Extracolumn band broadening in capillary liquid chromatography

Prüß, Anja; Kempter, Christine; Gysler, Jens; Jira, Thomas

doi:10.1016/s0021-9673(03)01290-1

Cited by 64 publications

(46 citation statements)

References 40 publications

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“…Previous studies of injector design have shown that a good injection requires a narrow, low-volume plug of sample with no poorly swept flow paths [20,53,[58][59][60][61][62], which are explained more in the next section.…”

Section: Injector Contributionsmentioning

confidence: 99%

“…The geometry of the detection cell used in optical detection has been studied in order to maintain high sensitivity while decreasing the overall volume (and variance contribution) [20,[74][75][76][77][78][79]. Since this cell can be the most significant contributor to extra-column broadening [15], alternate detection modes have also been surveyed.…”

Section: Detector Contributionsmentioning

confidence: 99%

“…Extra-column effects in these capillary LC (and similar nano-LC) instruments have been described previously [20,21]. In the early development of capillary UHPLC, home-built instruments were constructed that eliminated nearly all instrumental effects and gave a direct measure of column efficiency while also allowing for backpressures in excess of 50,000 psi [22][23][24][25][26][27].…”

Section: Introductionmentioning

confidence: 99%

“…Compared to a previous study on extra-column band broadening in capillary LC [20], a higher-pressure UHPLC pump was used to expand the flow rate regime that could be investigated and microelectrode electrochemical detection was implemented [48,49] to eliminate effects that detector volume can have on the observed peaks. A novel application of the Foley-Dorsey exponentially-modified Gaussian method [50][51][52] for peak characterization was used to mathematically separate the peak variance from the tubing and the injector.…”

Section: Introductionmentioning

confidence: 99%

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Measurement and Modeling of Extra-Column Effects Due to Injection and Connections in Capillary Liquid Chromatography

et al. 2015

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Abstract:As column volumes continue to decrease, extra-column band broadening has become an increasingly important consideration when determining column performance. Combined contributions due to the injector and connecting tubing in a capillary LC system were measured and found to be larger than expected by Taylor-Aris theory. Variance from sigma-type and tau-type broadening was isolated from eluted peaks using the Foley-Dorsey Exponentially Modified Gaussian peak fitting model and confirmed with computational fluid dynamics. It was found that the tau-type contributions were the main cause for the excessive broadening because of poorly-swept volumes at the connection between the injector and tubing. To reduce tau-type contributions (and peak tailing), a timed pinch mode could be used for analyte injection.

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Section: Injector Contributionsmentioning

confidence: 99%

Section: Detector Contributionsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Measurement and Modeling of Extra-Column Effects Due to Injection and Connections in Capillary Liquid Chromatography

et al. 2015

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“…[1] para os processos de dispersão intracoluna, um grande número de pesquisadores vem propondo e desenvolvendo vários métodos e equações específicas para estimar as contribuições das diversas fontes de dispersão extracoluna [11][12][13][14][15][16][17][18][19][20][21][22] . A seguir discutiremos as suas cinco principais fontes, a citar:…”

Section: Processos De Dispersão Extracoluna -S 2 Exunclassified

Cromatografia líquida capilar: 2. Alargamento das bandas por efeitos extracoluna

Coutinho¹,

Lanças

2011

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ResumoO alargamento da banda é um fator altamente indesejável em todas as técnicas cromatográficas, uma vez que diminui a eficiência da coluna (menor número de pratos, N) e deteriora a resolução (menor Rs). Este efeito é particularmente crítico na cromatografia líquida capilar (c-LC) devido aos pequenos volumes da instrumentação, conexões, colunas, etc., empregados na técnica. Como parte de uma série de artigos a respeito da c-LC, neste trabalho serão abordados os principais fatores que ocasionam o alargamento das bandas cromatográficas em c-LC, assim como a maneira de evitá-lo. Palavras-chaveCromatografia líquida capilar; alargamento de bandas; fatores extra coluna; micro LC; LC capilar. Capillary liquid chromatography: 2. Band broadening due to extracolumn effects AbstractBand broadening is one of the major factors to be avoided in chromatographic techniques, once it decreases the column efficiency (the number of plates, N) and deteriorates the Resolution (Rs). This effect is particularly critical in capillary liquid chromatography due to the very low volumes, instrumentation, connections and columns employed in this technique. As a part in a series of papers dealing with c-LC, this work describes the major factors responsible for band broadening in chromatography, as well as the ways to minimize it.

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