CHINESE JOURNAL OF ENERGETIC MATERIALS
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亲水色谱-质谱联用分析硝酸羟乙基肼含量
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北京航天试验技术研究所, 北京 100074

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国防科工局技术基础科研项目(JSJL2016203B042)


Determination of Hydroxyethyl Hydrazine Nitrate by Hydrophilic Interaction Chromatography Coupled with Mass Spectrometry
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Beijing Institute of Aerospace Testing Technology, Beijing 100074, China

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    摘要:

    针对新型液体推进剂中硝酸羟乙基肼含量的分析需要,研发了一种基于亲水相互作用色谱-质谱联用的硝酸羟乙基肼含量分析方法。分别考察了流动相组成、质谱测定等分析条件对分离效果、分析时间、检测灵敏度的影响,优化得到了适合于硝酸羟乙基肼分析的液相色谱-质谱分析条件。所建立的分析方法在0.01~0.1 μg·mL-1的样品浓度范围内相关系数R2=0.9991,检出限为1.2 ng·mL-1。方法具有良好的准确度和精密度,对浓度分别为0.0250和0.0900 μg·mL-1的HEHN溶液进行测定,回收率分别为98.1%和97.7%,相对标准偏差≤1.6%。利用该方法对一液体推进剂实际样品中的硝酸羟乙基肼含量进行测定,测定结果为12.5%±0.3%,与配制值12.9%相符。

    Abstract:

    A method based on hydrophilic interaction chromatography (HILIC) coupled with mass spectrometry (MS) was developed for determination of hydroxyethyl hydrazine nitrate (HEHN). The effects of the composition of mobile phase and parameters for MS detection were investigated on the optimization of chromatography separation, time required for analysis, and detection sensitivity. Good linearity is obtained under the concentration range of 0.01-0.1 μg·mL-1 with R2=0.9991, and the limit of detection of 1.2 ng·mL-1. Recovery of two HEHN samples with concentration of 0.0250 and 0.0900 μg·mL-1 is determined as 98.1% and 97.7%, respectively, while relative standard deviation (RSD) is no more than 1.6%, indicating good precision of the method. A real sample of liquid propellant is determined by this method, and the content of HEHN measured as 12.5%±0.3% is in accordance with the prepared concentration of 12.9%.

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引用本文

徐林楠,张学军,赵坦,等.亲水色谱-质谱联用分析硝酸羟乙基肼含量[J].含能材料, 2020, 28(9):936-941. DOI:10.11943/CJEM2019325.
XU Lin-nan, ZHANG Xue-jun, ZHAO Tan, et al. Determination of Hydroxyethyl Hydrazine Nitrate by Hydrophilic Interaction Chromatography Coupled with Mass Spectrometry[J]. Chinese Journal of Energetic Materials, 2020, 28(9):936-941. DOI:10.11943/CJEM2019325.

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历史
  • 收稿日期: 2019-12-28
  • 最后修改日期: 2020-06-14
  • 录用日期: 2020-05-08
  • 在线发布日期: 2020-05-26
  • 出版日期: 2020-09-25