首页|微波消解-ICP-OES法测定聚酯中磷含量的方法研究

微波消解-ICP-OES法测定聚酯中磷含量的方法研究

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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 1 300 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2.6 μg/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.
Study on the determination of phosphorus in polyester by microwave digestion ICP-OES method
The microwave digestion ICP-OES method was used to measure the phosphorus content of polyes-ter 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 diges-tion solution was transparent and clear.The ideal parameters for ICP-OES's operation were as follows:radial obser-vation mode,phosphorus analysis spectral line of 213.617 nm,radio frequency power of 1 300 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 2.6 μg/g,its recovery rate ranged from 92.5%to 104.6%,and its RSD value was less than 5.5%.The results of the detec-tion demonstrated good accuracy and repeatability,and they were able to satisfy the requirements for phosphor-us content detection in polyester.

polyesterinductively coupled plasma emission spectrometermicrowave digestionphosphor-us content

周丽华、马平平

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中国石化仪征化纤有限责任公司研究院,江苏仪征 211900

江苏省高性能纤维重点实验室,江苏仪征 211900

聚酯 电感耦合等离子体发射光谱仪 微波消解 磷含量

2024

合成技术及应用
中国石化仪征化纤股份有限公司

合成技术及应用

影响因子:0.204
ISSN:1006-334X
年,卷(期):2024.39(1)
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