RDE2 manual - Metrohm Autolab
Contents
1. input the switch on the rear panel labelled lt CONTROL MODE gt should be set to lt REMOTE gt in the lt REMOTE gt state the lt CONTROL MODE gt switch on the rear panel and the lt REMOTE gt indicator light on the front panel are both illuminated The remote speed setpoint can be applied through the insulated BNC connector on the rear panel labelled lt REMOTE INPUT gt Core Hl in Shield LO in The speed of the motor can be set by applying a voltage of 0 1 V for 100 RPM to 10 0 V for 10 000 RPM to this input Note applying 2 V on the remote input sets the rotation rate of the RDE to 0 RPM Please note that it is not possible to set the rotation rate to values between 100 and O RPM 7 Page Autolab RDE User Manual 2 Metrohm Warning To exclude any deviations in remote speed set points due to the load impedance of the controller s remote input please respect the controller s input impedance of 1MQ 5 5 2 1 Controlling the RDE with the Autolab Connect the DAC164 channel 1 or 2 in the front of the AUTOLAB or the V of the uAutolab to the BNC connector on the rear panel of the motor controller labelled lt REMOTE INPUT gt 5 2 2 Software control in GPES FRA Start Autolab hardware configuration In the additional hardware section upper right section check the RDE connected to DAC option see Figure 8 Autolab hardware configuration Main module Additional modules Additional hardwa2. unit The line fuses and mains input range selector are listed in the specifications see Table 1 The power line voltage selector is factory set to the mains voltage of the country of interest along with the appropriate fuses by default before shipping 1 Page Autolab RDE User Manual 2 Metrohm 3 Powering the motor controller The mains power is applied to the unit by operating the mains switch on the rear panel labelled lt POWER gt When the unit is powered the numerical display on the front panel will be illuminated The lt SPEED gt display on the front panel should read 0000 4 RPM Note the front panel display shows the real time rotation rate of the rotator If the latter is not connected to the motor controller the rotation rate will be O RPM 4 Installation of the RDE rotating mechanical unit After unpacking inspect the unit to make sure that there is no damage The RDE contains a sealed rotating mercury contact In case any damage is observed contact your distributor or Metrohm Autolab immediately 4 1 Mounting the electrode Table 2 lists the electrode tips that can be used with the AUTOLAB RDE Item code Material and size 6 1204 300 Glassy carbon 3 mm 6 1204 010 Platinum 3 mm 6 1204 020 Gold 3mm 6 1204 030 Silver 3mm RDE GC50 Glassy carbon 5 mm RDE Pt50 Platinum 5mm RDE Au50 Gold 5mm RDE Ag50 Silver 5 mm RDE Blank Empty tip 5 mm Table 2 Overview of the RDE tips Figure 2 sho
3. 000 RPM In the DAC Channel Enter the channel that you have selected for details on which channel to use consult the AUTOLAB manual 9 Page Autolab RDE User Manual 2 Metrohm im RDE Setup RPM per volt hood Maximum rotation speed 10000 DAC channel 1 Warning Select DAC channel wih care DAC channel 1 nay be in use by the BIFOT ARRAY or ECD module Do not use these modules together with KDE control Users who wantto use the RDE in combination with the BIFOT ARRAY or ECO module e g with an RADE should contact their distributor to remove the AC Yoltammetry Hardware extension from the Autolab system see next point With the BA module the ROE or B DE can be connected without any problem ta DAC channel DAC channel 2 s normally used for 4C Yoltammetry and will therefore resultin wrong applied potentials on the potentiastat In normal cases this DAC channel is not selectable It can only be selected if there is no AL Yoltammetry Hardware extension present in the Autolab system Ask your distributor to remove this Hardware extension if you need to use this DAC channel Figure 10 The RDE Setup Click lt OK gt Set the motor controller on Run by toggling the Run Stop switch You can now control the speed of the RDE from the RDE control window Note that the minimum RPM of the RDE is 100 rpm i e off in the RDE control window corresponds to 100 rpm To switch the RDE completely please press the st
4. H OCG anal 2 4 2 Connecting the RDE rotating mechanical unit to the motor controller 4 4 3 Connecting the RDE tothe Autolab u ca 4 SIS GS RO DO WERDE Eee ee nee Esel 6 5 1 Mandal ont Oo Node eier 6 5 1 1 Viewing and setting the speed the speed when the motor is off 7 5 1 2 Viewing and setting the speed the speed when the motor is FUN 7 5 2 Remote control mode software controlled operation 7 5 2 1 Controlling the RDE with the Autolab smsen 8 5 2 2 Software control in GPES FRA usssseueesenssssnneennnnsnnnnennnennnnnn 8 5 2 3 Software control in NOW A au ea 10 6 Cleaning and INS PECUO NM ae en 11 7 Changing and polishing the electrode Ip aa 12 SRDE STOO rare o e ee Coe ere er eer ee 12 9S DIAGNOSTICS ans ne einen 13 OR Sk E E E E PPNRSERERENEDERFEERUERL EEE BETERFEALTERSERTERERTERENEREEELUFEUERIELRURFEIETRURSERPEUEN 14 2 Metrohm Autolab RDE User Manual Autolab s v 1 Description The AUTOLAB RDE Rotating Disc Electrode consists of the rotating mechanical unit RDE 2 and the motor control unit MCUR shown below in figure 1 Figure 1 The Autolab RDE motor controller MCUR left and the rotating mechanical unit RDE 2 mounted on the electrochemical cell right 2 Installation of the motor controller Make sure that the motor controller is correctly configured for the applicable mains voltage prior to applying power to the
5. Metrohm Autolab for custom electrode tips requests info metrohm autolab com 14 Page 7 2011 Kanaalweg 29 G 3526 KM Utrecht The Netherlands Metrohm Autolab s v
6. RDE2 User manual DECLARATION OF CONFORMITY We Metrohm Autolab B V Utrecht The Netherlands Certify that the product AUTOLAB RDE is in conformity with EC Directives 89 336 EEC and 73 23 EWG Standards used EMC EN 61326 1 Safety EN 61010 Description of the instrument Rotating Disk Electrode RDE with a rotating liquid Hg contact including a system for controlling rotational speed of a dedicated DC motor Utrecht J J M Coenen QC Manager Metrohm Autolab B V at Utrecht will not accept any liability for damages caused directly or indirectly by connecting this instrument to devices which do not meet relevant safety standards The AUTOLAB RDE was developed as a laboratory research instrument Metrohm Autolab B V cannot under any circumstance be held responsible for the results of the use of the RDE Please read this manual carefully before using the RDE system This manual describes the RDE system The sections deal with appearance and use of the RDE and contain necessary information regarding operation and installation Not following these instructions when using the RDE may cause The next sections deal with appearance and use of the module and contain necessary information regarding operation and installation SAFETY PRACTICES General The following safety practices are intended to ensure safe operation of the equipment Not following these instructions when using the RDE motor controller may cau
7. ercury contact Do not throw the unit with ordinary waste This mercury seal may break if the unit is dropped or used with excessive force Breaking the mercury seal will result in irreparable damage and the unit will need to be replaced 12 Page 2 Metrohm Autolab RDE User Manual Do not for any reason attempt to open the unit There are no user serviceable parts Failure to conform to user specifications described above may result in the void of any warranty claims 9 Diagnostics Problem The controller does not seem to power up after toggling the power switch front speed display does not show any readings Cause The controller is not powered Solution Check mains connection Check fuses Problem The lt RUN STOP gt switch illumination keeps blinking and the motor cannot be set to lt RUN gt although the controller seems to power up normally and the set point can be set using the front panel controls Cause The motor assembly is not or not properly connected to the controller Solution Check the motor connection cable to be sure the RDE rotator is attached Problem The speed display does not show motor speeds under 100 RPM although a set point under 100 RPM is applied to the remote input Cause To meet the controller s accuracy specification motor speeds fewer than 100 RPM are not allowed Therefore the remote set point is internally limited to 100 RPM on the low end of the speed range Solution Do not attempt to set
8. ight Safety designed to EMC compliance Warm up time Motor speed range Manual speed setting Remote speed setting Connection through insulated BNC connector Settling time Remote Acceleration Deceleration Pollution degree Installation category RDE Motor controller 100 240 V 10 selectable in 4 ranges 100 90 110 V 120 108 132 V 220 198 242 V 240 216 264V 50 60 Hz 50 VA max 100 V 630 mAT 120 V 630 mAT 220 V 315 mAT 240 V 315 mAT 0 C to 40 C ambient temperature without derating 80 relative humidity 10 C to 60 C ambient temperature 196mm x 77mm x 245mm excl connectors 2 8 kg controller only 0 5 kg rotator only EN61010 EN61326 1 Not applicable 100 10 000 Revolutions Per Minute RPM 100 10 000 RPM in 1 RPM steps Speed set point 0 1 10 0 V for 100 10 000 RPM respectively Core Hl in Shield LO in Differential input impedance 1 MQ 5 Vin max 40 V lt 200 ms to within 2 of F S step non linear operation motor current limited lt 40 ms to within 2 of 1000 RPM step 4000 RPM s MANUAL Approx slope CONTROL 2 Il run stop Table 1 General specifications Table of Contents MISS CMO COM accents EEN Ed 1 2 Installation of the motor controller aunuunnnene 1 5 Powering te motor CONTONE rana ner re Deres 2 4 Installation of the RDE rotating mechanical unit nnsseeeeennnseeeeeen 2 A l MOUNTING the ClC
9. not with both at the same time NOVA includes a ready to use Hydrodynamic linear sweep voltammetry procedure in the Autolab group of procedures This can be used as a template for NOVA experiments during which remote control of the Autolab RDE is required Refer to the NOVA Getting Started and the NOVA User Manual for more information about the control of the RDE in NOVA 6 Cleaning and inspection It is recommended to clean the instrument on a regular basis Use a damp cloth with a mild detergent Never use excessive amounts of water as it may damage the instrument As a precaution always disconnect the unit from the mains before cleaning Note that channels 1 and 2 on the front panel are labeled 3 and 4 in the software 11 Page Autolab RDE User Manual 2 Metrohm Always perform an inspection of the instrument and all its connecting cables before use If you find any cable with damaged insulation or other irregularities stop using the instrument until it has been repaired Damaged equipment or damaged cables may be hazardous 7 Changing and polishing the electrode tip It is recommended first to remove the electrode tip from the rotating mechanical unit prior to cleaning and polishing the electrode tips used in your chemical experiment Please always follow the manufacturer s suggestions for polishing your particular electrode To remove the electrode tip from the rotating mechanical unit first turn off the rotator Alwa
10. oller Connect RDE 2 rotating mechanical unit to the controller unit via the circular multi pole connector and mating chassis connector labelled lt MOTOR gt located on the rear panel of the controller shown in Figure 4 Connect also the BNC 2 m cable to the lt REMOTE INPUT gt and DAC164 on the PGSTAT or the V of the out uAutolab Figure 4 Motor controller back plane 4 3 Connecting the RDE to the Autolab Connect the red working electrode WE banana plug and sense S from the AUTOLAB to the red receptor of the Y cable provided with the RDE shown in Figure 5 AUTOLAB Figure 5 The RDE and the Y connector used to connect the WE S and Ground cables from the Autolab 4 Page 2 Metrohm Autolab RDE User Manual Autolab s v Connect the green ground cable from the AUTOLAB to the green receptor of the Y connector in order to shield the metallic housing of the rotating mechanical noise Connect the Y cable to the top of the RDE 2 mechanical rotating unit see Figure 6 as e S Figure 6 The Y cable connected to the top of the RDE 2 mechanical rotating unit Place the RDE in your cell Take care not to submerge the entire electrode in solution Figure 7 shows proper positioning of the tip in the cell Note the RDE rotating mechanical unit must be placed vertically It is recommended to allow for enough room around and below the tip to prevent interference to the hydrodynamic flow It is recommended
11. op switch on the front panel NOTE It is possible to use the RDE together with either a BIPOT or an ECD but not with both at the same time Refer to the GPES user manual for more information 5 2 3 Software control in NOVA Start the NOVA software The rotation rate of the Autolab RDE can be controlled during an experiment using the following command located in the Measurement general group of commands see Figure 11 Refer to the NOVA User Manual for more information Chapter 2 10 Page 2 Metrohm Autolab RDE User Manual Measurement general Timed procedure Autolab control set potential set current set cell Weut time 3 Optimize current range OCF determination set reference potential set BIPFOT potential set pH measurement temperature o RESET CULM 4rrequency Control Autolab ADE Switch Autolab ROE off UTE BLE Wie LA Figure 11 The control Autolab RDE and Switch Autolab RDE off commands can be found in the Measurement general group of commands e Control Autolab RDE this command can be used to set the rotation rate of the Autolab RDE to any value between 100 and 10000 RPM The DAC channel used to control rate is specified e Switch Autolab RDE off this command switches sets the rotation rate to 0 RPM the DAC voltage is set to 2 V These two commands can be used in combination with any other NOVA commands NOTE It is possible to use the RDE together with either a BIPOT or an ECD but
12. re PSTATIO Ir ECO Automatic Electrode OPGSTATIO I BIPOT BA OPGSTATI2 px PGSTAT ZO I Fl20 Integrator PGSTATS0 302 302N T Booster PGSTAT100 I SCAN GEN Hardware extensions pAutolab r ADC750 x PSA extended range CO aAutolab type Il M Fl20 Filter x AC voltammetry pAutolab type Ill C FRA modules x AC coupled inputs FRA Dynamic iR compensation Multichannel 3 C MUX CECN AD converter DA converter Line frequency C ADC 124 DAC 124 50 Hz ADC 164 DAC 164 60 Hz C Custom Calibration o o confirmation CO Calibration factor for integrator 4 Figure 8 Select the RDE connected to DAC Start GPES or FRA software From the Utilities Menu select RDE Control The RDE control window will be displayed see Figure 9 8 Page N Metrohm Autolab RDE User Manual m RDE control Setup gt gt Close Figure 9 The RDE control window The RDE control window can be used to control the rotation rate of the rotating mechanical unit This can be done using the slider from off to X RPM where X is the maximum rotation rate defined in the RDE control Setup or by typing a rotation rate in RPM or in Rad s in the respective boxes in the RDE control window Click on the Setup gt gt button The RDE Setup window will be displayed see Figure 10 In the RPM per Volt box Enter 1000 rpm V in the Maximum rotation speed box Enter X where X is the maximum rotation rate in RPM default 10
13. se unsafe operation Metrohm Autolab is not liable for any damage caused by not complying with the following instructions Electrical Hazards e There are no user serviceable parts inside Servicing should only be done by qualified personnel e Removal of panels exposes to potentially dangerous voltages Always disconnect the controller from all power sources before removing protective panels e Replace blown fuses only with size and rating stipulated on or near the fuse panel holder and in the manual e Replace or repair faulty or frayed insulation on power cords and motor cable e Replace motor cable only with the original spare part e When replacing power cord use only approved type and conform local regulations e Be sure power cords are plugged into the correct voltage source and always use a wall outlet with protective earth e Check all connected equipment for proper grounding Do not move the motor controller with power cords connected General Precautions e Do not place the controller on an unstable surface e Do not expose the controller to damp or wet conditions WARNING The RDE 2 mechanical unit contains a sealed mercury contact In case of damage to the unit please handle with care Do not throw the unit Hg with ordinary waste ay GENERAL SPECIFICATIONS Power Supply V Power line frequency Power consumption Fuse A slow slow Operating environment Storage environment Dimensions W x H x D We
14. the motor is switched off lt STOP gt When the motor is not running the speed set point can be viewed on the front panel display by pressing and releasing the lt MANUAL gt lt UP gt or lt DOWN gt front panel switch The display will show the speed set point for approximately 3 seconds To change the speed set point continue holding the lt UP gt or lt DOWN gt switch The speed setpoint will change in steps of 1 RPM If you continue holding the lt UP gt or lt DOWN gt switch then every 4 s the step size will increase by a factor of 10 with a maximum step size of 1000 rom Once the new speed set point has been entered the motor can be set to run by pressing the lt RUN STOP gt switch The motor will accelerate to the desired set point 5 1 2 Viewing and setting the speed the speed when the motor Is running When the motor is running the actual rotation speed is displayed on the front panel To increase or decrease the speed press the front switch labelled lt MANUAL gt in either the lt UP gt or lt DOWN gt position The speed will change in steps of 1 RPM If you continue holding the lt UP gt or lt DOWN gt switch then every 4 s the step size will increase by a factor of 10 with a maximum step size of 1000 rom 5 2 Remote control mode software controlled operation The unit can be controlled remotely by providing a remote speed setpoint to the motor controller To enable the unit to be controlled through the remote
15. the speeds to values under 100 RPM Problem The motor cannot be operated at the maximum speed of 10 000 4 RPM while in lt MANUAL gt control mode Cause 1 The mains voltage probably does not meet the lower limit specification according to the line setting Solution Check line setting see Installation guide Cause2 The motor assembly is blocked or obstructed in any way under normal operating conditions the motor requires to run freely without any additional mechanical loads except for some inertia of the RDE electrode tip and some work due to viscous friction of the air or electrolyte respectively Solution Make sure the motor is able to run freely by ensuring that the motor block pin is released Problem The rotation speed cannot be set to zero in remote mode with the software GPES FRA 13 Page Autolab RDE User Manual 2 Metrohm Solution Upgrade software to release 4 9 6 or higher 10 Limited warranty The Autolab RDE rotating mechanical unit as well as the Motor controller do not contain any user serviceable parts Any attempt to open or disassemble the rotator and or the motor controller will void any warranty Please contact your Autolab distribitor or Metrohm Autolab if the rotator or the motor controller The Autolab RDE rotating mechanical unit is intended to be used with Metrohm Autolab certified electrode tips only see Table 2 Using uncertified tips will immediately void any warranty Please contact
16. to use a large cell volume cell 6 1415 340 or similar 5 Page Autolab RDE User Manual 2 Metrohm Autolab s v Figure 7 Correct position of the RDE in the cell 5 Controlling the RDE The motor controller operates in 2 modes Manual and Remote 5 1 Manual control mode To run the unit in Manual Mode the lt CONTROL MODE gt switch on the rear panel should be in outermost lt MANUAL gt position no LED glowing If the lt Remote gt led on the front panel is switched off then the motor speed can be set on the front panel using the lt UP DOWN gt button The motor can start or stop by toggling the lt RUN STOP gt switch on the front panel Pressing the switch when the motor is not running will cause it to accelerate to the set point Pressing the switch when it is running will cause the motor to decelerate back to 100 RPM When the motor is running then the front panel always displays the actual speed of the motor The manual speed set point 6 Page 2 Metrohm Autolab RDE User Manual can be altered either when the motor is running or when the motor is stopped Please note that the manual speed setpoint is volatile so a previously entered setpoint before the unit was switched off the mains cannot be recalled 5 1 1 Viewing and setting the speed the speed when the motor is off Immediately after power up the initial internal manual speed setpoint of the controller is set to 100 RPM for the RDE configuration and
17. ws the 5 millimeter tips from left to right RDE Blank RDE Ag50 RDE Au50 RDE Pt50 RDE GC50 Note the RDE Blank tip is an empty 5 mm diameter tip in which any 5 mm sample can be fitted tolerance 0 02 mm 2 Page 2 Metrohm Autolab RDE User Manual Autolab s v Figure 2 Overview of the 5 mm tips compatible with the Autolab RDE To mount the electrode tip on the RDE shaft press the shaft block button shown in Figure 3 This should lock the working electrode shaft If the button cannot be engaged rotate the shaft by hand while pressing the locking button until it locks around the shaft While pressing the button mount the electrode tip on the shaft and turn the tip until it is firmly in place Once the electrode tip is attached release the blocking button Turn the working electrode shaft gently with your fingers The shaft should turn freely If it does not turn freely make sure that the shaft blocking button is completely released RDE tip Shaft blocking button Figure 3 Overview of the RDE Warning Running the RDE with the shaft blocking button not completely released or with the working electrode shaft blocked can result in damage to the RDE motor A force feedback mechanism prevents locking of the shaft during the rotation of the RDE if the locking button Is pressed accidentally 3 Page Autolab RDE User Manual L Metrohm Autolab s v 4 2 Connecting the RDE rotating mechanical unit to the motor contr
18. ys remember to press the lt RUN STOP gt button on the motor controller unit and be sure the LED is not illuminated lt STOP gt the rotation completely otherwise damage may result to the shaft blocking button and maybe even the Hg contact itself Second remove the rotator from the electrochemical cell being sure to rinse off all solution material salts Dry both the electrode and the axis carefully with a soft lab tissue Block the shaft of the rotating mechanical unit by pressing the blocking button to lock the RDE shaft and very gently by hand untwist the RDE electrode Exert no force beyond that of your own fingers WARNING If the electrode cannot be removed by hand using the axis locking button the unit must be returned to Metrohm Autolab for repair Using excessive force on the axis may break the Hg contact If the Hg contact leaks you will have trouble with future measurements 8 RDE storage In experimental conditions take care not to expose the axis to a corrosive environment for long periods of time Between samples always rinse the rotating tip and dry thoroughly before continuing analyses Do not store the RDE upside down Do not store the RDE with an electrode attached Always rinse the RDE electrodes and rotation axis with demineralised water store dry and separately before leaving for prolonged periods To avoid damage to the unit please handle with care WARNING The RDE rotating mechanical unit contains a sealed m
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