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Troubleshooting Noise in an Electrochemical System with a Rotator

DRK10039 (REV001 | JUN 2017)

Page 3

polishing the end of a brush rod with a sandpaper. First, remove the brush rod assembly from the clamshell door by

unscrewing it by hand. Then, take the brush rod out from its plastic housing, and polish the rod with a piece of

sandpaper. The sandpaper should be secured to a flat surface, and the brush rod is perpendicular to this surface

while being polished. To facilitate polishing with a defined perpendicular orientation, it may be advantageous to

hold the brush rod in a fixture, such as the chuck of a drill press. Brush contact rods should be replaced when the

carbon portion is about to be worn through. Replacement brush contacts can also be purchased.

2.4

Grounding the Rotator Motor

Electrical noise associated with the brush contacts can also be the result of electromagnetic interference from

either a nearby AC power supply or the rotator motor itself. For example, a rotator motor often emits magnetic field

into its surrounding space, and any unshielded signal line around the motor will likely pick up this noise source. The

frequency of electromagnetic noise could be the line-frequency (

𝐻𝐻𝐻𝐻

) of the AC power supply or some other

frequencies generated from the rotator motor. Motor noise can sometimes be reduced by grounding the rotator

motor case. First, to check for motor case grounding, use a multimeter to measure the resistance between the

support post of the rotator and the chassis ground (the silver post)on the front panel of the rotator control unit. The

resistance should be less than

𝑂𝑂ℎ𝑚𝑚

. Next, connect the chassis ground of the rotator control unit to the chassis

ground of the potentiostat. For the WaveDriver series potentiostats, the chassis ground is a silver post (banana

socket connector) on the back panel. The Pine Research CBP bipotentiostat chassis ground is a silver post on the

front panel beneath the electrode connections. For WaveNow series potentiostats, the chassis ground is shorted to

the DC common by default, and the DC common can be accessed through the black banana plug of the

WaveNow cell cable. Optionally, the chassis ground can be attached to an earth ground in the lab or to a large

metal conductor such as the main metal post of the rotator (see: Figure 2).

Figure 2. Schematic of Grounding the Rotator to the Potentiostat

Contact Us/Support

Please contact Pine Research Instrumentation with any of your needs including general and technical questions,

pricing/quote assistance, selection guidance, applications questions, etc. We are here to serve you. Contact us

via the means provided below.

3.1

By Phone

Our offices are located in Durham, NC in the eastern US time zone. We are available by phone Monday through

Friday from 9 AM EST to 5 PM EST. You can reach a live person by c1 (919) 782-8320.

3.2

By E-mail

Send an email to [email protected]. This is the general sales email and our team will ensure your email

is routed to the most appropriate technical support staff available. Our goal is to respond to emails within 24 hours

of receipt.

Rotator

Rotator Control Box

Potentiostat

GND

WKG REF AUX

Содержание MSR 636A

Страница 1: ...r MSR User Guide Pine Research Instrumentation Inc 2741 Campus Walk Avenue Building 100 Durham NC 27705 USA http www pineresearch com Phone 1 919 782 8320 Fax 1 919 782 8323 Copyright 2013 2017 Pine R...

Страница 2: ......

Страница 3: ...Unit Components 24 2 5 Typical Rotating Disk Electrode Design 26 2 6 Typical Rotating Ring Disk Electrode Design 27 3 Installation 28 3 1 Site Preparation 28 3 2 Unpacking and Setting Up the Rotator...

Страница 4: ...n Rate Ratio 106 6 8 Changing the Motor Stop Signal Logic 108 7 Parts and Accessories 112 7 1 Mechanical Parts and Hardware 112 7 2 Power Cords 115 7 3 Power Supplies 118 8 Troubleshooting 121 9 Stora...

Страница 5: ...gure 4 13 Connect Potentiostat to Earth Ground on Control Box Front Panel 55 Figure 4 14 Glove Box Configuration 56 Figure 4 15 Connecting the Rotation Rate Control Cable 58 Figure 6 1 Rotator Calibra...

Страница 6: ...vi DRU10002 REV 004 JAN 2017...

Страница 7: ...esearch Instrumentation provides online support for the rotator at the following URL www pineresearch com shop rotators standard msr 1 2 Copyright This publication may not be reproduced or transmitted...

Страница 8: ...d to as SUPPLIER is warranted to be free from defects in material and workmanship for a one 1 year period from the date of shipment to the original purchaser hereafter referred to as the CUSTOMER if u...

Страница 9: ...of uniquely identifying a particular instrument there is a label on the back panel of the control unit which indicates the model number and the serial number A matching serial number is also found on...

Страница 10: ...es rotation rate RPM Rate Accuracy 100 to 200 RPM accurate to within 2 counts of display reading 200 to 10 000 RPM accurate to within 1 of display reading Controls front panel 10 turn rotation rate co...

Страница 11: ...ocedure where the user must stop the procedure ARR T Dans une op ration impliquant l action ou l activit d un utilisateur cette ic ne indique une partie de l op ration o l utilisateur doit arr ter l o...

Страница 12: ...ou de mort d un individu cause de la vitesse lev e de rotation de l arbre RISK OF ELECTRICAL SHOCK Indicates information needed to prevent injury or death to a person due to electrical shock RISQUE DE...

Страница 13: ...e lectrostatique CHEMICAL INCOMPATIBILTY Indicates chemical incompatibility information needed to prevent damage to equipment INCOMPATIBILIT CHIMIQUE Indique un renseignement relatif l incompatibilit...

Страница 14: ...of the rotator More specific safety warnings are found in later sections of this document which pertain to particular operations and procedures involving the rotator Des avertissements de s curit plus...

Страница 15: ...tate the electrode shaft unless the enclosure window is secured to all four pins as shown below Use extreme caution when operating the rotator at rotation rates above 2000 RPM AVERTISSEMENT Arbre en r...

Страница 16: ...lockwise towards the zero rotation rate position before turning on the rotator ATTENTION Tournez toujours le bouton de commande de la vitesse de rotation compl tement dans le sens inverse des aiguille...

Страница 17: ...t fix e sur l arbre de l lectrode Inspectez l embout d lectrode pour vous assurer qu elle est bien fix e WARNING Do not use or attempt to rotate an electrode shaft that has been dropped bent or otherw...

Страница 18: ...ile rotating Such an electrode tip is either improperly installed or physically damaged Turn off the rotator disconnect electrical power and remove the electrode tip immediately AVERTISSEMENT N utilis...

Страница 19: ...sque vous montez ou descendez le bloc moteur le long de la barre principale veillez bien le tenir pour viter qu il ne chute brutalement et ne casse la cellule de verre situ e sous le bloc moteur CAUTI...

Страница 20: ...hazardous substance contained in all of the homogeneous materials for this part is below the limit requirements of GB T 26572 X indicates that said hazardous substance contained in at least one of the...

Страница 21: ...Cd Cr VI PBB PBDE X O O O O O X O O O O O O X O O O O SJ T 11364 O GB T 26572 X GB T 26572 wwyynn ww yy nn 01 RoHS Table 1 6 Hazardous Material Disclosure Table Chinese Tableau 1 6 Le tableau de la di...

Страница 22: ...potentiostat to control the rotation rate using a constant voltage level for steady state rotation or a more complex waveform such as a sine wave for hydrodynamically modulated voltammetry The rotator...

Страница 23: ...s the enclosure window is secured to all four pins as shown below Use extreme caution when operating the rotator at rotation rates above 2000 RPM AVERTISSEMENT Arbre en rotation Ne mettez pas le rotat...

Страница 24: ...rotating ring disk electrodes RRDEs and rotating cylinder electrodes RCEs Connections to the rotating electrode shaft are made by two pairs of silver carbon brushes For RDEs and RCEs all four brushes...

Страница 25: ...DRU10002 REV 004 JAN 2017 2 1 Major System Components The table and photo below see Figure 2 1 show the major system components Figure 2 1 Major Components of the MSR Rotator System 7 5 1 4 3 6 2 8 9...

Страница 26: ...support for cell clamps and can be installed in one of two positions 7 Enclosure Window This is a transparent window covering the front of the overall enclosure 8 Motor Control Cable This cable conne...

Страница 27: ...led from three separate panes see Figure 2 2 right Figure 2 2 Two Styles of Enclosure Window There are four hooks on the enclosure window which are secured to four anchor pins on the enclosure base Th...

Страница 28: ...l control of the rotation rate is possible by applying a voltage signal across these banana jacks see Section 4 7 3 1 2 or 4 RPM mV ratio 50K impedance 17 Rotation Rate Output Signal A voltage signal...

Страница 29: ...23 DRU10002 REV 004 JAN 2017 Figure 2 4 Control Unit Front and Back Panels 10 17 16 14 11 12 13 15 23 25 24 18 19 22 20 15 21...

Страница 30: ...disk electrodes 29 Clamshell Doors These doors open to permit access to the brush chamber 30 Door Latch Secures clamshell doors in closed position 31 Brush Contact Spring loaded silver carbon brush pr...

Страница 31: ...25 DRU10002 REV 004 JAN 2017 Figure 2 5 Motor Unit Components 27 28 29 30 31 26 29 31 35 32 33 34...

Страница 32: ...The electrode surface is typically polished to mirror smoothness 38 Threads on Shaft These threads are normally in electrical contact with disk 39 Threads inside Tip These threads are normally in ele...

Страница 33: ...ot in use 45 Ring Threads on Tip These threads contact the ring electrode 46 Disk Core on Tip This disk core is in electrical contact with the surface of the disk electrode 47 Insulating Shroud on Sha...

Страница 34: ...figures found in Section 2 of this manual Inspect the contents of the shipping carton Remove the top piece of cardboard to reveal the two smaller boxes in the carton The control unit 10 is packed ins...

Страница 35: ...m of the center post 1 with the platform facing up Tighten the knob to secure the cell platform to the center post Next slide the support collar 5 on to the center post and position it slightly above...

Страница 36: ...n Insert one banana plug stud into the red banana cable and insert the other banana plug stud into the blue banana cable These flat studs are an ideal place to make connections using alligator clips T...

Страница 37: ...le de la vitesse de rotation Attach the enclosure by hooking it on to the four pins The enclosure will rest securely on the enclosure base An appropriate power cord 10 amp rating is provided with the...

Страница 38: ...power cord is provided with the rotator Do not replace this cord with an inadequately rated cord ATTENTION Un cordon d alimentation amovible est fourni avec le rotateur Ne remplace pas ce cordon par u...

Страница 39: ...tator the upper 2 7 68 mm of the shaft is inside the motor unit while the remaining length of the shaft extends down below the motor unit The rotator accepts shafts for use with Rotating Disk Electrod...

Страница 40: ...4 1 right there are two insulating spacers The portion of the shaft between the two insulating spacers provides electrical contact with the disk electrode The lower portion of the shaft below the lowe...

Страница 41: ...lectrode l extr mit de l arbre WARNING Do not use or attempt to rotate an electrode shaft that has been dropped bent or otherwise physically damaged Inspect the shaft to be certain that it is not dam...

Страница 42: ...t loosen them by one or two turns of the hex driver Usually it is necessary to hold the motor coupling in place with one hand while loosening the screws with the other hand Note A new rotator has tape...

Страница 43: ...e shaft to make sure it is securely mounted in the motor coupling Close the clamshell doors and tighten the latch Remount the motor unit on the center post in the non inverted position CAUTION Before...

Страница 44: ...ith the rotation rate knob in the fully counterclockwise position turn on the control unit Slowly turn the rotation rate knob clockwise until the shaft rotates between 100 and 200 RPM While the shaft...

Страница 45: ...soit install de mani re incorrecte soit endommag physiquement teignez le rotateur d connectez l alimentation lectrique et retirez l arbre imm diatement If the shaft is rotating properly along the axi...

Страница 46: ...ally damaged Inspect the shaft to be certain that it is not damaged AVERTISSEMENT N utilisez pas et ne tentez pas de mettre en rotation un arbre d lectrode qui est tomb a t tordu ou a t endommag physi...

Страница 47: ...the other hand to gently turn the tip Remove the old tip from the shaft by gently unscrewing the tip by hand No tools are required to remove a tip from a shaft CAUTION Do not use tools on the shaft o...

Страница 48: ...ontrol unit WARNING Do not turn on the rotator or rotate the electrode shaft if the shaft is not securely mounted in the motor coupling Inspect the shaft to be certain that it is securely mounted AVER...

Страница 49: ...tion Ce embout d lectrode est soit install e de mani re incorrecte soit endommag e physiquement teignez le rotateur d connectez l alimentation lectrique et retirez l embout d lectrode imm diatement No...

Страница 50: ...N When raising or lowering the motor unit along the main support rod be sure to hold the motor unit carefully so that it does not unexpectedly fall and break the glass cell located below the motor uni...

Страница 51: ...nst the walls of the opening Damage will occur if the rotating shaft or tip abrades against these walls ATTENTION Centrez l lectrode rotative dans l ouverture de la cellule pour qu elle ne frotte pas...

Страница 52: ...qu indiqu ci dessous Soyez extr mement prudent lorsque vous utilisez le rotateur des vitesses de rotation sup rieures 2000 tr min Figure 4 6 Enclosure Properly Mounted on All Four Pins Figure 4 6 Bo...

Страница 53: ...ce electrode cable is color coded as white and the counter electrode cable is color coded as green Many commercially available reference electrodes have a sturdy pin connector on the top end which can...

Страница 54: ...haft see Figure 4 8 The upper pair of brush contacts red is used to make electrical contact with a rotating disk electrode RDE or a rotating cylinder electrode RCE To make good contact on opposite sid...

Страница 55: ...tor brushes see Figure 4 8 Note Older Pine bipotentiostats use only one cable connection for both the drive and the sense signals This connection is marked with a YELLOW banana jack on the bipotentios...

Страница 56: ...tentiostat is required when working with a rotating ring disk electrode A bipotentiostat provides independent control of two different working electrodes in the same electrochemical cell Note Cell cab...

Страница 57: ...anana plugs then these plugs can simply be inserted directly into either end of the jumper cable If the cell cables from the potentiostat terminate with alligator clips then the easiest way to connect...

Страница 58: ...r receptacle for the local power system The power system infrastructure for a laboratory building usually has a long metal probe buried in the earth and the third prong in the building wiring is conne...

Страница 59: ...n contact with the chassis of the control unit The chassis of the control unit is in turn in contact with earth ground via the third prong on the power cord thus the motor unit chassis is also earth g...

Страница 60: ...ats offer either a chassis terminal connection or a signal ground DC Common connection Some potentiostats offer both options and if this is the case only one of the two options should be used at a tim...

Страница 61: ...ol unit the potentiostat no longer floats with respect to earth ground If the potentiostat does not offer a chassis terminal connection or if earth grounding the chassis terminal is not an option then...

Страница 62: ...the wear rate of the brush contacts it is recommended that four special low humidity brushes sold separately be installed prior to placing the rotator in the glove box Contact Pine for more details C...

Страница 63: ...e fully counterclockwise position The fully counterclockwise position corresponds to the slowest rotation rate and it is always safest to turn on the rotator with the knob in this position 4 7 1 Manua...

Страница 64: ...ontrol Cable A special cable is available to connect Pine potentiostats to the MSR rotator see Figure 4 15 One line of this cable carries an analog rate control signal from the potentiostat to the INP...

Страница 65: ...y be either active HIGH or active LOW For the Pine MSR rotator the MOTOR STOP is configured at the factory to use active HIGH logic If desired a jumper setting inside the control box can be configured...

Страница 66: ...he circuit breaker trips then it can be reset by turning the power switch to the full off position and then turning the switch back on again A secondary circuit breaker on the front panel protects the...

Страница 67: ...ped bent or otherwise physically damaged Inspect the shaft to be certain that it is not damaged AVERTISSEMENT N utilisez pas et ne tentez pas de mettre en rotation un arbre d lectrode qui est tomb a t...

Страница 68: ...Turn off the rotator disconnect electrical power and remove the electrode tip immediately AVERTISSEMENT N utilisez pas un embout d lectrode qui semble osciller vibrer ou d vier de l axe de rotation pe...

Страница 69: ...ids to seep into the joint between the shaft and tip ATTENTION Positionnez le bloc moteur en fonction de la position de la cellule de verre de telle sorte que l embout d lectrode soit immerg e sur env...

Страница 70: ...ote After each use of rotating electrode or electrode tip clean and dry the electrode and then return it to the plastic storage box in which it was originally shipped Note A polishing kit is available...

Страница 71: ...Specifically this shaft is compatible with E3 E4TQ Series RDE tips and with classic 12 mm OD rotating cylinder electrode tips A bearing assembly for mounting this shaft in a 24 25 ground glass joint...

Страница 72: ...for 15 mm OD RCE shaft AC01TPA6M Precision Gas Purged Bearing Assembly 15 mm ID This gas purged bearing assembly fits into the 24 25 center port on an electrochemical cell A small plastic hose barb on...

Страница 73: ...e from PTFE and the internal diameter of the opening in the stainless steel bearing is 6 35 mm This 6 35 mm ID opening is compatible with the standard RDE and RCE shaft part number AFE3M and with E2 S...

Страница 74: ...to concentrated acids Part numbers for these E3 Series RDE tips and compatible shafts are listed below If the part number for an item is not listed contact Pine for more details Shafts RDE Tips precio...

Страница 75: ...below If the part number for an item is not listed contact Pine for more details Shafts RDE Tips precious metals Standard RDE Shaft AFE3M gold Au AFE3T050AU platinum Pt AFE3T050PT RDE Tips carbon mate...

Страница 76: ...E tips AFE3M ChangeDisk RDE tip 12 mm OD PTFE shroud for 5 mm OD x 4 mm thick disks AFE4TQ050 Toolkit for removing and polishing disk inserts AFE4K050 Disk Inserts carbon materials Disk Inserts precio...

Страница 77: ...ible shafts are listed below If the part number for a particular item is not listed contact Pine for more details Shafts RDE Tips precious metals Precision RDE RRDE Shaft AFE6MB gold Au AFE5T050AUPK p...

Страница 78: ...a part number is not listed contact Pine for more details Shafts RDE Tips precious metals Precision RDE RRDE Shaft AFE6MB gold Au AFE5T050AU platinum Pt AFE5T050PT RDE Tips carbon materials palladium...

Страница 79: ...om 10 C to 80 C AFE6TQ050 ChangeDisk RDE tip 15 mm OD PTFE shroud for use from 15 C to 25 C AFE5TQ050 Precision RDE RRDE Shaft for 15 mm OD tips AFE6MB Toolkit for removing and polishing disk inserts...

Страница 80: ...4 6 OPERATING TEMPERATURE RANGE 10 C to 80 C Do not use this electrode outside the operating temperature range Part numbers for single piece RDEs are listed below If the part number for a particular e...

Страница 81: ...e en rotation voir figure 4 6 OPERATING TEMPERATURE RANGE 15 C to 25 C Do not use this electrode outside the operating temperature range Part numbers for single piece RDEs are listed below If the part...

Страница 82: ...ing Assemblies Shafts and Tools platinum PTFE shroud AFE6R1PT Precision RDE RRDE shaft AFE6MB gold PTFE shroud AFE6R1AU Toolkit disk removal polishing AFE6K050 glassy carbon PTFE shroud AFE6R1GC Disk...

Страница 83: ...K shroud AFE6R1PTPK Precision RDE RRDE shaft AFE6MB gold PEEK shroud AFE6R1AUPK Toolkit disk removal polishing AFE6K050 glassy carbon PEEK shroud AFE6R1GCPK Disk Inserts carbon materials Disk Inserts...

Страница 84: ...se de rotation maximum OPERATING TEMPERATURE RANGE 10 C to 80 C Do not use this electrode outside the operating temperature range CHEMICAL INCOMPATIBILTY Shrouds fabricated from PEEK may be discolored...

Страница 85: ...15 C to 25 C Do not use this electrode outside the operating temperature range Part numbers for RRDE tips and shafts are listed below If the part number for a particular item or electode material is n...

Страница 86: ...the cell and other accessories The RCE shaft accepts standard cylinder samples 15 mm OD x 6 3 mm tall fabricated from carbon steel or various stainless steels Contact Pine for more details about this...

Страница 87: ...or stainless steel Other materials are available on request The 12 mm OD RCE tips fit on to a standard RCE RDE shaft part number AFE3M Contact Pine for details CAUTION Maximum Rotation Rate 2000 RPM D...

Страница 88: ...otating shaft A thin film on the shaft actually improves the contact between the brush and the shaft This film does not need to be cleaned off of the shaft unless the film is rough or bumpy 6 2 Brush...

Страница 89: ...Remove the entire brush assembly from the rotator by unscrewing it as shown below It should be possible to remove the brush assembly by hand Use the small hex key to remove the set screw Note that the...

Страница 90: ...o the brush holder Be careful to properly align the set screw hole with the slot on the side of the brush holder While squeezing the new brush into the brush holder use the hex key to reinstall the se...

Страница 91: ...onal wear actually improves the electrical contact between the brush and the shaft 6 2 2 Complete Brush Assembly Replacement In the event that the main body of the brush assembly is damaged it may be...

Страница 92: ...n period wears a concave groove into the new brush This intentional wear actually improves the electrical contact between the brush and the shaft 6 3 Lower Bearing Replacement The lower bearing assemb...

Страница 93: ...les from the brush banana jacks red and blue Use a flathead screwdriver to loosen the four screws that secure the lower bearing assembly to the motor unit As you are loosening the final screw with one...

Страница 94: ...inuing with this procedure AVERTISSEMENT Arbre en rotation Danger d enchev trement teignez le rotateur et d branchez le cordon d alimentation de la source d alimentation avant de poursuivre cette proc...

Страница 95: ...he internal cable assembly where two white connectors are joined together By disconnecting the cable assembly at this junction it is possible to remove the cowling completely Disconnect the junction b...

Страница 96: ...are connected to the tachometer and the white positive and green negative lines are connected to the motor There are four screws which hold the motor in place Using a flathead screwdriver loosen and...

Страница 97: ...embly may be installed CAUTION After installing a new motor it is necessary to recalibrate the rotation rate using an optical tachometer see Section 6 6 ATTENTION Apr s l installation d un nouveau mot...

Страница 98: ...the motor control cable from the top of the motor unit Disconnect any signal cables from the brush banana jacks red and blue Examine the new motor coupling unit There should be one cable tie securing...

Страница 99: ...ure the motor and chamber to the support using four screws Connect the internal cable within the cowling to the motor by joining the two white connectors together Replace the cowling on top of the mot...

Страница 100: ...the cable and several conductors are grouped together see Table 6 1 The HD 15 connector on top of the motor unit connects internally with the motor wiring harness which has four colored signal wires s...

Страница 101: ...04 JAN 2017 Figure 6 1 Rotator Calibration Toolkit including simple handheld tachometer Figure 6 2 Professional Optical Tachometer with Traceable Calibration Figure 6 3 Use of Optical Tachometer with...

Страница 102: ...tachometer reads the rotation rate when it is pointed at a rotating shaft equipped with a reflective target see Figure 6 3 The MSR Calibration Kit includes a shaft suitable for use as a target Altern...

Страница 103: ...S AWAY FROM THE POWER ENTRY MODULE AND THE TWO POWER SUPPLY MODULES DANGER Haute Tension Risque de d charge lectrique Cette proc dure doit tre confi es un lectricien ou un technicien qualifi Cette pro...

Страница 104: ...disposer d une mise la terre appropri e lorsque vous manipulez des composants sensibles en portant un ruban de mise la terre Note When performing a traceable rotation rate calibration verify the date...

Страница 105: ...er is switched off install the tachometer target into the motor coupling on the motor unit This target should be a metal rod with the appropriate diameter 1 4 or 6 35 mm Many tachometers require that...

Страница 106: ...tion rate knob on the front panel until the tachometer indicates a rotation rate of approximately 2800 RPM WAITING PERIOD Allow the rotator to rotate at 2800 RPM for one 1 hour before continuing with...

Страница 107: ...ion rate control knob very slowly until the motor comes to a complete stop Adjust trimmer P7 until the rotation rate display on the front panel reads 0000 1 Connect the red lead of the digital voltmet...

Страница 108: ...RPM If JP2 is set for 2 RPM mV the display should read 2000 RPM 1 RPM If JP2 is set for 4 RPM mV the display should read 4000 RPM 1 RPM Adjust P5 until the rotation rate display on the front panel is...

Страница 109: ...tion rates at or above 10000 RPM Before continuing verify each of the following points Verify that the shaft has been removed from the rotator Verify that the hex screws in the motor coupling are tigh...

Страница 110: ...ntrol unit should read approximately 10050 RPM Adjust trimmer P4 until the rotation rate display on the front panel of the control unit reads 10050 RPM 10 RPM Turn the rotation rate knob fully counter...

Страница 111: ...0 1000 1000 10 0 2000 2000 20 0 5000 5000 50 0 Control Unit Input Signal Calibration Input Signal volts Expected Rotation Rate RPM Tachometer Reading RPM Control Unit Display Reading 0 100 100 2 0 0...

Страница 112: ...of 1 0 RPM mV because this ratio is compatible with Pine potentiostat systems WARNING Risk of electric shock Disconnect all power before servicing the rotator AVERTISSEMENT Risque de d charge lectriq...

Страница 113: ...the configuration pins with the designation JP2 There is a small jumper that can be used to short together one of three pairs of pins Place the jumper across one of the three pairs of pins at JP2 Cho...

Страница 114: ...r stop signal usually originates from a potentiostat that is controlling the rotator A cable from the potentiostat applies the signal to the Motor Stop banana jack blue on the back panel This signal i...

Страница 115: ...the choice for the Motor Stop signal logic is selected to match the control signal provided by a particular potentiostat When shipped from the factory the MSR rotator is pre configured with active HIG...

Страница 116: ...unit Loosen the screw that secures the main analog board to the front panel and then carefully remove the analog board On the board locate the configuration pins with the designation JP1 There is a sm...

Страница 117: ...tiostat being used with the rotator Active LOW Position Active HIGH Position Reinstall the board in the control unit and secure the board to the front panel Replace the cover on the control unit At th...

Страница 118: ...na jack and a spring loaded brush contact already mounted in the assembly Description Part Number Standard Brush Kit ACAR063RM Low Humidity Brush Kit ACAR063RMLHM Description Part Number Brush Assembl...

Страница 119: ...ption Part Number Stainless Steel Bearing Assembly ACMR3301X Description Part Number Complete Enclosure Kit AFMSRCE ENCL Three Pane Enclosure Window ACMRN05 Flask Support Post 5 8 OD AC01MSRD Three Pr...

Страница 120: ...escription Part Number Cell Platform ACPR103 Description Part Number Motor Control Cable EWC15DSUB Rotation Rate Calibration Kit This kit contains a handheld tachometer trimmer adjustment tool and a s...

Страница 121: ...elow This cord is for use in the USA Canada Mexico Brazil Columbia Korea Mexico Saudi Arabia and Taiwan This cord is for use in continental Europe Russia and Indonesia Description Part Number Power Co...

Страница 122: ...IL This cord is for use exclusively in Japan This cord is for use exclusively in Argentina Description Part Number Power Cord Japan EWM18B8JP Description Part Number Power Cord Argentina EWM18B8AR Thi...

Страница 123: ...EV 004 JAN 2017 This cord is for use exclusively in Switzerland Description Part Number Power Cord Switzerland EWM18B8CH This cord is for use exclusively in Italy Description Part Number Power Cord It...

Страница 124: ...and Internal Power Supplies WARNING Risk of electric shock Disconnect power before servicing the control unit The shaded region in Figure 7 2 above shows the location of the high voltage power entry...

Страница 125: ...ambda Later rotators after October 2014 use power supplies manufactured by XP Power Depending upon when the rotator was manufactured choose the appropriate replacement part shown below Power Supplies...

Страница 126: ...e proc der l entretien du rotateur WARNING Rotating shaft Entanglement hazard Turn off the power to the rotator and disconnect the power cord from the power source before continuing with this procedur...

Страница 127: ...h ends of this cable must be secured using the two screws on each connector The rotation rate knob may be set to full counterclockwise position If this is the case then rotate the knob clockwise to in...

Страница 128: ...cularly viscous liquid if the shaft is rubbing against something or if an applied periodic waveform controlling the rotation rate has too great an amplitude or frequency This breaker thermal type is s...

Страница 129: ...at and rotator are located as far as possible from hotplates ovens video monitors computers network hubs wireless devices or cellular telephones Electrical Noise in Voltammograms grounding issues see...

Страница 130: ...h impedance at the reference electrode is often caused by a plugged frit which impedes current between the inner chamber of the reference electrode and the main test solution High impedance may also b...

Страница 131: ...stored in the original packaging material to prevent damage It should be stored at temperatures between 17 C and 37 C and at humidity levels less than 95 non condensing Retain the original packing mat...

Страница 132: ...n an unstirred solution is generally negligible On longer timescales however even unstirred solutions are prone to convective interference from thermal gradients and subtle environmental vibrations Fo...

Страница 133: ...is direction is said to be a cathodic current The general form of a reduction half reaction occurring at an electrode may be written as follows O n e R where R represents the reduced form of the molec...

Страница 134: ...entrations of the dissolved molecules or ions in the oxidized and reduced forms respectively at the surface of the electrode Note that any liquid or solid phase materials at the electrode surface such...

Страница 135: ...s potential there is little or no current because there is nothing to oxidize the molecule or ion is already oxidized and the potential is not yet negative enough to cause any appreciable reduction of...

Страница 136: ...y the reduced form R of the molecule or ion being studied The rotating electrode is initially poised at a potential that is about 200 mV more negative than the standard potential At this potential the...

Страница 137: ...plot positive anodic oxidizing potentials toward the right while others plot negative cathodic reducing potential toward the right as per classical polarography tradition Furthermore some researchers...

Страница 138: ...132 Figure 10 3 A Voltammogram is a Plot of Current versus Potential The North American Convention The European Convention Figure 10 4 Two Popular Voltammogram Plotting Conventions...

Страница 139: ...nsport limited current In actual real world experiments the wave may be observed on top of a background current and furthermore the background current may be slightly sloped see Figure 10 5 This undes...

Страница 140: ...re 10 5 right Figure 10 5 Sloping Backgrounds in Voltammograms Figure 10 6 Voltammogram for a Solution Containing Both O and R Finally it should be noted that when the oxidized form O and the reduced...

Страница 141: ...lk solution to the electrode surface While the bulk solution far away from the electrode remains well stirred by the convection induced by rotation the portion of the solution nearer to the electrode...

Страница 142: ...ion coefficient D of the oxidized form and the angular rotation rate Alternatively when the solution initially contains only the reduced form the Levich equation for the anodic limiting current iLA ca...

Страница 143: ...led voltammograms will be sigmoidal regardless of the rotation rate This means that the current observed at any given potential along the voltammogram will vary linearly with the square root of the ro...

Страница 144: ...transport Figure 10 9 Koutecky Levich Study Voltammograms with Sluggish Kinetics 10 4 2 Koutecky Levich Analysis When the rate of a half reaction occurring at an electrode surface is limited by a comb...

Страница 145: ...p is evident see Figure 10 9 right when these sampled currents are plotted on a Koutecky Levich Plot For the set of currents sampled on the limiting current plateau red circles an extrapolation back t...

Страница 146: ...placed the new technique on a firm theoretical foundation Albery returned to Oxford and working with his student Michael Hitchman drew these theoretical papers together in a seminal volume titled Rin...

Страница 147: ...nal quantities are defined in terms of the normalized diameters as follows 1 3 ID A 3 3 ID OD B B A C If a complex function G x is defined as follows 3 1 2 arctan 2 3 1 1 ln 4 3 4 1 3 1 3 3 1 x x x x...

Страница 148: ...to the reduction of ferricyanide to ferrocyanide at the disk 4 6 3 6 CN Fe e CN Fe reduction of ferricyanide to ferrocyanide at disk As ferricyanide is reduced at the disk electrode the ferrocyanide...

Страница 149: ...K is a measure of how much X is being generated at the disk electrode At the same time the ring electrode is poised at a more positive potential where X is oxidized back to A and the anodic limiting c...

Страница 150: ...As long as one of these pathways leads to an electrochemically active chemical species that can be detected at the ring it is possible to determine which decay pathway is favored Consider the followi...

Страница 151: ...of reasons including the fact that peroxide can damage various polymer membrane materials found in a fuel cell Further details on how to use an RRDE generator collector experiment to distinguish betw...

Страница 152: ...ley Sons New York 2000 Chapter 9 3 DC Johnson SG Weber AM Bond RM Wightman RE Shoup and IS Krull Electroanalytical voltammetry in flowing solutions Analytica Chimica Acta 180 1986 187 250 4 H Gunasing...

Страница 153: ...Napp Ring disc electrodes Part 3 Current voltage curves at the ring electrode with simultaneous currents at the disc electrode Trans Faraday Soc 62 1966 1932 1937 25 WJ Albery S Bruckenstein and DC Jo...

Страница 154: ...nd FC Walsh Enhanced Mass Transfer at the Rotating Cylinder Electrode I Characterization of a Smooth Cylinder and Roughness Development in Solutions of Constant Concentration J Appl Electrochem 14 198...

Страница 155: ...DC Silverman The Rotating Cylinder Electrode for Velocity Sensitive Corrosion A Review Corrosion 60 2004 1003 63 DC Silverman Technical Note Conditions for Similarity of Mass Transfer Coefficients and...

Страница 156: ...r of about 4 mm which can be inserted into a matching banana jack Banana Jack Female banana connector Banana Plug Male banana connector BNC Connector The BNC Bayonet Neill Concelman connector is a ver...

Страница 157: ...rotating ring disk electrode where the ring potential is held constant while the disk potential is swept slowly between two limits Convection Convection is the movement of molecules or ions through a...

Страница 158: ...of mass transport This thin layer is known as the diffusion layer The diffusion layer should not be confused with the stagnant layer The diffusion layer exists entirely within the thicker stagnant la...

Страница 159: ...Laminar Flow Laminar flow sometimes known as streamline flow occurs when a fluid flows in parallel layers with no disruption between the layers Levich Equation The Levich equation describes the mass t...

Страница 160: ...ymer often used as an insulating shroud for an electrode PCTFE is an abbreviation for polychlorotrifluoroethylene PEEK A chemically inert polymer often used as an insulating shroud for an electrode PE...

Страница 161: ...s layer of solution is known as the stagnant layer or in the context of fluid dynamics the stagnant layer is more properly called the hydrodynamic layer Mass transport across the stagnant layer occurs...

Страница 162: ...k potential is swept slowly between two limits and the ring potential is swept in the same manner as the disk potential but with a constant offset between the ring and disk potentials Working Electrod...

Страница 163: ...65 EU The Restriction of Hazardous Substances Directive Conformity is shown by compliance with the applicable requirements of the following documents Reference and Date Title EN 61326 1 2013 EMC Requ...

Страница 164: ...the Pine WaveNow or WaveDriver potentiostats to the MSR Control Unit to allow automated control software control of the rotation rate 2 Overview The MSR Rotator consists of the motor assembly and the...

Страница 165: ...he menu bar of AfterMath a new AfterMath instrument license may be required to enable Rotator methods If the rotator was purchased after the potentiostat was purchased a Rotator methods capable licens...

Страница 166: ...d of the dual banana jack has a small black tab labeled with the letters GND on it Make certain the jacks are installed with the correct orientation into the banana ports Figure 3 Connection of the Ro...

Страница 167: ...n colored block receptacle on the Pine potentiostat Compatible Pine potentiostats are shipped with a blank three block connector installed into the block receptacle First remove the blank connector by...

Страница 168: ...onversion ratio of1 mV RPM Other rotator systems maybe set for a different conversion ratio such as 2 mV RPM or 4 mV RPM Consult with the rotators User Guide for a full description of conversion ratio...

Страница 169: ...n our website https www pineresearch com shop knowledgebase 2 Brush Replacement Options The brushes contact the rotating shaft slowly wearing during normal use and periodically the brushes must be rep...

Страница 170: ...ing Out Right Use the small hex key to remove the set screw Note that the required hex key 0 035 is included with the brush replacement kit see Figure 3 3 Figure 3 3 Removal of the Brush Set Screw INF...

Страница 171: ...y Brush Housing Left and the Removal of New Set Screw Right INFO The set screw should protrude slightly into the slot and the brush should be free to travel to the extent permitted by the width of the...

Страница 172: ...ay be necessary to replace the entire brush assembly DISCONNECT POWER Before replacing a brush turn off the power to the rotator and disconnect the power cord from the power source Remove the entire b...

Страница 173: ...eriod wears a concave groove into the new brush This intentional wear actually improves the electrical contact between the brush and the shaft 5 Support If you have any questions about the MSR Rotator...

Страница 174: ...thereby creating high impedance and noise Bubbles inside the fritted tube are most commonly introduced by the pipetting tool used to place electrolyte within the tube Bubbles on the exterior of the fr...

Страница 175: ...d BNC cables terminated with banana plug to BNC female adapters The shield or the ground line of a shielded cable for the working or the counter electrode can be connected to the chassis ground a silv...

Страница 176: ...he support post of the rotator and the chassis ground the silver post on the front panel of the rotator control unit The resistance should be less than 1 Next connect the chassis ground of the rotator...

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