Exploring Novel Strategies for Universal Detection in Chromatography

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atmire.migration.oldid4227
dc.contributor.advisorThurbide, Kevin B.
dc.contributor.authorScott, Andrea Ferelyth
dc.contributor.committeememberHinman, Allen Scott
dc.contributor.committeememberLangford, Cooper Harold
dc.contributor.committeememberNorman, Ann-Lise
dc.contributor.committeememberMurch, Susan Jean
dc.date.accessioned2016-04-08T18:48:20Z
dc.date.available2016-04-08T18:48:20Z
dc.date.issued2016
dc.date.submitted2016en
dc.description.abstractThis thesis presents novel strategies for the universal detection of polar analytes in chromatography. This included the further development of a universal detector that is compatible with organic solvents, as well as exploring separation techniques that are compatible with the universal Flame Ionization Detector (FID). For instance, the universal response of the Acoustic Flame Detector (AFD) was comprehensively compared to the FID, where a very close linear correlation (r2 of 0.9103) was found between them. A few minor exceptions were also observed, where the most notable differences occurred for organometallic compounds. Overall, results indicate that the AFD provides a uniform response toward most hydrocarbons that is qualitatively very similar to that of an FID. Interestingly, a novel response mode for alkali metals was also observed in a Subcritical Water Chromatography operating regime. Optimal hydrogen flame gas flow rates were found near 40 mL/min for hydrocarbon response and 80 mL/min for alkali response. KCl, NaCl, LiCl and ethanol each displayed a linear FID response with respective sensitivities of 7500, 980, 130 and 1 mV/µg of analyte. This was subsequently demonstrated to greatly alter the FID response of organic salts. Accordingly, their presence in analytical samples or mobile phases must therefore be accounted for when using this detector. Finally, a novel method of separating polar analytes in Supercritical Fluid Chromatography through dynamically controlling analyte retention by tuning the pH of a water stationary phase is presented. The method utilizes a change in mobile phase from N2 to CO2 to effectively reduce stationary phase pH and control the elution of organic acids from the column. This effect is also observed to be reasonably independent of column length and time. For example in the latter case, at 80oC, a hexanoic acid standard analyte can be readily eluted on demand from a 10 m column by switching to CO2 at any point over a run time of about 1 hour. The N2/CO2 switching system is used to analyze organic acids present in a variety of different samples and it is found that they can be eluted on demand with high selectivity over other matrix components.en_US
dc.identifier.citationScott, A. F. (2016). Exploring Novel Strategies for Universal Detection in Chromatography (Doctoral thesis, University of Calgary, Calgary, Canada). Retrieved from https://prism.ucalgary.ca. doi:10.11575/PRISM/26094en_US
dc.identifier.doihttp://dx.doi.org/10.11575/PRISM/26094
dc.identifier.urihttp://hdl.handle.net/11023/2883
dc.language.isoeng
dc.publisher.facultyGraduate Studies
dc.publisher.institutionUniversity of Calgaryen
dc.publisher.placeCalgaryen
dc.rightsUniversity of Calgary graduate students retain copyright ownership and moral rights for their thesis. You may use this material in any way that is permitted by the Copyright Act or through licensing that has been assigned to the document. For uses that are not allowable under copyright legislation or licensing, you are required to seek permission.
dc.subjectChemistry--Analytical
dc.titleExploring Novel Strategies for Universal Detection in Chromatography
dc.typedoctoral thesis
thesis.degree.disciplineChemistry
thesis.degree.grantorUniversity of Calgary
thesis.degree.nameDoctor of Philosophy (PhD)
ucalgary.item.requestcopytrue
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