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TA Instruments Nano ITC 5300, Getting Started Manual

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Nano ITC Getting Started Guide

Chapter 3: Use, Maintenance, & Diagnostics  ................................................................................ 23

Overview  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

Calibrating Chemicals  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

Heat of Protonation of Tris Base . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

Sample Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

Experiment Setup   . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

Experiment Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

Preparing and Degassing the Solutions  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27

Degassing Solutions   . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27

Preparing the Sample and Reference Cells  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

Loading the Buret  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
Installing the Buret Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
Starting the Experiment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32

Cleaning the Nano ITC  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33

Analyzing the Data   . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36

Maintaining the Nano ITC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37

Purging the Nano ITC  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37

Troubleshooting the Nano ITC  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38

Minimizing Blank Corrections  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
Operating at Non-Ambient Temperatures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
Stirring Speeds   . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
Stable Instrument Operation  . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .39

Appendix A: Buret Position Functions ........................................................................................... 41

Index ................................................................................................................................................... 43

Summary of Contents for Nano ITC 5300

Page 1: ...Revision F Issued February 2011 Getting Started Guide for Models 5300 5301 5302 Nano Isothermal Titration Calorimeter Nano ITC...

Page 2: ...ule Data Analysis and Utility Software and their asso ciated manuals and online help are proprietary and copyrighted by TA Instruments Purchasers are granted a license to use these software programs o...

Page 3: ...nual Supplement Please click the TA Manual Supplement link to access the following important information supplemental to this Getting Started Guide TA Instruments Trademarks TA Instruments Patents Oth...

Page 4: ...nstrument was designed specifically as a test and measuring device Compliance to the EMC directive is through IEC 61326 1 Electrical equipment for measurement control and laboratory use EMC require me...

Page 5: ...g the instrument before doing any maintenance or repair work voltages as high as 125 250 VAC are present in this system Lifting the Instrument The Nano ITC is not a portable instrument In order to avo...

Page 6: ...Page 6 Nano ITC Getting Started Guide This page is intentionally blank...

Page 7: ...lications 10 Batch Incremental Titration 10 Titration Data Analysis 11 Calculation of Equilibrium Constants 11 System Components 12 Measuring Unit 12 Reaction Vessel 13 Syringe Stirrer 14 Buret Assemb...

Page 8: ...s 27 Degassing Solutions 27 Preparing the Sample and Reference Cells 28 Loading the Buret 30 Installing the Buret Assembly 31 Starting the Experiment 32 Cleaning the Nano ITC 33 Analyzing the Data 36...

Page 9: ...method T power compensation and heat flow has its advantages and disadvantages The TA Instruments Nano Isothermal Titration Calorimeter ITC uses a differential power compensation design for maximum se...

Page 10: ...ed on the back of the calorimeter unit all func tions of the Nano ITC are controlled remotely by the computer through the USB connection Figure 1 Nano ITC2G Applications Batch Incremental Titration In...

Page 11: ...etween titrant and titrate solutions These corrections are most easily accomplished by performing a blank titration experiment and subtracting the blank heat data from the experimental thermogram In t...

Page 12: ...system are briefly described in the following sections Measuring Unit The measuring unit includes the calorimeter block and two non removable reaction vessels sample and reference cells Access tubes...

Page 13: ...sible condensation and evaporation of moisture around the unit which would create excessive baseline noise CAUTION The purge port valve on the back of the Nano ITC should remain in the closed posi tio...

Page 14: ...ou can verify the feel of the normal resistance by installing a buret with no syringe in place The titrant syringe needle also functions as the stirrer and extends down into the reaction vessel from t...

Page 15: ...y constant and adjustable speed The motor drives the rotating shaft of the buret which holds the titrant syringe Buret Assembly The buret accurately delivers the titrant to the reaction vessel at spec...

Page 16: ...elative Humidity 5 to 80 non condensing Installation Category II Pollution Degree 2 Maximum Altitude 2500 m 8200 ft Emissions class Class A Temperature range 2 to 80 C Injection interval 150 s minimum...

Page 17: ...ion Only limited instructions are given in this manual consult the online documentation for additional information Installation involves the following procedures Inspecting the system for shipping dam...

Page 18: ...m dusty environments exposure to direct sunlight direct air drafts fans room air ducts poorly ventilated areas noisy or mechanical vibrations high traffic areas where constant movements from passing p...

Page 19: ...ncludes the C1E setting which should be disabled Others may call it the Enhanced Halt State Other settings that should be disabled if available are EIST Intel SpeedStep and AMD s Cool n Quiet Set the...

Page 20: ...e surge suppressor power switch and the computer system and monitor 2 Turn on the power switch to the calorimeter which is located on the back panel The front LED will light up green when in the on po...

Page 21: ...nd its associated components on when the Nano ITC will be inactive for several days If the Nano ITC will be inactive for more than 5 days we recommend that you first thoroughly clean then empty the ce...

Page 22: ...Page 22 Nano ITC Getting Started Guide This page is intentionally blank...

Page 23: ...ed with the software program It is assumed that you are familiar with standard laboratory procedures and techniques It is critical that the Nano ITC cells be cleaned immediately at the end of each exp...

Page 24: ...mum of 45 minutes Do not degas the prepared solutions because this can result in the loss of sample The solutions can be kept for a short time in stoppered containers Use nitrogen or argon to fill the...

Page 25: ...reading on the calorimeter is stable Then begin the experiment Enter a file name at the prompt The results should be similar to those shown in the figure below Figure 9 Example of successful calibrati...

Page 26: ...late an average of the C F for several injection peaks In the Settings screen shown below enter the new calibration factor in the provided entry box Calibration factors for the ITC always have a negat...

Page 27: ...late solutions of any large molecule sample compounds at this time using the buffer solution Small molecule sample compounds will be made up in a following step 3 Dialyze the solution s inside the rem...

Page 28: ...and slowly load the sample into the sample cell middle access tube inside the Nano ITC to allow air bubbles to evacuate through the top of the cell a When liquid is just visible at the opening of the...

Page 29: ...ss tubes 3 Load the 100 L syringe with the titrant taking care to remove any bubbles from the barrel of the syringe but leaving a small 5 to 10 L air gap between the plunger tip and the liquid in the...

Page 30: ...he buret handle displays a graduated scale with an indicator showing the relative posi tion of the syringe plunger during an experiment The indicator must be in the fully raised position before instal...

Page 31: ...with the syringe into the Nano ITC 3 Hold the rotating shaft on the buret securely in one hand Use the knurled knob at the base of the syringe barrel to finger tighten the syringe into place with the...

Page 32: ...te speed For instruments with gold cells this is typically in the range of 250 400 rpm Hastelloy cell instruments typically use 150 200 rpm 2 Allow the system to re equilibrate until the calorimeter h...

Page 33: ...the next experiment Fill the cells with pure deionized water between experiments to prevent contamina tion from drying the cell walls The cleaning tool is used as follows 1 Ensurethattheinstrumenttem...

Page 34: ...ard to the outlet at the top of the tool and out to the vacuum flask The figure below shows the flow of water through the apparatus Note that the cleaning tool for the Nano ITC Low Volume instrument i...

Page 35: ...g devices described beginning on page 33 Caustic solutions should be loaded and removed with the appropriate syringe or micropipette Soapy Water Flush 1 Exit from the ITCRun software This must be done...

Page 36: ...acquisition The main components are Experiment Settings Instrument Control Main Menu Functions Buret Menu Feature Tabs Monitor Tabs Data Tab NanoAnalyze Quick easy integration of heat rate data from I...

Page 37: ...act TA Instruments for service Check for stability by operating the Nano ITC near ambient temperature with the cells filled with degassed water Stirring should be switched off and the instrument allow...

Page 38: ...ime between injections for the titrant to equilibrate to the calorimeter temperature before injection Thorough degassing of the titrant is especially important when operating above the ambient tempera...

Page 39: ...on when the cells have been filled with degassed deoinized water and allowed to settle with the syringe and reference needles in place with room tempera ture controlled to within 1 C Table 3 Typical V...

Page 40: ...Page 40 Nano ITC Getting Started Guide This page is intentionally blank...

Page 41: ...y The positioning can be performed either via a percent of the full stroke or directly in microliters Click Home Reset The desired buret position can be entered directly in L In the case if the Standa...

Page 42: ...th of the syringe stroke Follow the instructions on the screen paying particular attention to removing the syringe from the buret handle before proceeding Click Home Reset to start the Home Reset proc...

Page 43: ...tions 38 buret 30 33 installing 31 loading 30 position markers 41 removal 30 C cautions 4 cell cleaning 33 cells flushing 28 cleaning 33 adapter 33 conical overflow reservoir 29 contamination 33 D dei...

Page 44: ...choosing a location 18 components 12 inspecting 17 installing 17 lifting 5 maintenance 37 purging 37 shut down 21 starting 20 unpacking repacking 17 instrument symbols 5 ITCRun 32 36 L license agreeme...

Page 45: ...ompliance 4 S safety 5 electrical 5 instrument symbols 5 Safety Standards 4 safety standards 4 sample cell cleaning 33 set up connecting cables and cords 19 shut down 21 solutions preparing 27 startup...

Page 46: ...Page 46 Nano ITC Getting Started Guide tubing connecting 33 V viscous mixing 38 W warnings 4...

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