気相シリル化法により不活性化されたガスクロマトグラフ用セライトの性能 : 塩酸前処理後の取り扱いがシリル化セライトの品質に及ぼす影響
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Performance of Celite deactivated by vapor phase method for gas chromatography; Effect of succesive treatment of acid washed Celite on quality of silylated Celite. (Research on deactivation methods for diatomaceous earth. III.) Yuji TAKAYAMA (Materials Science, Toyohashi University of Technology, 1-1, Hibarigaoka, Tempaku-cho, Toyohashi-shi, Aichi) A large scale method was reported in preceeding paper {(1) J. Chromatogr., 178,63 (1979)} for the prepa- ration of high quality diatomaceous earth for gas chromatography. However, differently from the previous small scale case {(2) Bunseki Kagaku, 28, 579 (1979)} the deactivated Gelite of first rank could not be obtained sometimes by this method. Therefore, effects of various drying conditions of pretreated wet diatomaceous earth and its storage days prior to silylation which are designated by I〜V were examined. I: The sample was laid in thin layer on a plate, airdried for about 2 h and stored. II: The sample was rinsed with methanol, air-dried quickly, and stored. III: The sample was stored in a polyethylene vessel without use of any drying procedure, and air-dried immediately before the silylation at each time. IV: The sample was heat-dried at 220 ℃ or so in a thick layer (4 cm in thickness) for about 1.5 h and stored. V: The sample was dried in a gas oven with air circulation at 110 ℃ for about 1 h, and stored. After storage of various lengthes, the silylation was carried out in a way described in the previous paper {(3) ibid., 28, 307 (1979)}. The characterization of properties of the silylated supports were made with TGD gas chromatograph packed a 0.5 m × 3 mm packed column with these supports as presented in the previous paper (3). The quality of the supports was graded as A, B and C in the descending order. We report in the present paper the following finding which is an important notice to apply the proposed method {(1), (2)}. The drying process must be carried out at room temperature as quickly as possible after the hydrolysis of the raw material diatomaceous earth and followed by the silylation in no time. The longer the storage time of the hydrolyzed and dried material, the lower the quality of the products. (Received Dec. 9, 1980)
- 社団法人日本分析化学会の論文
- 1981-05-05
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