Vapor phase silylation of laboratory glassware
Vapor phase silylation of laboratory glassware
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实验室玻璃器皿的气相硅烷化
DOI：
10.1021/ac50008a065
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发表时间：
1976
影响因子：
7.4
通讯作者：
C. Harrington
中科院分区：
文献类型：
--
作者：
D. Fenimore;C. M. Davis;J. Whitford;C. Harrington
样品在实验室玻璃器皿表面的不可逆吸附是测定微克和亚微克极性化合物时经常遇到的问题。问题的严重性可能构成限制某些分析程序的灵敏度的主要因素。为此，许多实验室，特别是那些涉及生物来源样品分析的实验室，通过用各种硅烷化试剂处理来使样品制备中使用的玻璃器皿的表面失活。这些程序通常用于钝化气相色谱柱材料(1，2)，通常涉及用六甲基二硅氮烷、二甲基二氯硅烷或这些或类似的硅烷化试剂的混合物处理玻璃表面，这些试剂溶解在甲苯或吡啶等溶剂中。然后，玻璃器皿在额外的溶剂中漂洗，然后用甲醇进一步漂洗，以水解任何未反应的二甲基二氯硅烷，如果该化合物用于试剂混合物中。
Irreversible adsorption of sample material on the surfaces of laboratory glassware is a problem encountered frequently in determinations of microgram and submicrogramamounts of polarcompounds. The severity of the problem can be such as to constitute the major contributing factor limiting the sensitivity of certain assay procedures. For this reason many laboratories, particularly those involved in assays of samples of biological origin, inactivate the surfaces of glassware used in sample preparation by treatment with various silylating reagents. These procedures, which are often used for inacti-vation of gas chromatographic column materials (1, 2), usually involve treatment of the glass surface with hexamethyldi-silazane, dimethyldichlorosilane, or mixtures of these or similar silylating reagents dissolved in solvents such as toluene or pyridine. The glassware is then rinsed in additional solvent followed by further rinsing with methanol to hydrolyze any unreacted dimethyldichlorosilane ifthat compound is used in the reagent mixture.