微波消解-ICP-OES法测定聚酯中磷含量的方法研究

Study on the determination of phosphorus in polyester by microwave digestion ICP-OES method

为了监控聚酯生产中含磷添加剂的含量,采用微波消解-电感耦合等离子体发射光谱(ICP-OES)法测定聚酯中磷含量,选择消解剂的种类和用量,优化ICP-OES工作条件参数。结果表明:选择3 mL硫酸和3 mL硝酸微波消解聚酯试样,制得消解液澄清透明;ICP-OES最佳工作条件为磷分析谱线213.617 mm,射频功率1300 W,雾化气流速0.55 L/min,观测高度15 mm,蠕动泵泵速1.5 mL/min,观测方式为径向。在优化的ICP-OES工作参数下,测定聚酯中磷含量的检出限为2.6μg/g,相对标准偏差RSD值小于5.5%,加标回收率为92.5%~104.6%,检测结果具有较好重复性和准确度,能够满足聚酯中磷含量的检测需求。

The microwave digestion ICP-OES method was used to measure the phosphorus content of polyester in order to track the amount of phosphorus additives used in the production process.The ICP-OES s operating parameters were optimized along with the digestion agent s type and dosage.Based on the results,3 mL of sulfuric acid and 3 mL of nitric acid were chosen to microwavely digest the polyester samples.The generated digestion solution was transparent and clear.The ideal parameters for ICP-OES s operation were as follows:radial observation mode,phosphorus analysis spectral line of 213.617 nm,radio frequency power of 1300 W,atomizing gas flow rate of 0.55 L/min,observation height of 15 mm,peristaltic pump speed of 1.5 mL/min.With the ICP-OES operating parameters optimized,the method s detection limit for phosphorus content in polyester was 2.6μg/g,its recovery rate ranged from 92.5%to 104.6%,and its RSD value was less than 5.5%.The results of the detection demonstrated good accuracy and repeatability,and they were able to satisfy the requirements for phosphorus content detection in polyester.