DETERMINATION OF HYDROXYL-GROUPS IN POLY(ETHYLENE GLYCOLS)

被引：31

作者：

FRITZ, DF ^{[1
]}

SAHIL, A ^{[1
]}

KELLER, HP ^{[1
]}

KOVATS, ES ^{[1
]}

机构：

[1] ECOLE POLYTECH FED LAUSANNE,CHIM TECH LAB,CH-1007 LAUSANNE,SWITZERLAND

来源：

ANALYTICAL CHEMISTRY | 1979年 / 51卷 / 01期

关键词：

D O I：

10.1021/ac50037a010

中图分类号：

O65 [分析化学];

学科分类号：

070302 ; 081704 ;

摘要：

An analytical method for the determination of hydroxyl content in poly (ethylene glycol) is presented and verified. It consists of substituting the hydroxyl group with a chromophoric siloxy group, purification of the silylated polymer, and a photometric determination of the chromophor concentration. The silan-ization of the primary hydroxyls with dimethylaminosilanes is shown to proceed quantitatively under very mild conditions and that the elimination of the excess reagent by precipitation is easy. The precision of the method is ±4.5% (95% confidence level) down to 5 X 10-4 mol kg-1 and it is estimated to be applicable to a lower limit of 10-4 mol kg-1. The method has about the same precision as the current standard acylation method but yields a 1000-fold gain in sensitivity. © 1979, American Chemical Society. All rights reserved.

引用

页码：7 / 12

页数：6

共 21 条

[1] USE OF PHOSGENE IN DETERMINATION OF HYDROXYL GROUPS IN POLYMERS [J].

BUSH, DG ;

MERRILL, SH ;

KUNZELSA.LJ .

ANALYTICAL CHEMISTRY, 1963, 35 (09) :1250-&

[2] DETERMINATION OF THE ALCOHOLIC HYDROXYL GROUP IN ORGANIC COMPOUNDS - PHTHALIC ANHYDRIDE METHOD [J].

ELVING, PJ ;

WARSHOWSKY, B .

ANALYTICAL CHEMISTRY, 1947, 19 (12) :1006-1010

[3] THE INFRARED SPECTRA OF SOME SILAZANES AND DISILAZANES [J].

FESSENDEN, R .

JOURNAL OF ORGANIC CHEMISTRY, 1960, 25 (12) :2191-2193

[4] MILD RAPID HYDROXYL DETERMINATION FOR PRIMARY ALCOHOLS [J].

FLORIA, JA ;

DOBRATZ, IW ;

MCCLURE, JH .

ANALYTICAL CHEMISTRY, 1964, 36 (11) :2053-&

[5] ACID-CATALYZED ACETYLATION OF ORGANIC HYDROXYL GROUPS [J].

FRITZ, JS ;

SCHENK, GH .

ANALYTICAL CHEMISTRY, 1959, 31 (11) :1808-1812

[6] THE PREPARATION OF SOME TRIARYLAMINOSILANES [J].

GILMAN, H ;

HOFFERTH, B ;

MELVIN, HW ;

DUNN, GE .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1950, 72 (12) :5767-5768

[7] SOME 1-NAPHTHYLSILICON COMPOUNDS [J].

GILMAN, H ;

BRANNEN, CG .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1951, 73 (10) :4640-4644

[8] THE PIPERIDINE-CATALYZED REACTION OF TRIPHENYLSILANE WITH SOME HYDROXY COMPOUNDS [J].

GILMAN, H ;

DUNN, GE ;

HARTZFELD, H ;

SMITH, AG .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1955, 77 (05) :1287-1288

[9]

KAMMERER H, 1966, MAKROMOLEKUL CHEM, V99, P49

[10]

KELLER HP, 1973, THESIS

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