首页|碱溶液提取-流动注射分析仪测定底泥中挥发酚

碱溶液提取-流动注射分析仪测定底泥中挥发酚

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准确高效地测定底泥中挥发酚含量,对保护生态环境具有重要的指导意义.控制液固比为15∶1,用10 g/L氢氧化钠溶液以180 r/min振荡15 min对样品中的挥发酚进行浸提,同时加入3.0 g硫酸铜去除样品中硫化物的干扰,实现了流动注射分析法对底泥中挥发酚的测定.结果表明,挥发酚质量浓度在0.02~1.0 mg/L范围内与其对应的峰面积呈线性关系,线性相关系数为0.999 9.方法的检出限为0.08 mg/kg,测定下限为0.32 mg/kg.应用实验方法对3个不同挥发酚含量的底泥样品进行测定,结果的相对标准偏差(RSD,n=6)为0.83%~1.4%.选取两种不同类型的底泥样品,分别进行3个含量水平的加标回收试验,加标回收率在93%~104%之间.分别采用实验方法和标准方法HJ 998-2018中4-氨基安替比林分光光度法对6个底泥样品中挥发酚进行测定,两种方法的分析结果基本一致.
Determination of volatile phenol in sediment by flow injection analyzer with alkali solution extraction
It is of great significance for ecological environment protection to determine accurately and effi-ciently volatile phenol content in sediment.The liquid-solid ratio was controlled at 15∶1.Volatile phenol in the sample was extracted with 10 g/L sodium hydroxide solution after oscillation at 180 r/min for 15 min.Meanwhile,3.0 g of copper sulfate was added to remove the interference of sulfides in the sample.Thus,the determination of volatile phenol in sediment was realized by flow injection analyzer.The results showed that the mass concentration of volatile phenol in range of 0.02-1.0 mg/L exhibited linear relation-ship to its corresponding peak area with correlation coefficient of 0.999 9.The limit of detection and lower limit of determination for this method were 0.08 mg/kg and 0.32 mg/kg,respectively.Three sediment samples with different concentrations of volatile phenol content in sediment were determined according to the proposed method,and the relative standard deviations(RSD,n=6)of determination results were be-tween 0.83%and 1.4%.Two types of sediment sample were selected for recovery tests with three content levels,respectively.The recoveries were between 93%and 104%.The contents of volatile phenol in six sediment samples were determined according to the proposed method as well as 4-ampyrone spectropho-tometry in standard method of HJ 998-2018.The results of the two above methods were basically consist-ent.

flow injection analyzervolatile phenolsedimentalkaline solution extraction

李小辉、胡新颖、高志军、孙慧莹、于亚辉、刘春霞

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河南省岩石矿物测试中心,自然资源部贵金属分析与勘查技术重点实验室,河南郑州 450012

苏州市姑苏区教育科学研究中心,江苏苏州 215000

流动注射分析仪 挥发酚 底泥 碱溶液提取

2024

冶金分析
中国钢研科技集团有限公司(钢铁研究总院) 中国金属学会

冶金分析

CSTPCD北大核心
影响因子:1.124
ISSN:1000-7571
年,卷(期):2024.44(12)