气泡隔断连续流动分析法测定水中痕量挥发酚

Determination of trace volatile phenols in water by segmented continuous flow analysis

目的建立一种快速准确测定水中痕量挥发酚的连续流动分析方法。方法利用水中酚在pH=10.2缓冲介质中,经铁氰化钾氧化后,与4-氨基安替吡啉缩合得到红色化合物这一原理,使用Alliance-Futura连续流动分析仪,通过气泡隔断模式,经过在线蒸馏及510 nm在线比色完成分析。结果在0~50.0μg/L范围内,挥发酚的浓度(y)与体系吸光度(x)成线性关系,线性回归方程为y=2 659.761x-0.374,相关系数r=0.999 9,检出限为0.23μg/L。对不同水样进行高、中、低3种浓度加标测定,回收率为97.1%~104.2%。对水中挥发酚标准样品(GSB 07-3180-2014,批号200344)进行测定,测定结果与标注值一致。结论气泡隔断连续流动分析法测定水中痕量挥发酚便捷准确,适合大批量水样中痕量挥发酚的检测。

Objective To establish a method for the rapid determination of trace volatile phenols in water by segmented continuous flow analysis. Methods In the buffer medium of pH =10.2, volatile phenols can condense with 4-aminoantipyrine to form red compounds after oxidation by potassium ferricyanide. Based on this principle, the analysis was completed by the segmented continuous flow analyzer Alliance-Futura under bubble isolation mode with on-line distillation and 510 nm on-line colorimetry.Results The concentration of volatile phenols(y) was linear with the absorption of the system(x) in the range of 0-50.0 μg/L. The linear regression equation was y=2 659.761 x-0.374, with a correlation coefficient of 0.999 9. The detection limit was 0.23 μg/L.This method was used to detect the standard sample of volatile phenols in water(GSB 07-3180-2014, batch No. 200344), and the results were in agreement with the reference values. Conclusion The developed method of segmented continuous flow analysis is convenient and accurate for the determination of trace volatile phenols in water, and it is suitable for the determination of trace volatile phenols in large quantities of water samples.