连续流动分析法测定二醋酸纤维素丝束中二氧化钛

Determination of TiO_2 in cellulose acetate tow by continuous flow analysis

建立了连续流动分析法测定烟用二醋酸纤维素丝束中二氧化钛(Ti O2)含量的方法。采用经微波消解后样品溶液中的钛离子与二安替比林甲烷显色反应的原理进行方法开发,并对流动分析仪管路设计以及温度、时间、流动相酸度等影响因素进行了探讨。结果表明:(1)经改进设计的流动分析管路模块在室温条件下以0.8:1体积比的盐酸为流动相,混合反应3 min左右,于420 nm检测波长处可获得较为灵敏的仪器检测信号;(2)钛离子的检出限0.04μg/mL,定量限0.14μg/mL,回收率97.8%～105.6%,重复性RSD≤3%;(3)该方法与现行行标(YC/T 169.11—2009)检测结果的差异无统计学意义。

In this study,the content of TiO2 in cellulose acetate tow for cigarette was determined by continuous flow analytical method(CFA).The method is based on chromogenic reaction of DAM and titanium(IV)which is contained in sample solution dissolved by microwave.Pipeline design of flow analyzer as well as factors such as mixing temperature,mixing time and acidity of mobile phase were investigated.Results showed that:(1)Under condition of room temperature,mixed reaction time of 3 min,and with hydrochloric acid(volume ratio of 0.8:1)as mobile phase,the redesigned flow line module of CFA could obtain more sensitive detection signals at 420nm wave length;(2)The LOD for titanium(IV)was 0.04μg/mL and LOQ was 0.14μg/mL with RSD≤3%,and the recovery was within the range of 97.8%~101.5%;(3)Results by CFA method were similar to those obtained by method of YC/T 169.11-2009.