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    全自动流动注射-分光光度法快速测定土壤中挥发酚的含量

    Rapid Determination of Volatile Phenol in Soil by Automatic Flow Injection-Spectrophotometry

    • 摘要: 取新鲜土壤样品10.0 g置于500 mL聚乙烯瓶中,加入5 g·L−1硫酸铜溶液10 mL和10 g·L−1氢氧化钠溶液190 mL,水平振荡10 min,静置5 min,取上清液经 0.45 μm滤膜过滤,通过流动注射分析仪于(165±2)℃在线蒸馏,被蒸馏出的挥发酚在铁氰化钾缓冲溶液(pH 10.3)中与0.65 g·L−14-氨基安替比林溶液反应,生成橙红色的吲哚酚安替比林染料,在510 nm处比色测定。结果表明,挥发酚的质量浓度在2.0 mg·L−1以内与对应的峰面积呈线性关系,检出限为0.07 mg·kg−1。对土壤挥发酚标准物质平行分析6次,测定值与认定值基本一致,测定值的相对误差为−3.9%~2.7%,相对标准偏差为1.4%~3.2%。方法用于分析6个实际土壤样品,测定结果与标准方法HJ 998—2018的基本一致。

       

      Abstract: The fresh soil sample (10.0 g) was taken and placed in a 500 mL-polyethylene bottle, and 10 mL of 5 g·L−1 copper sulfate solution and 190 mL of 10 g·L−1 sodium hydroxide solution were added. The mixture was shaken horizontally for 10 min and settled for 5 min. The supernatant was taken and passed through 0.45 μm filter membrane. Online distillation was performed using a flow injection analyzer at (165±2) ℃. The distilled volatile phenol was reacted with 0.65 g·L−1 4-aminoantipyrine solution in a potassium ferricyanide buffer solution (pH 10.3), to form an orange-red indophenol antipyrine dye. Colorimetric determination was performed at 510 nm. As shown by the results, linear relationship between the corresponding peak area and mass concentration of volatile phenol was kept within 2.0 mg·L−1, with detection limit of 0.07 mg·kg−1. Parallel analysis of soil volatile phenol certified reference materials was conducted 6 times, and the determined values were basically consistent with the certified values, with the relative error of the determined values in the range of −3.9%−2.7%, and RSDs in the range of 1.4%−3.2%. This method was applied to analysis of 6 actual soil samples, and the determination results were basically consistent with those by the standard method HJ 998—2018.

       

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