臭氧氧化对废水中RDX分光光度测试的影响因素

发布时间：2017-12-27 06:23

本文关键词：臭氧氧化对废水中RDX分光光度测试的影响因素　出处：《含能材料》2017年09期 　论文类型：期刊论文

【摘要】：为研究臭氧(O_3)氧化后废水中环三亚甲基三硝胺(RDX)分光光度测试的干扰因素,进行了一系列的探索性实验。借助秩和检验和F检验,估计了分光光度法和高效液相色谱法(HPLC)测定的RDX数据间的系统误差。对比了分光光度法和HPLC得到的O_3氧化前后的废水及标准溶液中的RDX数据。用液相色谱-质谱联用(LC/MS)、气相色谱-质谱联用(GC/MS)检测了可能的干扰物质。分析引起RDX分光光度测试结果误判的原因。结果表明,在给定的显著性水平α=0.05下,两种方法测得的RDX数据间不存在系统误差。RDX废水中的有机物质经O_3氧化可产生甲醛,对分析结果产生干扰,但这部分甲醛可通过样品预处理进行有效去除。同时,O_3氧化不能将RDX彻底矿化,产生了低分子量的中间体,亚甲基二硝胺、二羟甲基硝胺以及6-硝基-2,4,6-三氮杂-3,5-二氧-己醛等。其中,亚甲基二硝胺和二羟甲基硝胺等胺类中间产物可与浓硫酸发生类似RDX的分解反应生成甲醛,成为干扰RDX分光光度测量的直接影响因素。
[Abstract]:A series of exploratory experiments were carried out to study the interference factors of the spectrophotometric determination of methyl three nitramine (RDX) in the wastewater of Sanya after the oxidation of ozone (O_3). By means of rank sum test and F test, the systematic error between RDX data measured by spectrophotometric method and high performance liquid chromatography (HPLC) was estimated. The RDX data in the wastewater and the standard solution before and after O_3 oxidation were compared with the spectrophotometric method and HPLC. The possible interfering substances were detected by liquid chromatography-mass spectrometry (LC/MS) and gas chromatography-mass spectrometry (GC/MS). The reasons for the misjudgement of the RDX spectrophotometric test results were analyzed. The results show that, under the given significant level of alpha =0.05, there is no systematic error between the RDX data measured by the two methods. The organic matter in RDX wastewater can be oxidized by O_3 to produce formaldehyde, which can disturb the analysis result, but this part of formaldehyde can be effectively removed by sample pretreatment. At the same time, the oxidation of O_3 RDX cannot be completely mineralized. The intermediate low molecular weight, methylenedinitramine, dimethylol nitramine and 6- nitro -2,4,6- three aza -3,5- two oxygen - hexaldehyde etc.. The decomposition reaction of formaldehyde methylenedinitramine and dimethylol nitramine and amine intermediates can occur similar to RDX with concentrated sulfuric acid, become the direct influencing factor interference RDX spectrophotometric measure.
【作者单位】：中国工程物理研究院化工材料研究所;四川大学化学学院;
【分类号】：O657.3;X832
【正文快照】： 1引言环三亚甲基三硝胺(RDX)具有爆轰性能优异、感度适中、安定性好等优点,在军事和民用方面得到广泛应用。随着其规模化生产及应用,会产生大量含RDX的有害废水,存在环境污染风险。RDX具有致癌致畸性,世界各国对RDX的排放要求日趋严格,我国弹药装药行业对RDX废水的排放标准[1]

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