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基于铁酸钴(CoFe2O4)纳米材料催化硫化铵的氧化反应产生化学发光的现象,建立了一种检测空气中痕量硫化铵的催化发光气体传感器.在对合成的3种材料的催化发光性质进行比较的基础上,对分析方法条件进行了优化,其结果表明:在检测波长400 nm、反应温度306℃、载气流速400 mL/min的最优条件下,可测定的硫化铵浓度的线性范围为0.13～13 mg/L(r=0.9951,n=9),检出限为0.04 mg/L(3σ),对1.3 mg/L的硫化铵连续平行测定8次,其相对标准偏差为1.8%.此外,考察了相同浓度的常见挥发性有机物的干扰情况,其结果表明该传感器具有很好的选择性.连续60 h通过1.3 mg/L的硫化铵,发光强度无明显降低,相对标准偏差小于5%,表明此传感器使用寿命长.并将该传感器成功用于人工合成样品的分析,回收率为94.7%～103.9%.
A catalytic luminescence gas sensor for the determination of trace ammonium sulphide in air was developed based on the phenomenon of chemiluminescence generated by the oxidation of ammonium sulphide catalyzed by cobalt ferrite (CoFe2O4) nanomaterials. The catalytic luminescence properties of the synthesized three materials were studied The results show that the linear range of measurable concentration of ammonium sulphate under the optimal conditions of the detection wavelength of 400 nm, the reaction temperature of 306 ℃ and the carrier gas flow rate of 400 mL / min The detection limit was 0.04 mg / L (3σ), and the relative standard deviation was 1.8% for the continuous determination of 1.3 mg / L ammonium sulphate for eight times in the range of 0.13-13 mg / L (r = 0.9951, n = 9) In addition, the interference of common volatile organic compounds with the same concentration was investigated, and the results showed that the sensor had good selectivity.It did not decrease the luminescence intensity of 1.3 mg / L ammonium sulphide continuously for 60 h, and the relative standard deviation was less than 5%, indicating that the sensor has a long service life and the sensor was successfully used in the analysis of synthetic samples, the recovery rate was 94.7% ~ 103.9%.