用微波消解样品-电感耦合等离子体原子发射光谱法测定几种阻燃纤维材料中磷的含量.探讨了消解条件的选择以及干扰情况,试验结果表明:在253.561 nm波长处存在材料中添加的消光剂二氧化钛产生的钛线的强烈干扰,微量铜对磷213.618 nm也有强烈干扰,选择波长214.914 nm的谱线可有效避免铜、钛等杂质元素的干扰,磷的标准曲线也无须做基体匹配;在硫酸-过氧化氢-硝酸体系下,采用高温(230 ℃)高压(4.0 MPa)微波密闭消解,可以获得较好的消解效果.方法的检出限(3σ)为36.0 μg·L-1,加标回收率在83.8%~107.8%范围,相对标准偏差(n=10)小于2%.

Sample of flame-retardant fiber was digested with a mixture of H2SO4,HNO3 and H2O2 in a closed PTFE vessel,heated at 230 ℃ and under the pressure of 4.0 MPa by using the microwave sample digestor.The solution obtained was used for ICP-AES determination of phoshporus.Among the 3 spectral lines tested (i.e.,213.618 nm,214.914 nm and 253.561 nm),serious interferences due to titanium(Ⅳ) and traces of Cu(Ⅱ) were encountered when the spectral lines of 253.561 nm and 213.618 nm were chosen as the analytical lines,and the interferences were effectively eliminated by choosing the spectral line of 214.914 nm as analytical line.It was also shown that under the optimum condition,matrix matching was not necessary in the preparation of standard curve of phosphorus.Detection limit (3σ) of the method was found to be 36.0 μg·L-1.Tests for recovery and precision were made,giving results of recovery in the range from 83.8% to 107.8% and RSD′s (n=10) less than 2%.