MicroCal VP-ITC User manual
Table Of Contents
General .............................................................................................................................................i
How To Use This Manual ............................................................................................................................i
How to Get Help From MicroCal............................................................................................................... ii
Section 1: VP-ITC System Introduction......................................................................................1
1.1 VP ITC – The Basics.............................................................................................................................2
1.2 Data Acquisition and Instrument Control..............................................................................................3
1.3 Suitable Laboratory Environment .........................................................................................................4
1.4 VP-ITC Parts and Accessories ..............................................................................................................5
1.5 Setting Up the VP-ITC Instrument........................................................................................................7
1.6 Pipette Assembly...................................................................................................................................9
1.7 The ThermoVac...................................................................................................................................11
Section 2: VPViewer and Origin Software................................................................................14
2.1 VPViewer and Origin Software Overview ..........................................................................................15
2.2 Powering Up the VP-ITC Instrument ..................................................................................................15
2.3 VPViewer Main Window ....................................................................................................................17
2.4 ITC Controls Window .........................................................................................................................21
2.5 Thermostat/Calibration Window .........................................................................................................26
2.6 Setup/Maintenance Window................................................................................................................27
2.7 Constants Window...............................................................................................................................30
2.8 Real Time Data Display in Origin.......................................................................................................31
2.9 ITC Cell Status ....................................................................................................................................33
Section 3: Running an ITC Experiment....................................................................................35
3.1 Designing ITC Experiments ................................................................................................................36
3.2 Using the ThermoVac to Degas Samples ............................................................................................40
3.3 Cell Loading........................................................................................................................................41
3.4 Loading the Auto-Pipette.....................................................................................................................42
3.5 Choosing The Run Parameters ............................................................................................................45
3.6 Carrying Out Experimental Runs ........................................................................................................46
3.7 Using the ThermoVac for Cleaning the ITC Sample Cell...................................................................47
3.8 Cleaning Syringes................................................................................................................................49
Section 4: Experimental Tutorials .............................................................................................50
4.1 Water-Water Baselines........................................................................................................................51
4.2 Methanol Tutorial................................................................................................................................60
4.3 Rnase-2’CMP Experiment Tutorial.....................................................................................................63
Section 5: Instrument Maintenance............................................................................................64
5.1 Cleaning The Cells and Pipette ...........................................................................................................65
5.2 Replacing Pipette Plunger Tips ...........................................................................................................68
5.3 Y-axis Calibration ...............................................................................................................................72
5.4 Replacing Injection Syringes & Height Adjustment ...........................................................................74
Section 6: Tips and Troubleshooting .........................................................................................76
6.1 User Tips and FAQs ............................................................................................................................77
6.2 Troubleshooting...................................................................................................................................78
6.3 A Note About Buffers .........................................................................................................................79
6.4 Selecting the Proper Stirring Rate .......................................................................................................79
6.5 Estimation of Required Concentrations...............................................................................................80
Section 7: Additional Features ....................................................................................................81
7.1 Extended Data Display ........................................................................................................................82
.......................................................................................................................827.2 Customizing VPViewer
MAU130030 Rev. A 12/3/02
VP-ITC MicroCalorimeter User’s Manual
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Section 1: VP-ITC – General Information
General
How To Use This Manual
This manual describes the VP-ITC; its setup, operation and maintenance.
Once the instrument is setup (as described in Section 1), a new user may wish to go directly to
Section 4 and run through the experimental tutorials for a “hands on” approach to learning about
the instrument and software. The user should then refer back to sections 2 and 3 for detailed
descriptions toward a better understanding of the intricacies of the instrument. Section 5 contains
important information for maintaining the instrument performance. Section 6 provides tips for
optimizing the performance and troubleshooting techniques for commonly encountered problems.
Section 7 provides description of some more advanced features.
Much of this manual provides descriptions of the VP-ITC instrument and software. Bullets or
step numbers are typically used when the user is requested to perform an operation.
•Indicates a step to perform an operation
1. Steps are numbered when the sequence of operations is critical.
i
VP-ITC MicroCalorimeter User’s Manual
How to Get Help From MicroCal
The service department at MicroCal, LLC is available to help you during normal business hours, Monday
through Friday from 8:00 AM to 5:00 PM (EST). Service personnel may be contacted by e-mail, phone or
fax, with the preference being by phone or e-mail. When e-mailing MicroCal for technical assistance, if
possible, please attach a recent data file(s) (*.itc, raw ITC data files) that demonstrate the problem. Also,
please include with the correspondence, all details that may be relevant to the problem. In instances where
the problem or question relates to post run data analysis, it is best to attach the raw data file (*.ITC) and the
Origin document (*.opj) generated during data analysis.
There are 2 general categories of problems associated with the VP-ITC and its operation. The most
extreme category is when a system is simply not working, at all. Problems that prevent users from
operating the VP-ITC require immediate consultation with a MicroCal technician. Customers
should not attempt to repair the VP-ITC hardware or software unless instructed to do so by a
MicroCal service representative.
The second, and less extreme general category of problems is when a VP-ITC instrument is functioning,
but is not operating within its normal performance specifications. Large baseline drifting, non-repeatable
control peaks (Water/Water) and/or an increase in short term noise level are all examples of performance
problems, typically correctable by the operator. For performance issues such as these it is recommended
that customers carry out the following minimum diagnostic steps prior to contacting MicroCal for service:
1.) Thoroughly clean the cells. Do not assume they are clean. As a minimum, use the provided
Cell Cleaning Apparatus to pass 500 ml of a 10-25% ammoniated detergent in water solution,
followed by 500 ml of cold water rinse, through the sample cell. Discretion may call for a
more rigorous cleaning procedure as described herein.
2.) Refill both the reference and sample cells with filtered, degassed water. Fill a thoroughly
cleaned syringe with water and/or use a different syringe.
3.) Go to the Setup/Maintenance window within VPViewer 2000 (as described, starting on page
27) and activate the extended data mode. (While in extended data mode, ITC data files will
contain all available information produced by the VP-ITC and often times is helpful in
diagnosis of problems).
4.) Carry out a minimum of 25, 10µL injections of water into water
5.) Consult the troubleshooting section of this manual.
If, after completion of the 5 steps listed above, the ITC performance is not corrected, contact the MicroCal
service department for help. The water run, in extended data mode, should be provided to the MicroCal
service technician for evaluation. The service department with comments and recommendations will then
contact customers.
MicroCal, LLC Contact Information:
Primary Contact Phone 413-586-7720
Toll Free Phone Number 800-633-3115
Facsimile 413-586-0149
Web Site: www.MicroCalorimetry.com
ii
Section 1: VP-ITC – General Information
Symbols
Symbols used in this manual
!Warns the user of possible damage to the unit, draws attention to the risk of injury or
contains safety notes and warnings.
Symbols used on the VP-ITC instrument
Caution: Read the instruction manual before operating
Instrument (supply) ON
Instrument (supply) OFF
Protective Earth (Ground) Terminal
Origin® is a registered trademark of Origin Lab, Northampton, MA
VPis a registered trademark of MicroCal, LLC, Northampton, MA
MicroCalis a registered trademark of MicroCal, LLC, Northampton, MA
Windows™ is a registered trademark of Microsoft Corporation
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VP-ITC MicroCalorimeter User’s Manual
Operators Safety
!The points below are intended to enhance your safety awareness and to draw your attention to risks
which only you, the operator, can prevent. MicroCal has set high standards for ourselves in
developing and constructing the VP-ITC. Each unit constructed is fully tested to operational and
safety standards. It should be noted that no amount of design or constructed safeguards can anticipate
or prevent improper handling. It is intended that this instrument be operated only by responsible
people trained in basic laboratory protocol in procedures and safety techniques. This product is
intended to operate from a power source that does not apply more than 260 V rms between the
supply conductors or between either supply conductor and ground. A protective ground
connection, by way of the grounding conductor in the power cord, is essential for safe operation
!To avoid any hazard, use only a fuse of the correct type, voltage rating and current rating as
specified on the back of the VP-ITC. This is a 1 Amp 250 Volt Time-lag (Time Delay) fuse.
!Repairs, alterations or modifications must only be carried out by specialist personnel. The
MicroCal Service Department will be happy to serve you for any repair work or operational
questions.
!This device is not designed to the Medical Devices Directive 93/42/EEC and should not be used
for medical purposes and/or in the diagnosis of patients.
!When using volatile or hazardous solutions in the cells, the operator should always follow proper
laboratory procedures in handling (e.g. wear safety glasses and protective clothing) and
disposing of such materials and allow the internal cells to cool down to room temperature before
removing any solutions from the cells.
!All solutions in the cells must be cooled down below 50 ºC before removing from the cells to
prevent the glass syringes from breaking due to the hot liquids.
Product Safety
We have used all means to design and produce the VP-ITC to prevent any damage to the instrument during
normal usage. The instrument is solidly built using the latest in micro-technology in its components and
design, but of course, this cannot prevent damage due to physical mistreatment. The attentiveness of the
operator to the identification of materials which could corrode the Hastelloy® Alloy C-276 cells, the
prevention of freezing solutions in the cells and the responsible handling and usage of the instrument
should ensure a long service life for the VP-ITC.
!The VP-ITC cells are constructed out of Hastelloy®C-276. Hastelloy is extremely resistant to
corrosion by strong bases, but strong acids should be avoided. Please refer to the accompanying
booklet “Hastelloy®Alloy C-276” for further information.
!The freezing of solutions in filled cells will cause irreparable damage to the cells due to the
expansion of the solution in the cells.
!When moving the VP-ITC the instrument should always be in its normal operating or its vertical
position. The instrument should never be moved in a sideways position, due to the nature of the
crystal detectors used for the instruments thermal sensing, which are strong in a compression
mode but weak when subjected to shear stresses.
iv
Section 1: VP-ITC – General Information
Instrument Specifications
Model or Type : VP-ITC
Performance Specifications (2 second filter)
Noise Level (3 minute RMS windows averaged over 1 hour) : 1 nanocal/sec (4 nanowatts)
Baseline Constancy (average one hour time intervals: 310 rpm stirring) : ±5 nanocal/sec (±20 nanowatts)
Minimum Response Time : 15 seconds
Operating Temperature Range : 2°to 80°C
Physical Specifications
Cell Material : Hastelloy® Alloy C-276
Dimensions (L x W x H in cm) : 45 x 20 x 18
Weight (approximate) : 9 kg
v
VP-ITC MicroCalorimeter User’s Manual
Safety Specifications
Instrument Specifications (excluding Controller)
Electrical Specifications
Electrical Ratings:
Voltage : 240 Volts
Frequency : 50 Hz
Current (maximum) : 1.0 Amp
Fuses (2) : Primary=1.0 A, 250 V, Time Delay
Output : Secondary/Data Connection only
Protective Earth Terminals : Internal/external marked
Mode of Operation : Continuous
Classification : Class I
Atmospheric Specifications
Operating:
Temperature : 10°to 40°C
Humidity : 0 to 75% RH noncondensing
Atmospheric Pressure : 700 HPa to 1060 HPa
Storage: (in original shipping containers with no liquid in cells)
Temperature : -40°to +70°C (no liquid in cells)
Humidity : 10% to 90%
Atmospheric Pressure : 500 HPa to 1060 HPa
vi
Section 1: VP-ITC – General Information
Cleaning the VP-ITC Instrument Case
Always shut down the computer controller and VP-ITC instrument and disconnect the mains power supply
cord before cleaning the case. To clean the instrument case, use a damp, lint-free cloth. Avoid abrasives or
solvents that can permanently damage the finish. With the damp cloth, gently wipe the external surfaces of
the instrument.
vii
VP-ITC MicroCalorimeter User’s Manual
European Users: CE Mark
Microcal VP-ITC calorimeters carry the CE marking which confirms that they meet the applicable
European Community Technical Directives. We declare that we have followed the provisions of EMC
Directive 89/336/EEC (Electromagnetic Compatibility) and Low Voltage Directive 72/23/EEC (Electrical
Safety). The following tests were carried out:
Directive Generic Standard Referenced standard
89/336/EEC (EMC) EN 55011, Group 1, Class B, 1991
EN 50082-1 (Immunity) EN 61000-4-2:1995
EN 61000-4-3:1995
EN 61000-4-4:1995
72/23/EEC (LVD) EN 61010-1:1993, EN 61010-1:1993/A2:1995
Please refer to the manuals which came with the computer controller for information relating to the CE
mark for this unit.
viii
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