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Determination of void volume in normal phase liquid chromatography
Ping Jiang1, Di Wu1, Charles A Lucy1
1Department of Chemistry, Gunning/Lemieux Chemistry Centre, University of Alberta, Edmonton, AB, Canada T6G 2G2.
Journal of Chromatography. A
|December 6, 2013
Summary
Determining void volume in normal phase liquid chromatography (NPLC) is crucial. This study compares methods, finding pycnometry and specific tracers like TTBB offer reliable void volume measurements for NPLC columns.
Area of Science:
- Analytical Chemistry
- Chromatography
Background:
- Void volume is a fundamental parameter in chromatography.
- Limited research exists on void volume determination in normal phase liquid chromatography (NPLC).
Purpose of the Study:
- To compare various methods for estimating total void volume in NPLC.
- To evaluate the suitability of different techniques across various column types.
Main Methods:
- Comparison of pycnometry, minor disturbance method, tracer pulse method, hold-up volume, and accessible volume.
- Application of these methods to NPLC on silica, RingSep, and DNAP columns.
Main Results:
- Pycnometry provides a theoretical maximum void volume but is limited by mobile phase conditions.
- 1,3,5-Tri-t-butyl benzene (TTBB) serves as a convenient void volume marker for RingSep and DNAP columns.
- Accessible volume methods consistently underestimate void volume and are not recommended.
Conclusions:
- No single method is universally superior for void volume determination in NPLC.
- Method selection depends on column type and mobile phase conditions.
- Pycnometry and TTBB offer valuable, albeit conditional, approaches to void volume measurement.
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