气相色谱内标法测定硅片切割液中一缩二乙二醇含量

Determination of Diethylene Glycol in Cutting Fluid for Silicon Wafer by Gas Chromatography with Internal Standard Method

采用气相色谱内标法,GC950型气相色谱仪汽化和检测温度均设为260℃,柱前压设为0.03MPa,柱温程序设为:150℃保留2min,以25℃/min速率升到260℃,保留10min。结果表明,1,2-丙二醇与一缩二乙二醇(DEG)的保留时间(色谱峰位置)最接近且两者分离良好,可作为定量分析切割液中DEG的内标物。5次平行测定得到1,2-丙二醇与DEG的相对校正因子平均值为1.114,不同加标浓度水平下DEG的平均回收率为98%～99%,RSD为2.8%～6.0%。测得某切割液中DEG质量分数平均值为73.7%,日内与日间标准偏差分别为1.1和2.2,日内与日间RSD分别1.4%和3.0%。该方法准确可靠、精密度高且重现性好,操作误差在允许范围之内。

The determination of diethylene glycol（DEG） in cutting fluid for silicon wafer was accomplished by gas chromatography with internal standard method.A gas chromatography（GC 950,Shanghai Haixin） was used and its vaporization temperature,detection temperature and pre-column pressure were set at 260℃,260℃ and 0.3 MPa,respectively.The initial temperature of column oven was kept at 150℃ for 2 min,and the temperature was increased to 260℃ at a rate of 25 ℃/min and was then held for 10 min at 260℃.The results showed that 1,2-propanediol was completely separated from DEG in GC column and its retention time was the nearest to DEG,so it was the most suitable internal standard.The average values of relative correction factor,coefficient of recovery and within-day RSD（n=5） were 1.114,98%~99% and 2.8%~6.0%,respectively.The average mass fraction of DEG was 73.7%,furthermore,the within-day and between-day standard deviation were 1.1 and 2.2,and their RSD were 1.4% and 3.0%,respectively.The experimental results obtained by this method have good accuracy,precision and reproducibility,and the error of experiment was acceptable.