论文部分内容阅读
建立了气相色谱(GC)和高效液相色谱(HPLC)测定高纯乙苯纯度的两种分析方法,并优化了检测条件。采用气相色谱-质谱(GC-MS)对乙苯中主要杂质进行定性,并通过比较杂质标准物质GC保留时间定性确认。主要杂质有苯、甲基环己烷、异丁基苯、仲丁基苯、苯乙酮。在乙苯中添加杂质标准物质,分别测定GC和HPLC两种方法杂质的校正因子,采用校正后的面积归一化法计算乙苯纯度,乙苯纯度校正后的结果与校正前的结果进行了比较。GC测定乙苯纯度结果为99.918%,RSD=1.9×10~(-3)%(n=6),主要杂质校正因子范围1.0~1.50;HPLC测定乙苯纯度结果为99.911%,RSD=2.6×10~(-3)%(n=6),主要杂质校正因子范围为0.02~0.43。两种方法简单、快速、准确,适用于高纯乙苯的纯度定值。
Two analytical methods were established for determination of purity of high purity ethylbenzene by gas chromatography (GC) and high performance liquid chromatography (HPLC), and the detection conditions were optimized. The major impurities in ethylbenzene were characterized by gas chromatography-mass spectrometry (GC-MS) and qualitatively confirmed by comparing the GC retention time of the standard reference substance. The main impurities are benzene, methylcyclohexane, isobutylbenzene, sec-butylbenzene, acetophenone. Add the standard substance of impurity in ethylbenzene, measure the correction factor of impurity of GC and HPLC respectively, calculate the purity of ethylbenzene by the corrected area normalization method, the corrected result of ethylbenzene purity and the result before correction Compare The purity of ethylbenzene by GC was 99.918%, and the RSD was 1.9 × 10 -3% (n = 6). The main impurity calibration factors ranged from 1.0 to 1.50. The purity of ethylbenzene by HPLC was 99.911% and the RSD was 2.6 × 10 ~ (-3)% (n = 6), the main impurity correction factor ranged from 0.02 to 0.43. The two methods are simple, fast and accurate, suitable for the purity of high purity ethylbenzene.