摘要
介绍了红外光谱(IR)分析过程中常用的测试方法以及与之匹配的样品制备方法,总结了常用的样品制备方法的操作注意事项和优缺点。选取了5种常用的固相或液相的炼化原料及产品作为分析对象,比较采用不同的IR测试方法和样品制备方法所带来的谱图结果上的差异,以寻求谱图质量更高、操作更简单、成本更低的样品制备方法。实验表明:衰减全反射(ATR)测得的IR谱图基线更为平整,能很好地保留高密度聚乙烯的原始结晶形态,满足对样品定性分析的需求;对于易吸湿的硬脂酸钙,石蜡油研磨法操作简便,能有效阻隔样品与水气的接触,有利于获得高质量的IR谱图;有挥发性的丙酮用液膜法制样,采用双片一次性KBr压片替代费用较高的KBr窗片,既减小了样品挥发对IR谱图质量的影响,又降低了分析成本,是很实用的液体制样改进方法。
Commonly used testing methods and the corresponding sample preparation methods in the process of infrared spectroscopy(IR)analysis were introduced,the operation notice,advantages and disadvantages of the commonly used sample preparation methods were summarized.Five kinds of commonly used solid phase or liquid phase refining raw materials and products were selected as analysis objects to compare the differences in spectrum results caused by different IR spectrum test methods and sample preparation methods,in order to find a sample preparation method with higher spectrum quality,simpler operation and lower cost.The experimental results showed that the baseline of the IR spectrum measured by attenuated total reflection(ATR)was smoother,and the original crystalline morphology of high density polyethylene could be well retained to meet the needs of qualitative analysis of the sample.For hygroscopic calcium stearate,paraffin oil grinding method was easy to operate,could effectively block the contact between the sample and water vapor,was conducive to obtaining high-quality IR spectra;The sample of volatile acetone was prepared by liquid film method.The high cost KBr window was replaced by double disposable KBr tablet,which not only reduced the influence of sample volatilization on the quality of IR spectrum,but also reduced the analysis cost.It was a very practical improved method of liquid sample preparation.
作者
弥迟芳
石朴
刘慧杰
梅丹丹
刘文超
韩春来
MI Chi-fang;SHI Pu;LIU Hui-jie;MEI Dan-dan;LIU Wen-Chao;HAN Chun-Lai(PetroChina Fushun Petrochemical Company Research Institute,Fushun Liaoning 113004,China;Fushun Special Equipment Supervision and Inspection Institution,Fushun Liaoning 113000,China)
出处
《当代化工》
CAS
2023年第3期743-747,共5页
Contemporary Chemical Industry
关键词
红外光谱分析
样品制备方法
ATR
谱图质量
Infrared spectroscopy analysis
Sample preparation methods
ATR
Quality of spectrum
