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气相色谱-串联质谱法测定水中硝酸羟胺含量OA

Determination of Hydroxylamine Nitrate in Water by GC-MS

中文摘要英文摘要

针对分光光度法和滴定法在分析含能材料生产废水中硝酸羟胺含量存在的灵敏度低、选择性差等问题,开发了一种基于气相色谱-串联质谱(GC-MS)的高灵敏度分析方法,用于测定水体中痕量硝酸羟胺.通过丙酮衍生化,硝酸羟胺与丙酮反应生成易于气相色谱测试的丙酮肟,并优化衍生化条件及GC-MS参数,以N,N-二甲基亚硝胺(NDMA)为内标进行定量分析.实验结果表明,硝酸羟胺在线性范围内线性关系良好(R2>0.999),检出限为0.015 mg·L-1,加标回收率为95%~108%,相对标准偏差为3.6%~5.7%.本方法成功应用于工业废水的分析,具有操作简便、灵敏度高、抗干扰能力强等优点,为环境水体中硝酸羟胺的监测提供了一种高效、准确的分析手段.

Aiming at the problems of low sensitivity and poor selectivity of spectrophotometry and titration in the analysis of hy-droxylamine nitrate content in energetic material production wastewater,a high sensitivity analysis method based on gas chroma-tography tandem mass spectrometry(GC-MS)was developed for the determination of trace hydroxylamine nitrate in water.Through acetone derivatization,hydroxylamine nitrate reacted with acetone to produce acetone oxime which was easy to be test-ed by gas chromatography.The derivatization conditions and GC-MS parameters were optimized,and N,N-dimethylnitrosamine(NDMA)was used as the internal standard for quantitative analysis.The results showed that the linear relationship of hydroxyl-amine nitrate in the linear range(R2>0.999)was good,the detection limit was 0.015 mg·L-1,the recovery rate was 95%-108%,and the relative standard deviation was 3.6%-5.7%.This method has been successfully applied to the analysis of industrial waste water.It has the advantages of simple operation,high sensitivity and strong anti-interference ability.It provides an efficient and accurate analytical method for the monitoring of hydroxylamine nitrate in environmental water.

赵坦;甄江涛;李俊;贾冬雪

北京航天试验技术研究所,北京 100074北京航天试验技术研究所,北京 100074北京航天试验技术研究所,北京 100074北京航天试验技术研究所,北京 100074

军事科技

硝酸羟胺衍生化气相色谱-串联质谱

hydroxylamine nitratederivatizationGC-MS

《含能材料》 2026 (8)

964-969,6

10.11943/CJEM2026107

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