X射线荧光光谱法测定间苯二胺中的总氯

Determination of total chlorine in m-phenylenediamine by X-ray fluorescence spectrometry

为有效监控间苯二胺生产过程中的杂质氯,建立一种借助X射线荧光光谱法快速、无损地测定间苯二胺中总氯的方法。在30~1 051 mg/kg区间内,氯强度值与其对应含量呈线性,相关系数大于0.999。准确度结果显示,在20、100、800 mg/kg 3种含量梯度下,各加标回收率均大于90%。精密度结果显示,相对标准偏差小于1.0%,重复性较好。最后经4批次实际间苯二胺样品测试,验证了该方法的实际可操作性。

In order to effectively monitor the impurity chlorine in the production of m-phenylenediamine,a rapid and nondestructive method for the determination of total chlorine in m-phenylenediamine by X-ray fluorescence spectrometry was established.Within the range of 30-1 051 mg/kg,the chlorine intensity value was linear with its corresponding content,with a correlation coefficient greater than 0.999.The accuracy results showed that under three mass fraction gradients of 20,100,and 800 mg/kg,the recovery rates of each spiked substance were all greater than 90%.The precision results showed that the relative standard deviation was less than 1.0% and the repeatability was good.Finally,the actual operability of this method was verified through testing of 4 batches of actual meta phenylenediamine samples.