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pubmed-article:14518759rdf:typepubmed:Citationlld:pubmed
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pubmed-article:14518759pubmed:dateCreated2003-10-1lld:pubmed
pubmed-article:14518759pubmed:abstractTextThis study describes the thermal pretreatment of a silica gel between 150 and 800 degrees C before derivatization with dimethyloctadecylchlorosilane as a means of reducing residual silanol activity in HPLC bonded stationary phases. A time study was done from 12 to 48 h to find the optimum time needed for dehydroxylation. With increasing pretreatment temperatures, the number of reactive silanols is reduced from 8 micromol/m2 to essentially zero at 1000 degrees C (where sintering occurs). The effects of the thermal pretreatments were observed with diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and solid state cross polarization magic angle spinning (CP-MAS) 29Si NMR. Following derivatization, residual silanol activity and pH stability were tested by packing columns with the derivatized silica and carrying out a series of reversed-phase liquid chromatography (RPLC) experiments. Residual silanol activity was greatly reduced when the silica was pretreated at 800 degrees C, leading to less peak tailing for basic solutes. In a strongly basic mobile phase (pH 11.5) the pretreated silica was surprisingly stable, although bond cleavage of C18 groups from the surface was observed.lld:pubmed
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pubmed-article:14518759pubmed:issn0021-9673lld:pubmed
pubmed-article:14518759pubmed:authorpubmed-author:CooperWilliam...lld:pubmed
pubmed-article:14518759pubmed:authorpubmed-author:DorseyJohn...lld:pubmed
pubmed-article:14518759pubmed:authorpubmed-author:SunseriJ...lld:pubmed
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pubmed-article:14518759pubmed:pagination23-9lld:pubmed
pubmed-article:14518759pubmed:dateRevised2009-1-15lld:pubmed
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pubmed-article:14518759pubmed:year2003lld:pubmed
pubmed-article:14518759pubmed:articleTitleReducing residual silanol interactions in reversed-phase liquid chromatography. Thermal treatment of silica before derivatization.lld:pubmed
pubmed-article:14518759pubmed:affiliationThe Florida State University, Department of Chemistry and Biochemistry, Tallahassee, FL 32306-4390, USA.lld:pubmed
pubmed-article:14518759pubmed:publicationTypeJournal Articlelld:pubmed