Persistent Link:
http://hdl.handle.net/10150/187573
Title:
DYE ASSISTED HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC).
Author:
GNANASAMBANDAN, THIRUPPUVANAM.
Issue Date:
1983
Publisher:
The University of Arizona.
Rights:
Copyright © is held by the author. Digital access to this material is made possible by the University Libraries, University of Arizona. Further transmission, reproduction or presentation (such as public display or performance) of protected items is prohibited except with permission of the author.
Abstract:
During the course of study of reversed phase ion partition chromatography, it was observed that non-ionic substances such as alcohols, ester, and ketones undergo chromatographic separation in some as yet undefined association with cationic dyes (methylene blue chloride or brilliant green). Detection of non-chromophore trace level compounds has been a major problem in liquid chromatography due to the lack of a universal detector. Refractive index detector, although a universal detector lacks sensitivity. The U.V. absorbance detector is the work horse of liquid chromatography. Its major drawback is its lack of universality. It is often desirable to extend the utility of this detector to compounds toward which they are normally insensitive. This research was directed to developing the U.V.-Visible absorbance detector into a 'universal detector'. Using a mixture of methanol/water or dioxane/water solvent containing 1 x 10⁻⁴ M cationic dye such as the mobile phase it was shown to separate on Partisil ODS or on Zorbax ODS a series of C₂-C₅ alcohols and other neutrals at submicrogram levels with good base line separation. The alcohols carry with them some dye which must come from the presaturated dye ODS column. The dye peaks are detected spectrophotometrically at λ maximum of dye and becomes a measure of the eluting alcohol concentration. Normally, these aliphatic alcohols have a poor sensitivity either with refractive index or U.V. absorbance detector. This novel mode of detection and separation of trace quantities of alcohols and other neutral species represents a significant increase in sensitivity and should be widely applicable. The experimental data on which these separations are based, poses very interesting questions. For example, is there a specific kind of interaction between the alcohol and the dye or do the alcohols distribute between the Partisil ODS and mobile phase in their customary fashion and dissolve some of the immobilized dye because of their local excess concentration? Furthermore why do the slopes of the linear calibration curves obtained for each of the alcohols vary with the particular alcohol? Retention model based on dye alcohol complex formation and equilibrium partitioning of these species is advanced.
Type:
text; Dissertation-Reproduction (electronic)
Keywords:
Liquid chromatography.; Dyes and dyeing -- Chemistry.
Degree Name:
Ph.D.
Degree Level:
doctoral
Degree Program:
Chemistry; Graduate College
Degree Grantor:
University of Arizona
Advisor:
Freiser, H.

Full metadata record

DC FieldValue Language
dc.language.isoenen_US
dc.titleDYE ASSISTED HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC).en_US
dc.creatorGNANASAMBANDAN, THIRUPPUVANAM.en_US
dc.contributor.authorGNANASAMBANDAN, THIRUPPUVANAM.en_US
dc.date.issued1983en_US
dc.publisherThe University of Arizona.en_US
dc.rightsCopyright © is held by the author. Digital access to this material is made possible by the University Libraries, University of Arizona. Further transmission, reproduction or presentation (such as public display or performance) of protected items is prohibited except with permission of the author.en_US
dc.description.abstractDuring the course of study of reversed phase ion partition chromatography, it was observed that non-ionic substances such as alcohols, ester, and ketones undergo chromatographic separation in some as yet undefined association with cationic dyes (methylene blue chloride or brilliant green). Detection of non-chromophore trace level compounds has been a major problem in liquid chromatography due to the lack of a universal detector. Refractive index detector, although a universal detector lacks sensitivity. The U.V. absorbance detector is the work horse of liquid chromatography. Its major drawback is its lack of universality. It is often desirable to extend the utility of this detector to compounds toward which they are normally insensitive. This research was directed to developing the U.V.-Visible absorbance detector into a 'universal detector'. Using a mixture of methanol/water or dioxane/water solvent containing 1 x 10⁻⁴ M cationic dye such as the mobile phase it was shown to separate on Partisil ODS or on Zorbax ODS a series of C₂-C₅ alcohols and other neutrals at submicrogram levels with good base line separation. The alcohols carry with them some dye which must come from the presaturated dye ODS column. The dye peaks are detected spectrophotometrically at λ maximum of dye and becomes a measure of the eluting alcohol concentration. Normally, these aliphatic alcohols have a poor sensitivity either with refractive index or U.V. absorbance detector. This novel mode of detection and separation of trace quantities of alcohols and other neutral species represents a significant increase in sensitivity and should be widely applicable. The experimental data on which these separations are based, poses very interesting questions. For example, is there a specific kind of interaction between the alcohol and the dye or do the alcohols distribute between the Partisil ODS and mobile phase in their customary fashion and dissolve some of the immobilized dye because of their local excess concentration? Furthermore why do the slopes of the linear calibration curves obtained for each of the alcohols vary with the particular alcohol? Retention model based on dye alcohol complex formation and equilibrium partitioning of these species is advanced.en_US
dc.typetexten_US
dc.typeDissertation-Reproduction (electronic)en_US
dc.subjectLiquid chromatography.en_US
dc.subjectDyes and dyeing -- Chemistry.en_US
thesis.degree.namePh.D.en_US
thesis.degree.leveldoctoralen_US
thesis.degree.disciplineChemistryen_US
thesis.degree.disciplineGraduate Collegeen_US
thesis.degree.grantorUniversity of Arizonaen_US
dc.contributor.advisorFreiser, H.en_US
dc.identifier.proquest8403230en_US
dc.identifier.oclc690262499en_US
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