強アルカリ触媒フェノールレゾール樹脂のゲルパーミエーションクロマトグラフィー用試料調製法

概要

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A part of phenol groups in the strongly alkaline catalyst phenol resole resin (PFR) exists as a formof sodium phenoxides which makes the resin hardlysoluble in tetrahydrofuran (THF). In the presentmethod, sodium phenoxides in PFR were converted to phenols with a weak cation exchange resin, to make the resin soluble in the solvent. About 300 mg of PFR was dissolved in 0.5 ml of methanol, then thesample solution was passed through the open column packed with 4 ml of a weak cation exchange resin, Amberlite IRC-50 which is one of the carboxylic acid type cation exchangers. The eluate was introduced directly into 9 ml of THF in 50 ml flask. Finally, the cation exchange resin was eluted with 0.5 ml of methanol. 300*l of the eluate was injected into chromatograph without delay. Analytical conditions were as follows: apparatus; Toyo Soda HLC-801A, column; Toyo Soda TSK-GEL, G-3000H_8, G-2000H_8, X2, G-1000H_8, eluting solvent; THF, flow rate; 1 ml/min, detector; differential refractometer. It seemed that the influence of this procedure on the digree of condensation of PFR was fairly as small as the direct neutralization method of PFR with 2N acetic acid. However, the latter method produces sodium acetate, which gives an unfavourable effect on the column packing materials.
1982-02-05