In situ synthesis of silicone liquid phases for chromatography

Hastings, Corazon R.; Aue, Walter A.; Larsen, F.N.

doi:10.1016/s0021-9673(00)95570-5

Cited by 30 publications

(4 citation statements)

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“…Chlorosilanes react with surface hydroxyl groups to form bonded films of varying structure (1). A number of adsorbent modification procedures employing diand trlchlorosilanes have been used to form bonded phases for chromatographic use (1)(2)(3)(4)(5)(6)(7)(8)(9)(10)(11)(12)(13)(14)(15)(16).…”

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“…Previously several workers have described in-situ processes for preparing bonded phases for chromatographic application. Hastings et al (7) have described a partial insitu process in which the final polymerization was carried out directly in the column. Later, Gilpin and coworkers (14, 15) discussed a simple, totally in-situ process for preparing bonded phases for HPLC use.…”

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In-situ chemically bonded stationary phases for high pressure liquid chromatography

Gilpin¹,

Korpi²,

Janicki³

1975

Anal. Chem.

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Chemically bonded stationary phases for high pressure Iiquld chromatography (HPLC) have been used In a variety of applications. In previous work, we have described a slmpie and totally In-situ process for preparing bonded phases for high pressure iiquld chromatographic use. Columns were prepared by reaction of either octadecyltrichlorosllane or phenyltrlchiorosllane with porous layer slilca beads. Inltlaliy, pre-reaction surface moisture was controlled by drying with flowing nitrogen. However, the performance and reproducibility of bonded phase packings are controlled to a large degree by the amount of bonded material on the surface. Since the trlchlorosilanes used polymerire readily In the presence of moisture, the amount of material bonded to the silica surface can easily vary between different columns unless the amount of water Is controlled to a reproducible degree. This paper describes a set of In-situ reaction condltlons which produce columns with a better degree of reproducibility. The amount of physically adsorbed surface water was established by first pumping water-saturated toluene followed by a specified volume of dry toluene through packed columns. In addition to discussing the actual preparation technique, the general chromatographic behavior of several In-situ prepared columns has been examined.Chemically bonded stationary phases for high pressure liquid chromatography (HPLC) have been used in a variety of applications. The most familiar means of preparing these phases is by bonding various organosilane molecules to a silica type surface. Perhaps the most common of these have been the reactions of the chlorosilanes. Chlorosilanes react with surface hydroxyl groups to form bonded films of varying structure (1). A number of adsorbent modification procedures employing di-and trichlorosilanes have been used to form bonded phases for chromatographic use ( I -16).Previously several workers have described in-situ processes for preparing bonded phases for chromatographic application. Hastings et al. (7) have described a partial insitu process in which the final polymerization was carried out directly in the column. Later, Gilpin and coworkers (14,15) discussed a simple, totally in-situ process for preparing bonded phases for HPLC use. Columns were prepared by the reaction of either octadecyltrichlorosilane or phenyltrichlorosilane with porous layer silica beads (Corasil 11, 37-50 p). Advantages of the method were ease and convenience of preparation.One of the most important factors affecting the performance of bonded phase columns is the amount of material deposited on the surface (8). Since the trichlorosilanes used polymerize readily in the presence of moisture, the amount of material bonded to the silica surface can easily vary between different columns unless the amount of water is controlled to a reproducible degree.This paper describes a set of in-situ reaction conditions which produce columns with a good degree of reproducibilAuthor to whom correspondence should be addressed.ity. In addition, several...

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In-situ chemically bonded stationary phases for high pressure liquid chromatography

Gilpin¹,

Korpi²,

Janicki³

1975

Anal. Chem.

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“…Poly (ester-acetals), such as those obtained by co-polymerization of methyl azelaaldehyde pentaerythritol acetal (a spiro acetal diester), dimethyl 1,3-cyclohexanedicarboxylate and diethylene glycol, cross-linked and bonded to silanol groups of an acidic siliceous support were recommended as polar stationary phases for use from -60 to 200 °C (632). The in situ polymerization of silicone liquid phases from monomers of octadecyltrichlorosilane, dimethyldichlorosilane, and phenylmethyldichlorosilane on Chromosorb G and W supports was also reported (375).…”

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Gas chromatography

Juvet¹,

Cram²

1974

Anal. Chem.

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This review surveys developments in the field of gas chromatography since publication of the last review in this series (178) and covers the years 1972-73. Gas chromatography continues to be one of the most active areas in analytical chemistry. In the 1973 Directory of Membership of the ACS Division of Analytical Chemistry (356), those listing their research specialty as "gas chromatography" were second in numbers only to those listing the drugs compiled by the editorial staff (423) and articles on applications of GC in alcohol analysis (417), hallucinogenic drugs ( 818), the analysis of narcotic analgesics and amphetamines (622), barbiturates (446), and phenothiazine drugs (158).

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“…Effects of Heterogeneity. If the protein or ligand is heterogeneous so that there are a number of different association constants, then the slope of the curve as viewed from the concentration axis is decreased (6). The extent of heterogeneity may be represented by the constant c, less than unity, in the equation:…”

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