Effect of the feed injection method on band broadening in analytical supercritical fluid chromatography

Vanderlinden, Kim; Desmet, Gert; Broeckhoven, Ken

doi:10.1016/j.chroma.2020.461525

Cited by 10 publications

(7 citation statements)

References 18 publications

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“…were rather low, around 0.2-0.3, showing that a strong dilution of the sample solvent was advantageous even though this resulted in a strong increase of the volume of the injected sample plug. The overfeed solvent plug, required to fully inject the loaded sample volume, was found to have a detrimental effect on the peak width, as was also observed by Berger [18,86]. Switching from methanol to hexane as overfeed solvent resulted in a significant decrease in band broadening and an almost negligible effect of overfeed volume on peak width [86].…”

Section: Sample Solvent Effects and Injection Methodssupporting

confidence: 58%

“…An alternative injection method, the so-called feed injector, was recently introduced by Agilent Technologies on their SFC instrument. Whereas typically a loop is switched in-line with the mobile phase flow path to inject the sample, this feed injector adds the sample volume to the mobile phase flow, increasing the total flow rate for a short time [86]. This yields only a limited increase in pressure drop due to the compressible nature of the mobile phase in SFC.…”

Section: Sample Solvent Effects and Injection Methodsmentioning

confidence: 99%

“…Whereas the dilution of the sample inherently results in the injection of a larger sample volume, the concomitant mixing of the sample solvent with the mobile phase reduces the solvent mismatch and its associated band broadening effects [19,83]. Vanderlinden et al investigated this injection method in detail and found that the optimal ratio Ffeed/F of injection flow rate (Ffeed) over mobile phase flow rate F is independent on the employed F [86]. This is not unexpected as a fixed Ffeed/F results in the same dilution of sample plug and sample solvent.…”

Section: Sample Solvent Effects and Injection Methodsmentioning

confidence: 99%

See 2 more Smart Citations

Advances in the limits of separation power in supercritical fluid chromatography

Broeckhoven¹

2022

TrAC Trends in Analytical Chemistry

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Section: Sample Solvent Effects and Injection Methodssupporting

confidence: 58%

Section: Sample Solvent Effects and Injection Methodsmentioning

confidence: 99%

Section: Sample Solvent Effects and Injection Methodsmentioning

confidence: 99%

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Advances in the limits of separation power in supercritical fluid chromatography

Broeckhoven¹

2022

TrAC Trends in Analytical Chemistry

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“…First, we introduce a different approach for sample introduction that is attractive in the context of high throughput retention measurement work. This approach is based on the principles of what has become known as "feed injection" [17]. Second, we present some characteristics of the data collected with our high throughput approach to give the community a quantitative sense for the repeatability and reproducibility of the measurements and the performance tradeoff made when increasing throughput.…”

Section: Introductionmentioning

confidence: 99%

Characterization of a High Throughput Approach for Large Scale Retention Measurement in Liquid Chromatography

Kempen

Dahlseid

Lauer

et al. 2023

Preprint

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Many contemporary challenges in liquid chromatography - such as the need for “smarter” method development tools, and deeper understanding of chromatographic phenomena - could be addressed more efficiently and effectively with larger volumes of experimental retention data than are available. The paucity of publicly accessible, high-quality measurements has largely been due to the high cost in time and resources associated with traditional retention measurement approaches. Recently we described an approach to improve the throughput of such measurements by using very short columns (typically 5 mm), while maintaining measurement accuracy. In this paper we present a perspective on the characteristics of a dataset containing about 13,000 retention measurements obtained using this approach, and describe a sample introduction method that improves upon the prior work. The dataset is comprised of results for 35 different small molecules, nine different stationary phases, and several mobile phase compositions for each analyte/phase combination. During the acquisition of these data, we have interspersed repeated measurements of a small number of compounds for quality control purposes. The data from these measurements not only enable detection of outliers but also assessment of the repeatability and reproducibility of retention measurements over time. For retention factors greater than 1, the mean relative standard deviation (RSD) of replicate (typically n=5) measurements is 0.4%, and the standard deviation of RSDs is 0.4%. Most differences between selectivity values measured six months apart for 15 non-ionogenic compounds were in the range of +/- 1%, indicating good reproducibility. A critically important observation from these analyses is that selectivity defined as retention of a given analyte relative to the retention of a reference compound (kx/kref) is a much more consistent measure of retention over a time span of months compared to the retention factor alone. While this work and dataset also highlight the importance of stationary phase stability over time for achieving reliable retention measurements, we are nevertheless optimistic that this approach will enable the compilation of large databases (>> 10,000 measurements) of retention values over long time periods (years), which can in turn be leveraged to address some of the most important contemporary challenges in liquid chromatography. All the data discussed in the manuscript are provided as Supplemental Information.

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“…highlighted that deformations can even happen at very low injection volume, starting at 0.3 % column volume [5]. Using specific flow-through needle injectors that increment the sample plug with a feed solvent has shown recently to be able to reduce the impact of MeOH diluent on the separation [6], but water as a diluent was not investigated. On the other hand, the situation where SFC is online with an LC instrument is even more demanding.…”

Section: Introductionmentioning

confidence: 99%

Effect of the injection of water-containing diluents on band broadening in analytical supercritical fluid chromatography

Batteau

Faure

2022

Journal of Chromatography A

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Effect of the feed injection method on band broadening in analytical supercritical fluid chromatography

Cited by 10 publications

References 18 publications

Advances in the limits of separation power in supercritical fluid chromatography

Advances in the limits of separation power in supercritical fluid chromatography

Characterization of a High Throughput Approach for Large Scale Retention Measurement in Liquid Chromatography

Effect of the injection of water-containing diluents on band broadening in analytical supercritical fluid chromatography

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