科学研究

差示扫描量热单峰法测定二苯并(b,f)-1,4-氧氮吖庚因纯度

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  • 1.中北大学,太原038507;
    2.国民核生化防护国家重点实验室,北京102205;
    3.军事科学院化学防护所,北京102205;
    4.陆军防化驻太原地区军事代表室,太原030000
段晶钟(1995-),男,硕士研究生,主要研究方向为危险化学品分析检测。

收稿日期: 2021-01-28

  修回日期: 2021-05-07

  网络出版日期: 2021-08-19

基金资助

国家自然科学基金(21876202)

Purity determination of dibenz(b,f)-1,4-oxaxepin by monopeak method at differential scanning calorimetry

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  • 1. North University of China,Taiyuan 038507;
    2. State Key Laboratory of NBC Protection for Civilian,Beijing 102205;
    3. Research Institute of Chemical Defense,Acadmy of Military Sciences,Beijing 102205;
    4. Chemical Defense Military Delegate Office of Army Armament Department in Taiyuan,Taiyuan 030000

Received date: 2021-01-28

  Revised date: 2021-05-07

  Online published: 2021-08-19

摘要

利用差示扫描量热单峰法开展了二苯并(b,f)-1,4-氧氮吖庚因的纯度分析。通过优化升温速率和样品质量,获得了最佳实验条件为:升温速率1.0℃/min,样品质量2.50~3.50mg。测得的二苯并(b,f)-1,4-氧氮吖庚因纯度平均值为99.35%,相对标准偏差(RSD)为0.033%(n=5)。与高效液相色谱(HPLC)法和核磁共振氢谱(1H-NMR)法的测试结果进行比较,相差不大。差示扫描量热单峰法简单、快速,准确度高,可作为二苯并(b,f)-1,4-氧氮吖庚因生产过程中产品的质量控制方法。

本文引用格式

段晶钟, 刘斐, 武惠恩, 张远鹏, 汪海涛, 李斌 . 差示扫描量热单峰法测定二苯并(b,f)-1,4-氧氮吖庚因纯度[J]. 化工新型材料, 2021 , 49(7) : 133 -137 . DOI: 10.19817/j.cnki.issn 1006-3536.2021.07.031

Abstract

The purity of Dibenz(b,f)-1,4-oxaxepin was analyzed by monopeak method at differential scanning calorimetry.By optimizing the heating rate and the sample quality,the best experimental conditions were obtained:the heating rate was 1.0℃/min,and the sample quality was 2.5~3.5mg.The measured Dibenz(b,f)-1,4-oxaxepin purity was 99.35%,and the RSD was 0.033%(n=5).Compared with the test results of high performance liquid chromatography and nuclear magnetic resonance,there was not much difference.The monopeak method of differential scanning calorimetry was simple,fast and highly accurate,and can be used as a quality control method for products in the Dibenz(b,f)-1,4-oxaxepin production process.

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