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本文叙述了测定合成皂用脂肪酸的气相色谱法,着重饱和脂肪酸的定量。用作标准的奇碳脂肪酸(C_9—C_19)系自行合成的,色谱柱和聚酯类液相亦为自制,方法为先将标准酸和皂用脂肪酸试样进行甲酯化,先后在Apiezon L柱(240℃)和聚1,3-丁二醇丁二酸酯(PBDS)柱(200℃),以及在聚乙二醇己二酸酯(PEGA)柱,于两种翟序升温的条件下进行定性分离,在Apiezon L柱上得到的保留数据和文献查得值核对基本一致。定量系采用(PEGA)柱,在柱温150—210℃,2℃/分,N_2流速127毫升/分的条件下,在氢焰离子化鉴定器上,以不加校正峯面积百分比定量。结果表明,对标准酸的分析误差平均为±3.47％,并测得了上海制皂厂生产的合成皂用脂肪酸含有C_8—C_21共14个组分,按照定量结果计算的酸值和化学法测得的数据相比,结果能很好相符。
This article describes the gas chromatography for the determination of fatty acids for synthetic soaps, focusing on the quantification of saturated fatty acids. The odd-carbon fatty acid (C_9-C_19) used as a standard was self-synthesized. The column and the polyester-based liquid phase were also self-made by methylating the standard acid and soap fatty acid samples first and then successively in Apiezon L (240 ° C) and poly (1,3-butylene succinate) (PBDS) columns (200 ° C), as well as on polyethylene glycol adipate (PEGA) Under the qualitative separation, the retention data obtained on the Apiezon L column and the literature check value is basically the same. The quantification was carried out on a hydrogen flame ionization detector at a column temperature of 150-210 ° C, 2 ° C / min and a N 2 flow rate of 127 ml / min using a PEGA column. The results showed that the average error of analysis of standard acid was ± 3.47%, and 14 components of fatty acid containing C_8-C_21 of soap soap produced by Shanghai Soap Factory were measured. According to the acid value and chemical method calculated by quantitative results Compared to the data, the results can be very good match.