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Injection profiles in liquid chromatography: I. A fundamental investigation
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Physical and Analytical Chemistry, Analytical Chemistry.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Physical and Analytical Chemistry, Analytical Chemistry.
Analytical Chemistry, Department of Chemistry and Biomedical Sciences, Karlstad University, Sweden.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Physical and Analytical Chemistry, Analytical Chemistry.
2010 (English)In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1217, p. 4306-4312Article in journal (Refereed) Published
Abstract [en]

This is a fundamental experimental and theoretical investigation on how the injection profile depends on important experimental parameters. The experiments revealed that the injection profile becomes more eroded with increased (i) flow rate, (ii) viscosity of the eluent, (iii) size of the solute, (iv) injection volume and (v) inner diameter of the injection loop capillary. These observations cannot be explained by a 1D-convection-diffusion equation, since it does not account for the effect of the parabolic flow and the radial diffusion on the elution profile. Therefore, the 1D model was expanded into a 2D-convection-diffusion equation with cylindrical coordinates, a model that showed a good agreement with the experimental injection profiles dependence on the experimental parameters. For a deeper understanding of the appearance of the injection profile the 2D model is excellent, but to account for injection profiles of various injection volumes and flow rates in preparative and process-chromatography using computer-optimizations, a more pragmatic approach must be developed. The result will give guidelines about how to reduce the extra-column variance caused by the injection profile. This is important both for preparative and analytical chromatography; in particular for modern analytical systems using short and narrow columns.

Place, publisher, year, edition, pages
2010. Vol. 1217, p. 4306-4312
National Category
Chemical Sciences
Identifiers
URN: urn:nbn:se:uu:diva-151696DOI: 10.1016/j.chroma.2010.04.045ISI: 000278920900009OAI: oai:DiVA.org:uu-151696DiVA, id: diva2:410954
Available from: 2011-04-15 Created: 2011-04-15 Last updated: 2018-01-23Bibliographically approved
In thesis
1. Adsorption Studies with Liquid Chromatography: Experimental Preparations for Thorough Determination of Adsorption Data
Open this publication in new window or tab >>Adsorption Studies with Liquid Chromatography: Experimental Preparations for Thorough Determination of Adsorption Data
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Analytical chemistry is a field with a vast variety of applications. A robust companion in the field is liquid chromatography, the method used in this thesis, which is an established workhorse and a versatile tool in many different disciplines. It can be used for identification and quantification of interesting compounds generally present in low concentrations, called analytical scale chromatography. It can also be used for isolation and purification of high value compounds, called preparative chromatography. The latter is usually conducted in large scale with high concentrations. With high concentrations it is also possible to determine something called adsorption isotherms.

Determination of adsorption isotherms is a useful tool for quite a wide variety of reasons. It can be used for characterisation of chromatographic separation systems, and then gives information on the retention mechanism as well as provides the possibility to study column-column and batch-batch reproducibility. If a protein is immobilised on a solid support, adsorption isotherms can be used for pharmacological characterisation of drug-protein interactions. Moreover, they can be used for the study of unexpected chromatographic phenomena.

If the adsorption isotherm is known it is also possible to simulate chromatograms, and subsequently optimise the separation process numerically. The gain of a numerically optimised separation process is higher purity or yield of valuable compounds such as pharmaceuticals or antioxidants, as well as reducing the solvent usage. Taken all together, it saves time, money and the environment.

However, the process of the adsorption isotherm determination requires a number of careful experimental considerations and preparations, and these are the main focus of the thesis. Important steps along the way include the choice of separation system and of suitable analytes, preparation of mobile phases and sample solutions, calibration, determination of injection profiles and column void, and of course the adsorption isotherm determination method itself. It is also important to keep track of parameters such as temperature and pH. These issues are discussed in this thesis.

At the end, a description of useful methods for processing of the raw adsorption isotherm data is presented, as well as a brief passage on methods for numerical optimisation.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2014. p. 56
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 1118
Keywords
Liquid chromatography, HPLC, UHPLC, Reversed phase, Preparative chromatography, Adsorption isotherm, Injection profile, Sample pH, pH stable conditions, Peak deformation, Band distortion, Overloaded band, Chiral preparative chromatography
National Category
Chemical Sciences Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
urn:nbn:se:uu:diva-216235 (URN)978-91-554-8858-1 (ISBN)
Public defence
2014-03-14, B22, BMC, Husargatan 3, Uppsala, 10:15 (English)
Opponent
Supervisors
Available from: 2014-02-14 Created: 2014-01-20 Last updated: 2014-04-29

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Samuelsson, JörgenEdström, LenaFornstedt, Torgny

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