目的:建立直接进样气相色谱法测定微量乙酸乙酯含量的分析方法。方法:通过对仪器参数进行优化,包括进样口温度、初始柱温、柱流速、分流比,确定最佳分析条件:色谱柱SH-PolarWax(30 m×0.32 mm 0.25μm),程序升温:初始温度为45℃,保...目的:建立直接进样气相色谱法测定微量乙酸乙酯含量的分析方法。方法:通过对仪器参数进行优化,包括进样口温度、初始柱温、柱流速、分流比,确定最佳分析条件:色谱柱SH-PolarWax(30 m×0.32 mm 0.25μm),程序升温:初始温度为45℃,保持4min,以10℃/min升温至90℃,再以20℃/min升温至200℃;进样口温度220℃,分流比10∶1,流速1.00 m L/min。结果:在优化的色谱条件下,微量乙酸乙酯测试方法在0.01~1.00μg/mL范围内线性良好,相关系数(r)大于0.999,回收率在90%~110%范围内,RSD(n=3)均小于5%,检出限为0.004μg/mL,定量限为0.012μg/mL。结论:该方法具有检测时间短、灵敏度高的特点,研究结果可为乙酸乙酯含量检测方法研究提供数据支撑和参考。展开更多
The external calibration in conjunction with internal standardization(ECIS) coupled with laser-induced breakdown spectroscopic(LIBS) technique was proposed to perform the quantitative analysis of Fe content in iro...The external calibration in conjunction with internal standardization(ECIS) coupled with laser-induced breakdown spectroscopic(LIBS) technique was proposed to perform the quantitative analysis of Fe content in iron ore The plasma temperature and the electron number density were calculated to prove that the plasma was under local thermodynamic equilibrium(LTE) conditions and to ensure that the integral intensities of Fe I lines were reasonable. In addition, the result of the quantitative analysis shows a content of (20.26±0.59)% by mass of Fe in the iron ore. It was determined by four calibration curves, drawn for four emission lines of Fe I(373.48, 373.71,404.58 and 438.35 nm) normalized by Mn I line, base on the ECIS method which can eliminate the influence of matrix effect and improve the accuracy of quantitative analysis, compared with the standard addition method. Both the results of these two analytical methods were compared with that listed in the Standard Substance Certificate. The percentage content of Fe in the same sample of iron ore by the ECIS method was (20.17±0.08)% by mass, which shows a good performance to analyze the Fe content of iron ore in combination with LIBS.展开更多
文摘目的:建立直接进样气相色谱法测定微量乙酸乙酯含量的分析方法。方法:通过对仪器参数进行优化,包括进样口温度、初始柱温、柱流速、分流比,确定最佳分析条件:色谱柱SH-PolarWax(30 m×0.32 mm 0.25μm),程序升温:初始温度为45℃,保持4min,以10℃/min升温至90℃,再以20℃/min升温至200℃;进样口温度220℃,分流比10∶1,流速1.00 m L/min。结果:在优化的色谱条件下,微量乙酸乙酯测试方法在0.01~1.00μg/mL范围内线性良好,相关系数(r)大于0.999,回收率在90%~110%范围内,RSD(n=3)均小于5%,检出限为0.004μg/mL,定量限为0.012μg/mL。结论:该方法具有检测时间短、灵敏度高的特点,研究结果可为乙酸乙酯含量检测方法研究提供数据支撑和参考。
基金Supported by the China Instrumentation Program(No.2011YQ030113) and the National Natural Science Foundation of China (Nos.21175106, 21375105).
文摘The external calibration in conjunction with internal standardization(ECIS) coupled with laser-induced breakdown spectroscopic(LIBS) technique was proposed to perform the quantitative analysis of Fe content in iron ore The plasma temperature and the electron number density were calculated to prove that the plasma was under local thermodynamic equilibrium(LTE) conditions and to ensure that the integral intensities of Fe I lines were reasonable. In addition, the result of the quantitative analysis shows a content of (20.26±0.59)% by mass of Fe in the iron ore. It was determined by four calibration curves, drawn for four emission lines of Fe I(373.48, 373.71,404.58 and 438.35 nm) normalized by Mn I line, base on the ECIS method which can eliminate the influence of matrix effect and improve the accuracy of quantitative analysis, compared with the standard addition method. Both the results of these two analytical methods were compared with that listed in the Standard Substance Certificate. The percentage content of Fe in the same sample of iron ore by the ECIS method was (20.17±0.08)% by mass, which shows a good performance to analyze the Fe content of iron ore in combination with LIBS.