Purification Solution - Developer's Guide 79
Calibration Procedures
6
System Configuration and Delay Time Calibration
• G7159B and G1364E with Agilent Delay and Checkout Calibrant
(5190-8223):
• Positive polarity: M+H (545.2), M+Na (567.2) and M+2Na (589.2).
• Negative polarity: M-H (543.2).
• If another ion mass is required for the evaluation under given
conditions, select the relevant MSD signal in Selected signal and modify
the Ionic mass value.
c If all acquired delay times are valid (no red error icon is shown next to
the value), click Accept to write them into the respective boxes in the
Preparative systems dialog box.
d If any of the acquired delay times are invalid, click on the adjacent error
icon and follow the instructions provided.
e If the UV, MSD or fraction collector sensor signal is too low or too high,
adjust the injection volume between 20 μL and 200 μL, or adjust the
sample dilution. Repeat the calibration.
f If it is still not possible to calibrate all detector signals at once, then
there is a possibility to run the calibration piecewise:
• It is necessary to obtain the detector-to-fraction collector delay for at
least one detector signal in this window, which means that the
fraction collector signal and one more signal must be capable of being
evaluated. Note the correct delay value(s).
• Under identical flow conditions, and MSD and UV detector peakwidth
settings, acquire the signal data in Chemstation with another suitable
sample.
• Manually evaluate elution times, and from their differences together
with already noted delay values, calculate all missing delay values.
• Enter the delay values manually in the Delay Volumes tab.
g It is recommended that you repeat the calibration at least once to avoid
error from various sources such as bubbles in the instrument or its
insufficient equilibration.
8 In the Preparative systems dialog box, click Write delay times to write the
UV-to-fraction collector and auxiliary-to-fraction collector delays to the
firmware of all fraction collectors.
This prevents a warning that the preparative system contains a different
delay value than the collectors, and also avoids extra run time before and