Pine Research MSR Series User manual

DRU10002 (REV 004 / JAN 2017)
Modulated Speed Rotator (MSR)
User Guide
Pine Research Instrumentation, Inc.
2741 Campus Walk Avenue, Building 100
Durham, NC 27705
USA
http://www.pineresearch.com
Phone: [phone] Fax: [phone]
Copyright © 2013-2017 Pine Research Instrumentation, Inc. All Rights Reserved.

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DRU10002 (REV 004 / JAN 2017)
Table of Contents
1Preface 1
1.1 Scope 1
1.2 Copyright 1
1.3 Trademarks 1
1.4 Use Limitation 1
1.5 Service and Warranty Information 2
1.6 Instrument Markings 3
1.6.1 Certifications and Listings 3
1.6.2 Serial Number 3
1.6.3 Model Numbers 3
1.7 Specifications 4
1.8 Icons (Icônes) 5
1.9 Safety Labels (Étiquettes de sécurité) 8
1.10 General Safety Warnings (Avertissements de sécurité généraux) 8
1.11 Hazardous Material Disclosures 14
2Description 16
2.1 Major System Components 19
2.2 Enclosure Variations 21
2.3 Control Unit Components 22
2.4 Motor Unit Components 24
2.5 Typical Rotating Disk Electrode Design 26
2.6 Typical Rotating Ring-Disk Electrode Design 27
3Installation 28
3.1 Site Preparation 28
3.2 Unpacking and Setting Up the Rotator 28
4Operation 33
4.1 The Rotating Shaft 33
4.1.1 Installing a Shaft 35
4.1.2 Changing the Tip on a Shaft 40
4.2 Mounting the Cell 44
4.3 The Enclosure 46
4.4 Cell Connections 47
4.4.1 RDE and RCE Wiring 48
4.4.2 RRDE Wiring 49
4.4.3 Routing Cables and Tubing 51
4.5 Proper Grounding 52
4.5.1 Terminology 52
4.5.2 The Earth Ground Connection 52
4.5.3 A Typical Grounding Strategy 53
4.6 Using the Rotator in a Glove Box 56
4.7 Rotation Rate Control 57
4.7.1 Manual Control of Rotation 57
4.7.2 Monitoring the Rotation Rate 57
4.7.3 External Control of the Rotation Rate 58

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DRU10002 (REV 004 / JAN 2017)
4.7.4 External Motor Stop Control 59
4.8 Circuit Protection 60
5Electrodes 61
5.1 Electrode Handling Precautions 61
5.2 Shafts 65
5.3 RDE Tips 68
5.4 Single-Piece RDE Designs 74
5.5 RRDE Tips 76
5.6 15 mm OD RCE Tips 80
5.7 12 mm OD RCE Tips 81
6Maintenance 82
6.1 Routine Cleaning 82
6.2 Brush Replacement 82
6.2.1 Internal Brush Replacement 82
6.2.2 Complete Brush Assembly Replacement 85
6.3 Lower Bearing Replacement 86
6.4 Removing the Motor-Coupling Assembly 87
6.5 Installing a New Motor-Coupling Assembly 91
Motor Control Cable Wiring 94
6.6 Rotation Rate Calibration 96
6.7 Changing the Input Rotation Rate Ratio 106
6.8 Changing the Motor Stop Signal Logic 108
7Parts and Accessories 112
7.1 Mechanical Parts and Hardware 112
7.2 Power Cords 115
7.3 Power Supplies 118
8Troubleshooting 121
9Storage and Shipment 125
10 Theory 126
10.1 Forced Convection 126
10.2 Half Reactions 127
10.3 Voltammetry 128
10.3.1 Voltammogram Plotting Conventions 131
10.3.2 Measuring Limiting Currents 133
10.4 Rotating Disk Electrode (RDE) Theory 135
10.4.1 Levich Study 136
10.4.2 Koutecky-Levich Analysis 138
10.5 Rotating Ring-Disk Electrode (RRDE) Theory 140
10.5.1 Theoretical Computation of the Collection Efficiency 140
10.5.2 Empirical Measurement of the Collection Efficiency 142
10.5.3 Generator/Collector Experiments 143
10.5.4 Comparing Two Competing Pathways 144
10.6 Rotating Cylinder Electrode (RCE) Theory 145
10.7 References 146
11 Glossary 150

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DRU10002 (REV 004 / JAN 2017)
Table of Figures
Figure 2.1: Major Components of the MSR Rotator System ..............................................19
Figure 2.2: Two Styles of Enclosure Window......................................................................... 21
Figure 2.3: Three Styles of Anchor Pins .................................................................................. 21
Figure 2.4: Control Unit Front and Back Panels ................................................................... 23
Figure 2.5: Motor Unit Components ......................................................................................25
Figure 2.6: Typical Rotating Disk Electrode (RDE) Tip with Shaft....................................... 26
Figure 2.7: Typical Rotating Ring-Disk Electrode (RRDE) Tip with Shaft ...........................27
Figure 4.1: Contact Areas at Top of Rotating Electrode Shafts ....................................... 33
Figure 4.2: The Brush Chamber (side view) .......................................................................... 34
Figure 4.3: Proper (left) and Improper (right) Shaft Insertion Positions ............................ 38
Figure 4.4: Installing a Tip on to a Shaft ................................................................................ 39
Figure 4.5: Properly Supported and Clamped Electrochemical Cells............................43
Figure 4.6: Enclosure Properly Mounted on All Four Pins ................................................... 46
Figure 4.7: Connection of Counter and Reference Electrodes....................................... 47
Figure 4.8: Brush Connections for a Rotating Disk Electrode (RDE) or a Rotating
Cylinder Electrode (RCE) ..................................................................................... 48
Figure 4.9: Brush Connections for a Rotating Ring-Disk Electrode (RRDE)...................... 50
Figure 4.10: Stackable Banana Connector with Optional Stud Connector.................... 51
Figure 4.11: Routing Cables out of the Enclosure................................................................. 51
Figure 4.12: Connect Metal Objects to Earth Ground on Control Box Front Panel........ 54
Figure 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 Calibration Toolkit (including simple handheld tachometer) ........ 95
Figure 6.2: Professional Optical Tachometer with Traceable Calibration...................... 95
Figure 6.3: Use of Optical Tachometer with Reflective Target......................................... 95
Figure 7.1: Standard C18 Connection on Power Entry Module .....................................115
Figure 7.2: Location of High Voltage Power Entry and Internal Power Supplies .........118
Figure 7.3: Replacement Internal Power Supplies ............................................................119
Figure 10.1: Response to a Potential Sweep (Cathodic) from a Solution Initially
Containing only the Oxidized Form (O) with no Reduced Form (R)..........130
Figure 10.2: Response to a Potential Sweep (Anodic) from a Solution Initially
Containing only the Reduced Form (R) with no Oxidized Form (O)..........131
Figure 10.3: A Voltammogram is a Plot of Current versus Potential ................................132
Figure 10.4: Two Popular Voltammogram Plotting Conventions .....................................132
Figure 10.5: Sloping Backgrounds in Voltammograms ......................................................134
Figure 10.6: Voltammogram for a Solution Containing Both Oand R............................134
Figure 10.7: Levich Study –Voltammograms at Various Rotation Rates ........................137
Figure 10.8: Levich Study –Limiting Current versus Rotation Rate ...................................137
Figure 10.9: Koutecky Levich Study –Voltammograms with Sluggish Kinetics ..............138
Figure 10.10: Rotating Ring-Disk Voltammograms at Various Rotation Rates .................141

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DRU10002 (REV 004 / JAN 2017)
1Preface
1.1 Scope
The MSR rotator is a solid-state-controlled servo-system designed to rotate an
electrode in an electrochemical cell. This manual describes the proper use of the
MSR rotator and covers routine operating procedures, periodic maintenance and
calibration, and safety issues.
The reader of this manual is assumed to have some basic knowledge of
electronics, electrochemistry, and the modern practice of voltammetry. While
some background information is presented in this manual, the reader is referred
to the appropriate scientific literature for more detail regarding the theory and
practice of hydrodynamic voltammetry.
Pine Research 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 in any form, electronic or
mechanical, including photocopying, recording, storing in an information
retrieval system, or translating, in whole or in part, without the prior consent of Pine
Research Instrumentation, Inc. in writing.
1.3 Trademarks
WaveDriver®, WaveNow®, WaveNano® and AfterMath® are registered
trademarks of Pine Research Instrumentation, Inc. (Durham, NC). All other
trademarks are the property of their respective owners.
1.4 Use Limitation
The MSR rotator is not designed for use in experiments involving human subjects
and/or the use of electrodes inside or on the surface of the human body.
Any use of this instrument other than its intended purpose is prohibited.

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1.5 Service and Warranty Information
For questions about proper operation of the MSR rotator or other technical issues,
please use the contact information below to contact Pine directly.
TECHNICAL SERVICE CONTACT
Pine Research Instrumentation, Inc.
www.pineresearch.com
Phone: [phone]
FAX: [phone]
If the MSR rotator or one of its components or accessories must be returned to the
factory for service, please contact Technical Service (see above) to obtain a
Return Material Authorization (RMA) form. Include a copy of this RMA form in
each carton and ship to the Factory Return Service Address (below).
FACTORY RETURN SERVICE ADDRESS
Pine Instrument Company
ATTN: RMA #: <RMA number>
104 Industrial Drive
Grove City PA 16127
USA
Phone: [phone]
Return Material Authorization Required!
Do not ship equipment to the factory without first obtaining a
Return Material Authorization (RMA) form from Pine Research
Instrumentation, Inc.
LIMITED WARRANTY
The Pine MSR Rotator (Pine part number AFMSRCE, hereafter referred to as “WARRANTED
INSTRUMENT”) offered by Pine Research Instrumentation, Inc. (hereafter referred 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 used under
normal laboratory conditions. SUPPLIER’s obligation under this warranty is limited to replacing or
repairing parts which shall upon examination by SUPPLIER personnel disclose to SUPPLIER’s satisfaction
to have been defective. The CUSTOMER may be obligated to assist SUPPLIER personnel in servicing
the WARRANTED INSTRUMENT. SUPPLIER will provide remote support (via telephone or internet) to
guide the CUSTOMER to diagnose and effect any needed repairs. In the event that remote support
is unsuccessful in resolving the defect, SUPPLIER may recommend that the WARRANTED INSTRUMENT
be returned to SUPPLIER for repair. This warranty is expressly in lieu of all other warranties, expressed or
implied and all other liabilities. All specifications are subject to change without notice. The CUSTOMER
is responsible for charges associated with non-warranted repairs, such charges including but not
limited to travel expenses, tariffs, labor, parts and freight charges.
This warranty does not apply to shafts, electrodes, glassware or other accessories that are used in
conjunction with the WARRANTED INSTRUMENT.

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DRU10002 (REV 004 / JAN 2017)
1.6 Instrument Markings
Labels on the control unit and motor unit bear information to identify the MSR
rotator and to indicate any certifications or independent testing agency marks
which pertain to the instrument (see Figure 2.4).
1.6.1 Certifications and Listings
The MSR rotator complies with one or more EU directives and bears the CE
marking. See the "CE Declaration of Conformity" attached to the end of this
manual for more details.
The MSR rotator is listed by Intertek to UL 61010-1 (issued 11-MAY-2012; Ed. 3),
CSA C22.2 #61010-1 (issued 11-MAY-2012; Ed. 3), and IEC 61010-1 (issued 10-
JUN-2010; Corrigendum 1: 11-MAY-2011). Intertek is a Nationally Recognized
Testing Laboratory (NRTL) recognized by the United States Occupational Safety
and Health Administration (OSHA).
1.6.2 Serial Number
For purposes 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 a similar label located on the
motor unit. In laboratories with multiple MSR rotators, it is important to keep the
control unit together with the matching motor unit because the two components
are calibrated together as a system (see Section 6.6).
1.6.3 Model Numbers
Pine MSR rotator model numbers have the format 'AFMSRWXYZ' where W, X, Yand
Z are each single characters used to indicate the particular configuration of the
rotator (see Table 1.1). The final characters (X, Yand Z) may be blank. Part
numbers for electrodes and other accessories compatible with the MSR rotator
are described in more detail later (see Section 5 and Section 7).
Model
Number:
A
F
M
S
R
W
X
Y
Z
Model Name
A
F
M
S
R
C
E
Pine MSR Rotator
A
F
M
S
R
6
3
6
A
Model 636A Rotator
A
F
M
S
R
7
1
0
A
Model 710A Rotator
Table 1.1: Pine Rotator Part Numbering

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1.7 Specifications
All specifications are subject to change without notice.
Power
100 - 240 VAC, +/-10%; 50/60 Hz; 2A
Shipping Information
shipping weight: 60 pounds (27 kg)
shipping dimensions: 24.0 x 24.0 x 24.0 in (61 x 61 x 61 cm)
Dimensions
(L x W x H)
control unit: 11.4 x 10.1 x 5.75 in (29 x 26 x 15 cm)
rotator enclosure: 18.8 x 15.5 x 21.0 in (48 x 40 x 54 cm)
Operating Temperature
10 ºC to 40 ºC (50 ºF to 104 ºF)
Motor
motor power: 15 W
supply voltages: +30 VDC, –24 VDC
motor type: permanent magnet
Motor Protection
2 Amp thermal-type circuit breaker
current limited power supplies
Maximum Continuous
Torque
28.3 millinewton-meters
Rate Control
closed loop servo-system
temperature compensated tachometer mounted on motor shaft
Rate Display
4 ½ digit display indicates 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 control knob
button to reset circuit breaker
back panel: power switch
Rotation Rate Input
allows optional external signal to control rotation rate (banana
jack)
selectable control ratio: 1 RPM/mV (default)
2 RPM/mV
4 RPM/mV
Rotation Rate Output
allows optional external monitoring of rotation rate (banana jack)
output signal ratio: 1 mV/RPM (±1.0%)
Rotator Motor Stop
back panel input optional digital motor stop signal (banana jack)
Earth Ground
metal binding post (banana jack) connects to ground lead of
power cord and to control unit chassis
Common Jacks
DC common (3 black banana jacks), isolated from earth ground
Slew Rate of Motor
approximately 300,000 RPM/sec maximum (no load)
Bandwidth
> 50 Hz, -1 dB
(at 1000 RPM peak to peak modulation on a 2000 RPM base rate)