纳米TiO_2生产及应用现场浓度检测方法的研究——二安替吡啉甲烷分光光度法

A novel in-situ method for analyzing nano TiO_2 particle concentration during its formulation and application—a diantipyrylmethane photometric method

为了快速、简便、准确地测定空气中纳米TiO_2的浓度,在开发利用浓硫酸-硫酸铵为吸收液高效采集方法的基础上,研究了二安替吡啉甲烷分光光度法对纳米TiO_2测定的可行性,并分析了该方法的性能。相对于消解和显色后的溶液,在390 nm条件下,该方法的最佳测量范围为1～5 mg/L,99%置信度下,标准曲线线性相关,剩余相对偏差小于0.015,检出限为0 061 3 mg/L,相对标准偏差为0.45～2.13,加标回收率为96.0%～99.4%。在4 h置放的稳定性试验中,吸光度最大极差仅为0.016。结果表明,该方法可满足空气中纳米TiO_2粉尘浓度的分析需要。

This paper aims at introducing a novel in-situ method for analyzing nano TiO2 particle concentration during its formation and application. As is known, it is very difficult to determine the content of nano TiO2 in the natural environment, which brings about the need to innovate analytic methods to promote the research concerned. For this purpose, first of all, we have studied and understood that the nano TiO2 particles are potential with serious hazards to human health 1 than the fine ones. In order to collect such particles more efficiently in the workplace, we tried to use the mixture of sulfuric acid/ammo- nium sulfate as absorbent, and analyzed the content of TiO2 by using the diantipyryl methane photometric method. The determining range as we found was then tested by using the standard curve, which reveals a good linear correlation in the concentration range of 0- 5 mg/L from the tested solution. According to the optimal absorption range of the photometric instrument, the corresponding optimal testing concentration range proves to be 1 - 5 mg/L, whereas the minimum quantitative detection limit was to be 0.061 3 mg/L. The features of relativity of the method were tested by six standard curves, with the results indicating that all the squares of the relative coefficients were above 0.999 5, which can be said the higher linear relativity at 99% confidence. And at a 95 % confidence, no significant difference was shown between the intercept and 0, which proved a quite satisfactory accuracy. The relative standard deviations were within the range of 0.45 to 2.13 at 1.00 mg/L and 0.82 to 1.21 at 4.40 mg/L, which can also be thought of high precision, much higher recoveries in the range of 96.0% - 97.0% at about 1 mg/L and 98.2% - 99.4% at about 3 mg/L. During the 4h, the absorption values almost didn＇t change at t .00 mg/L and the extreme difference was only 0.016 at 4.00 mg/L, which also means a great stability. The evaluation results prove that this method can meet the analysis of nano TiO2 aerosol. Thus, by this collection and analysis method, we have successfully obtained the data of the concentration of the nano TiO2 dust in the workplace.