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Accurate determination of extra‐column band broadening using peak summation
Author(s) -
Verstraeten Matthias,
Liekens Anuschka,
Desmet Gert
Publication year - 2012
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201100771
Subject(s) - variance (accounting) , dispersion (optics) , pulse (music) , mathematics , column (typography) , boundary (topology) , statistics , algorithm , mathematical analysis , physics , optics , geometry , accounting , connection (principal bundle) , detector , business
The present contribution addresses the problem of the accurate determination of the extra‐column band‐broadening dispersion by applying the method of moments (MOM) on pulse response experiments. The MOM provides the only mathematically rigorous way to determine the variance of a pulse response, but suffers from the fact that the obtained variance values usually depend very strongly and unpredictably on the selected integration boundaries. In the present study, it is investigated whether the MOM cannot be made more accurate by repeating the pulse response experiment a number of times, then add all measured peaks (after retention time alignment) and subsequently perform the integration on this summed peak. Testing this approach for a number of different integration boundary detection methods consistently more accurate results are obtained than when the different repeat response pulses are integrated individually and the variances are averaged afterwards. It was also found that adding five repeats already leads to a significant improvement of the variance estimate, whereas the addition of 10–20 repeats is needed before the variance estimate converges to a steady value.