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水中挥发酚的在线蒸馏-固相萃取分离富集及测定
On-line distillation and solid phase extraction preconcentration of volatile phenolic compounds in water samples with detection by spectrophotometry
【摘要】 在顺序注射系统中实现了挥发酚的快速自动在线蒸馏,并用AmberliteXAD-7树脂微填充柱对其与4-氨基安替比林的衍生物在线固相萃取,被富集的衍生物可用少量乙醇有效地洗脱回收,以分光光度法检测.方法可用于较高浓度挥发酚(mg/L)样品的测定,也可根据需要适当增大进样体积,经富集后实现更低浓度水平(μg/L)挥发酚的测定.当富集过程中进样体积为4mL时,方法测定挥发酚的线性范围为0.004~0.3mg/L,检出限为0.002mg/L,相对标准偏差为1.4%(0.1mg/L,n=9).对多种实际水样中的挥发酚进行了测定,加标回收实验的回收率在96%~102%之间.
【Abstract】 A novel sequential injection on-line distillation procedure for volatile phenolic compounds is developed. The derivative between phenol and 4-aminoantipyrine (4-APP) is adsorbed onto an Amberlite XAD-7 resin packed mini-column. The phenol-4-APP derivative retained on the mini-column is effectively recovered by using a small amount of ethanol followed by spectromphotometric detection. The present procedure is suitable for the direct determination of volatile phenolic compounds at mg/L levels. It can also be used for the quantification of much lower concentration of volatile phenolic compounds at μg/L level after preconcentration with a larger sample volume. With the sample loading volume of 4 mL, a linear range of 0.004–0.3 mg/L is obtained along with a detection limit is 0.002 mg/L. A relative standard deviation of 1.4% (n = 9) is achieved at 0.1 mg/L. The procedure is applied to the determination of low level of volatile phenolic compounds in water samples and spiking recoveries within 96%–102% are achieved.
【Key words】 volatile phenolic compounds; sequectial injection; on-line distillation; separation and preconcentration; spectrophotemetry;
- 【文献出处】 中国科学:化学 ,Scientia Sinica(Chimica) , 编辑部邮箱 ,2011年05期
- 【分类号】X832
- 【被引频次】3
- 【下载频次】351