Metrohm Autolab RDE2 User manual

RDE2
Usermanual

DECLARATIONOFCONFORMITY
WeMetrohm Autolab B.V.
Utrecht
The Netherlands
Certifythatthe product
AUTOLABRDE
is in conformitywith ECDirectives 89/336/EEC and73/23/EWG.
Standardsused: EMC: EN 61326-1
Safety:EN 61010
Descriptionofthe instrument:
RotatingDisk Electrode(RDE)witharotatingliquidHg contact,includingasystem
forcontrollingrotationalspeedofadedicatedDC motor.
Utrecht,
J.J.M. Coenen, QC Manager
Metrohm Autolab B.V.atUtrechtwill notacceptanyliabilityfordamages caused
directlyorindirectlyby connectingthisinstrumenttodevices, whichdonotmeet
relevantsafetystandards. The AUTOLABRDEwasdevelopedasalaboratory
researchinstrument.Metrohm Autolab B.V.cannotunderanycircumstancebe
heldresponsible forthe results ofthe use ofthe RDE.
Please read thismanualcarefullybefore usingtheRDEsystem.
Thismanualdescribes the RDEsystem. The sections dealwithappearanceanduse
ofthe RDEandcontainnecessaryinformation regardingoperation and
installation. Notfollowingthese instructions when usingthe RDEmay cause
The nextsections dealwithappearanceanduse ofthe moduleandcontain
necessaryinformation regardingoperation andinstallation.

SAFETY PRACTICES
General
The followingsafetypractices areintendedtoensuresafeoperation ofthe
equipment.Notfollowingthese instructions when usingthe RDEmotorcontroller
may cause unsafe operation.
Metrohm Autolab isnotliableforanydamagecausedbynotcomplyingwiththe
followinginstructions.
ElectricalHazards
·Thereareno user-serviceablepartsinside. Servicingshouldonlybedoneby
qualifiedpersonnel.
·Removalofpanelsexposes topotentiallydangerousvoltages. Always
disconnectthe controllerfrom all powersources beforeremoving
protective panels.
·Replaceblown fuses onlywithsizeandratingstipulatedon ornearthe
fuse panelholderandin the manual.
·Replaceorrepair faultyorfrayedinsulation on powercordsandmotor
cable.
·Replace motorcable onlywith the originalspare part.
·When replacingpowercord,use onlyapprovedtypeandconformlocal
regulations.
·Be surepowercordsarepluggedintothe correctvoltagesourceand
always use awall outletwith protective earth.
·Checkall connectedequipmentforpropergrounding.Do notmovethe
motorcontrollerwith powercords connected.
GeneralPrecautions
·Do notplace the controlleron an unstable surface.
·Do notexpose the controllerto damporwetconditions.
WARNING: The RDE-2mechanicalunit contains a
sealedmercurycontact.Incase ofdamagetothe
unit please handlewithcare. Do notthrow theunit
with ordinarywaste.

GENERAL SPECIFICATIONS
PowerSupply(V) RDEMotorcontroller
100..240V±10%selectablein4ranges
100:90..110V
120:108..132V
220:198..242V
240:216..264V
Powerline frequency 50-60 Hz
Powerconsumption 50 VA (max)
Fuse(A-slow-slow) 100 V–630mAT
120 V–630mAT
220 V–315mAT
240 V–315mAT
Operatingenvironment 0°Cto40°Cambienttemperaturewithoutderating
80%relative humidity
Storageenvironment -10 °Cto60 °Cambienttemperature
Dimensions(Wx HxD) 196mmx 77mmx245mm(excl. connectors)
Weight 2.8kg(controlleronly),0.5kg(rotatoronly)
Safetydesignedto EN61010
EMCcompliance EN61326-1
Warm-uptime Notapplicable
Motorspeedrange 100 ~10.000RevolutionsPerMinute(RPM)
Manualspeedsetting 100 ~10.000RPMin1RPMsteps
Remotespeedsetting Speedsetpoint:0.1~10.0Vfor100~10.000 RPM
respectively
Connection throughinsulatedBNC
connector
Core=HI-in,Shield=LO-in
Differentialinputimpedance:1MW±5%
|Vin|max =40V
Settlingtime(Remote) <200mstowithin2%ofF.S.step
(non linearoperation:motorcurrentlimited)
<40mstowithin2%of1000RPMstep
Acceleration/Deceleration Approx.4000RPM/srun/stopslope(MANUAL
CONTROL)
Pollution degree 2
Installationcategory II
Table1– Generalspecifications

Table ofContents
1– Description ..................................................................................................1
2– Installation ofthe motorcontroller..............................................................1
3– Poweringthe motorcontroller.....................................................................2
4– Installation ofthe RDErotatingmechanicalunit...........................................2
4.1– Mountingthe electrode.......................................................................2
4.2– Connectingthe RDErotatingmechanicalunit to the motorcontroller.4
4.3– Connectingthe RDEto the Autolab .....................................................4
5– Controllingthe RDE.....................................................................................6
5.1– Manualcontrolmode..........................................................................6
5.1.1– Viewingandsettingthe speedthe speedwhen the motoris off7
5.1.2– Viewingandsettingthe speedthe speedwhen the motoris
running..................................................................................................7
5.2– Remote controlmode (software controlledoperation).........................7
5.2.1– Controllingthe RDEwith the Autolab.........................................8
5.2.2– Software controlin GPES/FRA....................................................8
5.2.3– Software controlin NOVA........................................................10
6– Cleaningandinspection.............................................................................11
7– Changingandpolishingthe electrode tip...................................................12
8– RDEstorage...............................................................................................12
9– Diagnostics................................................................................................13
10 – Limitedwarranty......................................................................................14

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1– Description
The AUTOLABRDE(RotatingDiscElectrode) consistsoftherotatingmechanical
unit (RDE-2) andthe motorcontrolunit (MCUR)shown below in figure 1.
Figure1– TheAutolabRDE motorcontroller(MCUR, left) andthe rotatingmechanicalunit
(RDE-2) mountedon the electrochemicalcell (right)
2–Installation of themotor controller
Make surethatthe motorcontrolleriscorrectlyconfiguredforthe applicable
mains voltagepriortoapplyingpowertothe unit.The line fuses andmains input
range selectorare listedin the specifications (see Table 1).
The powerline voltageselectorisfactorysettothe mains voltageofthe country
ofinterest, alongwith the appropriate fuses, bydefault, before shipping.

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3– Powering themotor controller
The mains powerisappliedtothe unit by operatingthe mains switchon the rear
panel, labelled:<POWER>. When the unit is powered, the numericaldisplay on the
frontpanelwill beilluminated.The <SPEED>display on the frontpanelshould
read 0000± 4RPM.
Note: the frontpaneldisplay shows the realtime rotation rateoftherotator.If
the latteris notconnectedto the motorcontroller, the rotation rate will be 0RPM.
4–Installation of theRDErotating mechanicalunit
Afterunpacking,inspectthe unittomakesurethatthereisnodamage. The RDE
contains asealedrotatingmercurycontact.Incase anydamageisobserved,
contactyourdistributororMetrohm Autolab immediately.
4.1 –Mounting theelectrode
Table 2lists the electrode tips thatcan be usedwith the AUTOLAB RDE.
Itemcode Materialandsize
6.1204.300 Glassycarbon, 3mm
6.1204.010 Platinum, 3mm
6.1204.020 Gold, 3mm
6.1204.030 Silver, 3mm
RDE.GC50 Glassycarbon, 5mm
RDE.Pt50 Platinum, 5mm
RDE.Au50 Gold, 5mm
RDE.Ag50 Silver, 5mm
RDE.Blank Emptytip, 5mm
Table2– Overviewofthe RDE tips
Figure2shows the 5millimetertipsfrom lefttoright:RDE.Blank, RDE.Ag50,
RDE.Au50, RDE.Pt50, RDE.GC50.
Note: the RDE.Blank tipisanempty5mm diametertipinwhichany5mm sample
can be fitted(tolerance:± 0.02 mm).

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Figure2– Overviewofthe 5mmtipscompatiblewiththe AutolabRDE
Tomountthe electrodetipon the RDEshaft,press the shaftblockbutton shown
inFigure3.Thisshouldlockthe workingelectrodeshaft.Ifthe buttoncannotbe
engaged,rotatetheshaftby hand,whilepressingthe lockingbutton until it locks
aroundthe shaft.Whilepressingthe button, mountthe electrodetiponthe shaft
andturn the tipuntil it is firmlyin place.Oncethe electrode tipis attached, release
the blockingbutton. Turnthe workingelectrodeshaftgentlywithyourfingers.
The shaftshouldturnfreely.Ifit does notturnfreelymake surethatthe shaft
blockingbutton is completelyreleased.
Figure3– Overviewofthe RDE
Warning: RunningtheRDEwiththeshaftblockingbuttonnotcompletelyreleased
orwiththe workingelectrodeshaftblockedcanresult indamagetothe RDE
motor.Aforcefeedbackmechanism preventslockingofthe shaftduringthe
rotation ofthe RDEifthe lockingbutton is pressedaccidentally.
RDEtip
Shaftblockingbutton
RDEtip
Shaftblockingbutton

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4.2 –Connecting theRDErotating mechanicalunitto themotor
controller
ConnectRDE-2rotatingmechanicalunit tothe controllerunitviathe circular
multi-poleconnectorandmatingchassisconnector,labelled<MOTOR>,located
on the rearpanelofthecontrollershown inFigure4.Connectalso theBNC(2m)
cabletothe <REMOTEINPUT>andDAC164 on the PGSTATorthe V
out ofthe
µAutolab.
Figure4– Motorcontroller(back plane)
4.3 –Connecting theRDEto theAutolab
Connectthe redworkingelectrode(WE)bananaplugandsense (S)from the
AUTOLABtothe redreceptorofthe Ycableprovidedwiththe RDE,shown in
Figure 5.
Figure5– TheRDE andtheYconnectorusedtoconnecttheWE/S andGroundcablesfrom
the Autolab

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Connectthe green groundcablefrom the AUTOLABtothegreen receptorofthe
Yconnectorinordertoshieldthe metallichousingofthe rotatingmechanical
noise. Connectthe Ycabletothe topofthe RDE-2mechanicalrotatingunit (see
Figure 6).
Figure6– TheYcableconnectedtothe topoftheRDE-2mechanicalrotatingunit
Placethe RDEinyourcell.Take carenottosubmergethe entireelectrodein
solution!Figure 7showsproperpositioningofthe tipin the cell.
Note: the RDErotatingmechanicalunit mustbeplacedvertically.It is
recommendedtoallowforenoughroom aroundandbelowthe tiptoprevent
interferencetothe hydrodynamicflow. It isrecommendedtouse alargecell
volume (cell 6.1415.340orsimilar).

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Figure7– Correctposition oftheRDE inthe cell
5–Controlling theRDE
The motorcontrolleroperates in 2modes: ManualandRemote.
5.1 –Manual control mode
Torunthe unit inManualMode, the <CONTROLMODE>switchon the rearpanel
shouldbeinoutermost<MANUAL> position (noLEDglowing). Ifthe <Remote>
ledon the frontpanelisswitchedoff,then themotorspeedcanbeseton the
frontpanelusingthe <UP/DOWN>button.
The motorcanstart orstopby togglingthe <RUN/STOP>switchonthe front
panel.Pressingthe switchwhen the motorisnotrunningwill cause it to
acceleratetothe setpoint.Pressingthe switchwhen it isrunningwill cause the
motortodeceleratebackto100 RPM. When the motorisrunningthenthe front
panelalwaysdisplaystheactualspeedofthe motor.The manualspeedsetpoint

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canbealteredeitherwhen the motorisrunningorwhen the motorisstopped.
Please notethatthe manualspeedsetpointisvolatile, so apreviouslyentered
setpointbefore the unit was switchedoff the mains cannotbe recalled.
5.1.1 –Viewing andsetting thespeedthespeedwhenthemotorisoff
Immediatelyafterpowerupthe initialinternalmanualspeedsetpointofthe
controllerissetto100 RPMforthe RDEconfiguration andthe motorisswitched
off <STOP>.
When the motorisnotrunning,the speedsetpointcanbeviewedon the front
paneldisplaybypressingandreleasingthe <MANUAL> <UP>or<DOWN>front
panelswitch. The display will show the speedsetpointforapproximately3
seconds.
To change the speedsetpointcontinue holdingthe <UP>or<DOWN>switch. The
speedsetpointwill changeinstepsof1RPM. Ifyoucontinueholdingthe<UP>or
<DOWN>switchthen every4sthe stepsizewill increase by afactorof10 witha
maximumstepsizeof1000 rpm. Oncethe newspeedsetpointhasbeen entered,
the motorcanbesettorunby pressingthe <RUN/STOP>switch. Themotorwill
accelerate to the desiredsetpoint.
5.1.2 –Viewing andsetting thespeedthespeedwhenthemotorisrunning
When the motorisrunning,the actualrotationspeedisdisplayedonthe front
panel.Toincrease ordecrease the speed,press the frontswitchlabelled
<MANUAL> ineitherthe <UP>or<DOWN>position. The speedwill changein
stepsof1RPM. Ifyoucontinueholdingthe <UP>or<DOWN>switchthen every4
sthe stepsizewill increase by afactorof10 withamaximumstepsizeof1000
rpm.
5.2 –Remotecontrol mode(softwarecontrolledoperation)
The unit canbecontrolledremotelyby providingaremotespeedsetpointtothe
motorcontroller.Toenablethe unit tobecontrolledthroughthe remoteinput,
the switchon the rearpanel,labelled<CONTROLMODE>shouldbesetto
<REMOTE>(inthe <REMOTE>state, the <CONTROLMODE>switchon the rear
panelandthe <REMOTE>indicatorlighton the frontpanelare both illuminated).
The remotespeedsetpointcanbeappliedthroughthe insulatedBNCconnector
on the rearpanel,labelled<REMOTE INPUT>.Core=HI-in, Shield=LO-in. The
speedofthe motorcanbesetby applyingavoltageof+0.1V(for100 RPM) to
+10.0V(for10.000RPM) to this input.
Note: applying-2Vonthe remoteinputsetsthe rotation rateofthe RDEto0
RPM. Please notethatitisnotpossibletosetthe rotation ratetovalues between
100 and0RPM.

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Warning: Toexcludeanydeviations inremotespeedsetpointsduetothe load
impedanceofthe controller’s remoteinputplease respectthe controller’s input
impedance of1M ± 5%.
5.2.1 –Controlling theRDEwiththeAutolab
Connectthe DAC164 channel1or2inthe frontofthe AUTOLAB(orthe Vout of
the µAutolab)tothe BNCconnectoron the rearpanelofthe motorcontroller,
labelled<REMOTE INPUT>.
5.2.2 –SoftwarecontrolinGPES/FRA
Start Autolab hardwareconfiguration. Intheadditionalhardwaresection (upper
rightsection), check the RDEconnectedtoDAC option (see Figure 8).
Figure8– Selectthe RDE connectedtoDAC
Start GPESorFRAsoftware. From the UtilitiesMenuselectRDEControl.The RDE
controlwindow will be displayed(see Figure 9).

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Figure9– TheRDE controlwindow
The RDEcontrolwindow canbeusedtocontrolthe rotation rateofthe rotating
mechanicalunit.Thiscanbedone usingthe slider(fromofftoXRPM, whereXis
the maximumrotation ratedefinedinthe RDEcontrolSetup)orby typinga
rotation rateinRPMorinRad/s inthe respectiveboxes inthe RDEcontrol
window.
Clickon the Setup>> button. The RDESetupwindow will bedisplayed(see Figure
10). Inthe RPMperVolt box:Enter1000 rpm/Vinthe Maximumrotation speed
box:EnterX,whereXisthe maximumrotation rateinRPM(default:10000 RPM).
In the DAC Channel: Enterthe channelthatyouhave selected(fordetails on which
channelto use consult the AUTOLAB manual).

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Figure10 – The RDE Setup
Click<OK>.SetthemotorcontrolleronRunby togglingthe Run/Stopswitch. You
can now controlthe speedofthe RDEfrom the RDEcontrolwindow.
Notethatthe minimumRPMofthe RDEis100 rpmi.e. off intheRDEcontrol
window correspondsto100 rpm. ToswitchtheRDEcompletelypleasepress the
stopswitch on the frontpanel.
NOTE: It ispossible touse the RDEtogetherwitheitheraBIPOToranECD butnot
with both atthe same time. Referto the GPESusermanualformore information.
5.2.3 –SoftwarecontrolinNOVA
Start the NOVAsoftware. The rotation rateofthe Autolab RDEcanbecontrolled
duringanexperimentusingthe followingcommand,locatedinthe Measurement
- general groupofcommands1(see Figure 11):
1Refertothe NOVA UserManual formoreinformation (Chapter2).

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Figure11 – The controlAutolabRDE andSwitchAutolabRDE offcommandscan befoundin
the Measurement– generalgroupofcommands
·ControlAutolab RDE:thiscommandcanbeusedtosetthe rotation rateof
the Autolab RDEtoanyvaluebetween 100 and10000 RPM. The DAC
channelusedto controlrate is specified2.
·SwitchAutolab RDEoff:thiscommandswitches setsthe rotation rateto0
RPM (the DAC voltage is setto -2V).
These two commandscanbeusedincombination withanyotherNOVA
commands.
NOTE: It ispossible touse the RDEtogetherwitheitheraBIPOToranECD butnot
with both atthe same time.
NOVAincludes aready-to-use Hydrodynamiclinearsweepvoltammetryprocedure
inthe Autolab groupofprocedures. ThiscanbeusedasatemplateforNOVA
experimentsduringwhichremotecontroloftheAutolab RDEisrequired.Referto
the NOVAGettingStartedandthe NOVAUserManualformore information about
the controlofthe RDEin NOVA.
6– Cleaning and inspection
It isrecommendedtocleanthe instrumenton aregularbasis. Use adampcloth,
withamilddetergent.Neveruse excessiveamountsofwaterasitmay damage
the instrument.Asaprecaution alwaysdisconnectthe unit from the mains before
cleaning.
2Notethatchannels1and2on the frontpanelarelabeled3and4inthesoftware.

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Alwaysperformaninspection ofthe instrumentandall itsconnectingcables
beforeuse. Ifyoufindanycablewithdamagedinsulation orotherirregularities,
stopusingthe instrumentuntil it hasbeen repaired.Damagedequipmentor
damagedcables may behazardous!
7– Changing and polishing theelectrodetip
It isrecommendedfirsttoremovethe electrodetipfrom the rotatingmechanical
unit priortocleaningandpolishingthe electrodetipsusedinyourchemical
experiment.Please alwaysfollow the manufacturer’s suggestions forpolishing
yourparticularelectrode.
Toremovethe electrodetipfrom the rotatingmechanicalunit –firstturnoff the
rotator.Alwaysremembertopress the <RUN/STOP>buttonon the motor
controllerunit andbesurethe LEDisnotilluminated.<STOP>therotation
completelyotherwise damagemayresult tothe shaftblockingbutton andmaybe
even the Hg contactitself.
Second,removethe rotatorfrom the electrochemicalcell beingsuretorinse off all
solution material/salts. Dryboththe electrodeandthe axiscarefullywithasoftlab
tissue. Blockthe shaftofthe rotatingmechanicalunit by pressingthe blocking
button tolockthe RDEshaftandverygently,byhand,untwistthe RDEelectrode!
Exert no force beyondthatofyourown fingers.
WARNING: Ifthe electrodecannotberemovedby handusingthe axislocking
button, the unitmustbereturnedtoMetrohm Autolab forrepair! Usingexcessive
forceon the axismay breakthe Hg contact.Ifthe Hg contactleaks youwill have
trouble with future measurements.
8– RDEstorage
Inexperimentalconditions take carenottoexpose the axistoacorrosive
environmentforlongperiodsoftime.Between samples alwaysrinse the rotating
tipanddrythoroughlybefore continuinganalyses.
Do notstorethe RDEupsidedown. Do notstorethe RDEwithanelectrode
attached.Alwaysrinse the RDEelectrodes androtation axiswithdemineralised
water, store dryandseparatelybefore leavingforprolongedperiods.
To avoiddamage to theunit please handle with care.
WARNING: The RDErotatingmechanicalunit contains asealedmercurycontact.
Do notthrow the unit withordinarywaste. Thismercurysealmaybreakifthe unit
isdroppedorusedwithexcessiveforce. Breakingthe mercurysealwill result in
irreparable damage andthe unit will needto be replaced.

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Do notforanyreason attempttoopenthe unit.Thereareno userserviceable
parts. Failuretoconformtouserspecifications describedabovemay result inthe
voidofanywarrantyclaims.
9– Diagnostics
Problem: The controllerdoes notseemtopowerup,aftertogglingthe power
switch (frontspeeddisplay does notshow anyreadings).
Cause The controlleris notpowered
Solution Check mains connection
Check fuses
Problem: The <RUN/STOP>switch illumination keeps blinkingandthe motor
cannotbe setto <RUN>, although the controllerseems to powerupnormallyand
the setpointcan be setusingthe frontpanelcontrols.
Cause The motorassemblyis notornotproperlyconnectedto the controller
Solution Checkthe motorconnection cabletobesurethe RDErotatoris
attached
Problem: The speeddisplay doesnotshow motorspeedsunder~100 RPM,
although asetpointunder100 RPM is appliedto the remote input.
Cause Tomeetthe controller’s accuracyspecification,motorspeedsfewer
than100 RPMarenotallowed.Thereforetheremotesetpointis
internallylimitedto ~100 RPM on the low endofthe speedrange
Solution Do notattemptto setthe speeds to values under100 RPM
Problem: The motorcannotbeoperatedatthemaximumspeedof10.000 ±4
RPM, while in <MANUAL> controlmode.
Cause 1 The mains voltageprobablydoes notmeetthe lowerlimit
specification (accordingto the line setting)
Solution Check line setting(see Installation guide)
Cause 2 The motorassemblyisblockedorobstructedinanyway (under
normaloperatingconditions the motorrequirestorunfreely,without
anyadditionalmechanicalloads,exceptforsome inertiaofthe RDE
electrodetipandsome workduetoviscousfrictionoftheair or
electrolyte respectively)
Solution Make surethemotorisabletorunfreelyby ensuringthatthe motor
block pin is released
Problem: The rotation speedcannotbe setto zero in “remote mode”with the
software (GPES/FRA).

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Solution Upgrade software to release 4.9.6(orhigher)
10 –Limited warranty
The Autolab RDErotatingmechanicalunit aswell asthe Motorcontrollerdonot
containanyuserserviceableparts. Anyattempttoopen ordisassemblethe rotator
and/orthe motorcontrollerwill voidanywarranty.Please contactyourAutolab
distribitororMetrohm Autolab ifthe rotatororthe motorcontroller.
The Autolab RDErotatingmechanicalunit isintendedtobeusedwithMetrohm
Autolab certifiedelectrodetips only (see Table2). Usinguncertifiedtipswill
immediatelyvoidanywarranty.Please contactMetrohm Autolab forcustom
electrode tips requests ([e-mail]).