ペーパークロマトグラフによる老化防止剤の識別について
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概要
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The paper chromatographic behaviour of the following antioxidants has been investigated.<BR>A. Aldol-α-naphthylamine (M. P. 65100°C) <BR>C. Aldol-α-naphthylamine (M. P. 140°C min) <BR>P. A. Phenyl-α-naphthylamine<BR>D. Phenyl-β-naphthylarnine<BR>F. Di-β-naphthyl-p-phenylenediamine<BR>H. N, N-diphenyl-p-phenylenediamine<BR>Agerire Stalite Mixture of mono and di-hepthlated diphenylamine<BR>Agrite Resin D. Polymerized trimethyl-dihydroquinoline<BR>Santoflex B. 1.2. -dihydro-2, 2, 4-trimethyl-6 phenylquinoline<BR>Santoflex BX Blend of Santoflex B (85) +H (15).<BR>After antioxidants (dissolved in acetone) were coupled with diazonium salt of aniline, reaction products were developed on paper strip (Toyo paper strip for Chromatography No.50) up to about 30 cm high. and then, after drying at room temperature, paper strip was treated with conc HCI vapor in order to observe developing spots having Specific colour.<BR>As developers a number of solvents and solvent mixtures were investigated.<BR>Acetone-benzene-water (61 : 4 : 35 by volume at 20°C) -was finally chosen as a best developer for separation and identification of antioxidants.<BR>The following paper chromatographic data were obtained on antioxidants alone. (Table 1) <BR>Table 1.<BR>Paper chromatographic data of various an-tioxidants (developed at 20°C) <BR>Developer. Aceton-Benzene-Water<BR>61 - 4 - 35<BR>(by volume at 20°C) <BR>Antioxiodants R<SUB><I>f</I></SUB> × 100 Specific Colour of Spot<BR>A 90, 78 Reddish Violet<BR>C 90, 78 Reddish Violet<BR>P A 61 Bluish Violet<BR>D 48 Orange<BR>F 98100 Pinkpale orange<BR>H 98100 Pinkpale brown<BR>Agerite stalite 37 (5052) Violet<BR>Santoflex B 49 Pink<BR>Agerite Resin D. 060 Pale Pink diffuse zone<BR>(a) A and C showed over laped spot.<BR>(b) H and F also showed oved laped spot<BR>(c) Agerite Resin D gave diffuse zone.<BR>(d) D and Santoflex B mutually interfered.<BR>With the above chromatographic deta as a guide, further experiment was carried out in order to detect and identify of antioxidants which are present in mixed state. It was possible to separate and identify component antioxidant in A+PA+D, A+H+PA, F+Agerite resin D, C+D, F +Agedite stalite etc, <BR>Therefore, it would be expected that the proposed method provides a very convenient means for identification of antioxidant mixture. when A and C or H and F. or D and Santoflex B are not present together with in the mixture.<BR>Based on the results obtained on above-mentioned experiments, the identification of antioxidants was carried out with tread mix accelerated with MBT and tube mix accelerated with MBTS.<BR>Vulcanized Rubber (5 g) grinded by passing through rolls was extracted with acetone (10 cc) at room temp. and acetone extract was evaporated to 2cc, then it was treated by the some method as antioxidants in acetone were treated.<BR>The chromatographic treatment has been successfully applied to the vulcanized rubber. Chromatographic data obtained were quite similar to the data of antioxidants in free state.<BR>The only exception was Santoflex B which was not detected.<BR>Paper chromatographic method proposed in this experiments could be applied successfully to the identification of antioxidants either alone or in vulcanized rubber accelerated with MBT and MBTS. But more precise and general method could be developed by finding diazonium salt and developer which gives more specific spot and colour than diazonium salt of aniline and developer proposed in this experiment does.