Vapour phase silylation for diatomaceous earth for gas chromatography

TAKAYAMA Yuzi

doi:10.2116/bunsekikagaku.28.5_307

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Other Title

けいそう土の不活性化方法に関する研究　Ｉ　　ガスクロマトグラフ用けいそう土の気相シリル化
ガスクロマトグラフヨウケイソウドノキソウシリルカ
ガスクロマトグラフ用けいそう土の気相シリル化
けいそうう土の不活性化方法に関する研究(第1報)

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Description

Adsorption properties of diatomaceous earth are reduced by a liquid phase silylation method. In this case, eliminating water from solvent, diatomaceous earth and others is very troublesome. The solvent and others used in this reaction are wasted after a single use, and hence the process is expensive. To overcome these difficulties, vapour phase silylation method was developed. Diatomaceous earth of about 1 g was packed in U-tube reactor, kept at a present temperature between (160310)°C, and dry nitrogen gas was passed through the reactor until getting dry exhaust gas. Then nitrogen gas was replaced by a silylating agent HMDS vapour and silylation was continued for (23)h. The characterization of properties of the treated supports were made with TCD gas chromatography having a 0.5m×3 mm packed column with these supports. The quality of the supports was graded as A, B, C and D in the descending order. By the present method, the class C supports were easily obtained, but only below the D class by the conventional method. Further, by this method the following merits were found : silylating agent can be reused; post-treatments, such as washing the silylated diatomaceous earth with methanol, can be omitted; wasted solutions are not produced.

Journal

BUNSEKI KAGAKU

BUNSEKI KAGAKU 28 (5), 307-313, 1979

The Japan Society for Analytical Chemistry

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