两种方法测定染整废水中总锑的比较

Comparison of two methods for determination of total antimony in dyeing and finishing wastewater

建立和比较了原子荧光(AFS)和电感耦合等离子体质谱(ICP-MS)测定染整废水中总锑的方法。对原子荧光法的还原剂用量及还原反应时间进行实验条件优化。结果显示:优化检测条件为还原剂用量15%、反应时间60 min;原子荧光法和电感耦合等离子体质谱法的标准曲线分别为y=318.214x-12.169和y=998.633x+6873.813,线性相关系数分别为0.9998、0.9997,RSD值分别为2.18%~3.22%和0.88%~1.94%,加标回收率分别为96%~104%和95%~102%,有证标准样品测定值均在不确定度范围内。使用两种方法分别测定实际染整排放口废水,检测结果总锑未超过标准限值。两种方法均有较好的线性、灵敏度、精密度及正确度,可应用于染整废水总锑检测,实际检测中应依据应用场景选择检测方法。

Atomic fluorescence spectrometry(AFS)and inductively coupled plasma mass spectrometry(ICP-MS)were established and compared for the determination of total antimony in dyeing and finishing wastewater.The amount of reductant and the reaction time were optimized.The results showed that the opti⁃mal detection conditions were 15%of reductant dosage and 60 min of reaction time.The standard curves of atomic fluorescence method and inductively coupled plasma mass spectrometry were y=318.214x-12.169 and y=998.633x+6873.813 respectively,the linear correlation coefficients were 0.9998 and 0.9997 respectively,the RSD values were 2.18%~3.22%and 0.88%~1.94%respectively,and the recovery rates were 96%~104%and 95%~102%respectively.The measured values of certified standard samples were within the uncertainty range.Two methods were used to determine the total antimony in the wastewater from the actual dyeing and finishing outlet,and the test results did not exceed the standard limits.Both methods had good linearity,sensi⁃tivity,precision and accuracy,and could be applied to the detection of total antimony in dyeing and finishing wastewater.In actual detection,the detection method should be selected according to the application scenario.