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为了建立工作场所空气中六硝基六氮杂异伍兹烷的高效液相色谱测定方法。按照《工作场所空气中毒物检测方法的研制规范》(简称《规范》)的要求,进行实验室试验和验证试验。该方法的检出限为0.012μg/ml(进样10μl洗脱液),最低检出浓度为0.0005 mg/m3。标准曲线的相关系数r=0.9996,高、中、低3个浓度的样品,6次重复测定,相对标准偏差为0.24%~1.96%,平均洗脱效率为96.59%~104.93%,方法的回收率为98.28%~101.15%,样品在室温至少可保存14 d,六硝基六氮杂异伍兹烷的浓度为0.28~11.87 mg/m3,采样效率为98.86%~99.82%,工作场所空气中与六硝基六氮杂异伍兹烷共存的三硝基甲苯、二硝基甲苯、黑索今、奥克托今在本条件下不干扰测定。提示,本方法各项指标达到《规范》的要求,适用于工作场所空气中六硝基六氮杂异伍兹烷的检测。
To establish a method for the determination of hexanitrohexaazaisowurtzitane in the workplace by high performance liquid chromatography (HPLC). In accordance with the “workplace air poisoning detection methods for the development of norms” (“Code”) requirements, laboratory tests and verification tests. The limit of detection of this method is 0.012μg / ml (injection of 10μl eluent), the minimum detectable concentration of 0.0005 mg / m3. The correlation coefficient of standard curve was 0.9996. The samples with high, medium and low concentrations were determined by 6 replicates. The relative standard deviations were 0.24% ~ 1.96%, and the average elution efficiencies were 96.59% ~ 104.93%. The recoveries Was 98.28% ~ 101.15%. The sample was stored for at least 14 days at room temperature. The concentration of hexanitrohexaazaisowurtzitane was 0.28 ~ 11.87 mg / m3. The sampling efficiency was 98.86% ~ 99.82% Trinitrotoluene, dinitrotoluene, and black oxynitrides co-existed with nitrohexaazaisowurtzitane and octoxynol did not interfere with the assay under this condition. It is suggested that the indicators of this method meet the requirements of “norms” and be applicable to the detection of hexanitrohexaazaisowurtzitane in the air of the workplace.