基于红外光谱法的工业水合肼鉴别及快速测定
Identification and Rapid Determination of Industrial Hydrazine Hydrate Based on Infrared Spectroscopy
刘鹏鲲 1马玲 1张文乐 1朱侠 1郝瑞瑞2
作者信息
- 1. 乌鲁木齐海关技术中心 乌鲁木齐 830000
- 2. 新疆大学 乌鲁木齐 830000
- 折叠
摘要
本文运用红外光谱法(Infrared Spectroscopy,IR)和气相色谱-质谱联用法(Gas Chromatography-Mass Spectrometry,GC-MS)对工业水合肼进行鉴别及快速测定.根据水合肼在 1550～1650 cm-1、3100～3600 cm-1 处有N-H变形振动、N-H伸缩振动和O-H伸缩振动等红外吸收特征对工业水合肼进行初步鉴别.GC-MS全扫描模式,水合肼的总离子流图(TIC)中仅存在1个明显峰,分析该峰为联胺,对工业水合肼进行进一步鉴别.此外,建立红外光谱法测定工业水合肼中水合肼含量的方法.选择水合肼的N-H变形振动吸收作为红外特征吸收峰,采用外标法定量,该方法工作曲线线性相关系数(r)为 0.9968;相对标准偏差(RSD)为 1.0%～1.9%;通过与HG/T 3259-2012《工业水合肼》中容量滴定法测定结果对比,两种方法测定结果的相对偏差为0.08%～0.61%.结果表明,红外光谱法具有准确、快速、无损、环保的优点,适用于工业水合肼鉴别和水合肼含量的测定.
Abstract
Infrared spectroscopy(IR)and gas chromatography-mass spectrometry(GC-MS)were used to identify and rapid determinate industrial hydrazine hydrate in the paper.Industrial hydrazine hydrate was preliminarily identified according to the infrared absorption characteristics of hydrazine hydrate at 1550-1650 cm-1 and 3100-3600 cm-1 with N-H deformation vibration,N-H expansion vibration and O-H expansion vibration.Industrial hydrazine hydrate was further identified by GC-MS.Only one obvious peak existed in the total ion chromatography(TIC)of hydrazine hydrate with full-scan mode,and analysis showed that the peak was hydrazide.In addition,a method for the determination of hydrazine hydrate content in industrial hydrazine hydrate by infrared spectroscopy was established.The absorption of the N-H deformation vibration of hydrazine hydrate was selected as the infrared characteristic absorption peak.Using the external standard method for quantification,the linear correlation coefficient(r)of the working curve was 0.9968.The relative standard deviation(RSD)of hydrazine hydrate samples was 1.0%-1.9%.By comparing measurement results with volumetric titration method in HG/T 3259-2012,the relative deviation(RD)of the two methods was 0.08%-0.61%.The results show that,owing to its advantages of accuracy,rapidity,non-destructive and environmental protection,infrared spectroscopy is suitable for the identification of industrial hydrazine hydrate and the determination of hydrazine hydrate content.
关键词
工业水合肼/红外光谱法(IR)/气相色谱-质谱联用法(GC-MS)/鉴别/快速测定Key words
industrial hydrazine hydrate/infrared spectroscopy(IR)/gas chromatography-mass spectrometry(GC-MS)/identification/rapid determination引用本文复制引用
出版年
2024
NETL
NSTL
万方数据