• Cooling

360 W per thermostat

max. 150 W per thermostat

Temperatures

• Range Tj: -40 °C (with Tc < -15 °C) to 180 °CTr: -40 °C (with Tc < -15 °C) to 180 °C*Tc: -40 °C to 60 °C

* The temperature range of Tr is limited by the corresponding heating or cooling requirements and cooling power.

• Resolution Tj: 0.1 KTr: 0.1 K

• Maximum permissible errors 1.0 °C for the whole range

• Measured value acqcuisition every 2 seconds

• Operating modes isothermal und isoperibolic

10.2 Reactors

Pressure 0.05 bar to ambient pressure

Volumes 100-mL 50-mL 10-mL 25-mL

• Nominal volume• Working volume• Start volume (without Tr sensor)• Start volume (with Tr sensor)

150 mL 100 mL 25 mL 50 mL

70 mL 50 mL 25 mL 30 mL

30 mL 5 mL 1 mL

25 mL25 mL 3 mL

10.3 Stirrers

Overhead stirrer• Operating mode• Measured value acquisition• Speed range

Control to constant value or rampevery 2 seconds50 to 1000 rpm

Magnetic stirrer• Speed range 50 to 1000 rpm


Technical Data

10.4 Cooling of the instrument

You can use salt-free tap water, ethanol, ethylene glycol or silicone oil.

Min. flow rate approx. 3 L/min

10.4.1 Cooling with a cryostat

Cooling power 350 W at -15 °C

Min. pump capacity 0.5 bar

10.5 Purge gas

Max. inlet pressure 7 bar

Min. gas flow 3 L/min (without purging the reactor)5 L/min (with purging the reactor)


Technical Data

For more informationwww.mt.com/EasyMax

EasyMax™ 102Chemistry Made Easy

Quality certificate. Development, production and testing according to ISO 9001. Environmental management system according to ISO 14001.

Worldwide service. Our extensive service network is among the best in the world and ensures maximum availability and service life of your product.

European conformity. The CE conformity mark provides you with the assurance that our products comply with the most recent EU directives.

On the internet. You will quickly find lots of essential information about our products, our services and our company at http://www.mt.com

Mettler-Toledo AG, AutoChem RXESonnenbergstrasse 74CH-8603 Schwerzenbach, SwitzerlandPhone +41-44 806 77 11Fax +41-44 806 72 90

Internet www.mt.com/autochemE-Mail [email protected]

Subject to technical changes.© 03/2013 Mettler-Toledo AGPrinted in Switzerland,51710591F

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