User`s manual

58 Chapter 5: Software Description
Calorimetry Sciences Corp.
CSC 5300 N-ITC III 59
User’s Manual
Chapter Six: Sample Experiments
Experiment Overview
Following is a brief description of the main steps of a titration experiment. The next
segment, Experiment Walk-Through, provides a more detailed presentation of a
typical experiment from start to nish. Read through these segments completely before
performing any of the operations described.
1. Load the sample cell with titrate and the reference cell with the appropriate buffer
or water. While ITCRun is idling, the N-ITC III cells must be allowed to equilibrate
so that a stable baseline can be observed; i.e., the heat reading on the calorimeter
does not exhibit prolonged upward or downward trends (refer to Calorimeter
Specications, Chapter 1: Introduction).
2. Load a syringe with the titrant, making sure to remove any bubbles, but keep a small
air gap (5-10 µL) between the plunger and the titrant solution. Wipe the needle with
a tissue and then load the syringe into the burette handle. Install the burette/syringe
assembly in the N-ITC III and start the stirrer (150-200 rpm). Allow the system to
re-equilibrate until the calorimeter heat reading is stable. Allowing the loaded syringe
to remain in the cell much more than 15 minutes before starting the experiment will
result in elevated baseline heat caused by diffusion of titrant into the cell, as well as a
smaller titration peak for the rst injection.
3. When a stable baseline is evident, click on ExperimentStart or the Go icon at the
top of the toolbar and the experiment will begin. Enter a le name when prompted.
The program indicator on the Setup tab will be red when the program is active. You
will be able to watch the progress of the experiment under the Monitor tab or the Data
tab.
4. When the experiment is complete, proceed to data analysis in BindWorks (see
Chapter 5: Software Description).