X射线荧光光谱法测定聚酯中红磷阻燃剂总磷含量

Determination of Total Phosphorus Content of Red Phosphorus Flame Retardant in Polyester by Energy Dispersive X-Ray Fluorescence Spectrometery

利用能量散射X射线荧光光谱法(ED-XRF)快速测定聚酯纤维或切片中红磷阻燃剂总磷含量,即先对聚酯纤维或切片进行简单预处理(熔片),然后使用X射线荧光光谱法建立聚酯纤维或切片中总磷含量与磷元素特征峰强度的校正工作曲线,分析聚酯样品中的总磷含量。该方法的磷元素检出限为0.002 5%,定量限为0.008 5%,测量定量限以上的聚酯纤维样品时,其准确性与化学分析结果相当,重复性和稳定性等测量结果完全符合GB/T 4889-2008数据的统计处理标准。该方法预处理时间不超过15 min,X射线荧光光谱仪对一个样品的检测时间不超过3 min,可应用于聚酯纤维生产企业对聚酯中红磷阻燃剂添加量的监控。

A rapid energy dispersive X-ray fluorescence spectrometery(ED-XRF) was used to analysis total phosphorus content of red phosphorus flame retardant in polyester fiber or chips. A simple pretreatment method of polyester fiber was used, such as melting. A calibration curve for the content and characteristic peak intensity of total phosphorus in polyester fiber or chips was established by energy dispersive X-ray fluorescence spectrometery, and total phosphorus content in polyester fiber samples was analyzed. The limit of detection(LOD) and limit of quantity(LOQ) of the method were 0.0025% and 0.0085% respectively. When measuring the sample containing total phosphorus above the LOQ, the accuracy of the test results was comparable to the results of the chemical analysis, and the repeatability and stability of the test results were in full compliance with the standard statistical treatment of date of GB/T 4889-2008. The pretreatment time of this method was no more than 15 min, and the measuring time of one sample was no more than 3 min by X-ray fluorescence spectrometer. The method could be applied to the monitoring of the addition amount of phosphorus flame retardant in polyester fiber manufacturers.