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恒温氧化还原反应-氢化物原子荧光法测定水中总硒含量

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目的 建立一种操作简单、准确的氢化物原子荧光法测定水中总硒含量的方法,为实现样品消解的标准化操作流程提供参考.方法 在恒温氧化还原反应-氢化物原子荧光法过程中,取10.00 mL水样于锥形管中,采用聚丙烯锥形管,在水样中加入硝酸,110 ℃恒温消解水中硒15 min,加入还原剂盐酸和硫脲溶液,110 ℃恒温消解35 min,冷却,加水至刻度,完成样品消解.测定检出限、精密度、加标回收率,计算相对标准偏差(RSD),进行标准物质测定.确定最优实验条件后,用氢化物原子荧光法测定总硒含量.结果 在优化条件下,四价硒线性范围为1.00~10.00μg/L,r=0.9 997;四价硒加标回收率为97.98%~101.00%,相对标准偏差(RSD)为0.99%~1.28%;六价硒加标回收率为96.32%~98.82%,RSD为0.84%~1.44%;标准物质测定值在可信范围内;最低检出限0.20 μg/L.结论 本实验中氢化物原子荧光法测定水中四价硒、六价硒的方法优化后,测定结果的线性、检出限、精密度、准确度均满足方法学要求,恒温消解法能准确测定水中总硒含量,操作简单.
Determination of total selenium in water by constant temperature REDOX reaction-hydride atomic fluorescence method
Objective To develop a simple and accurate method to determine the total selenium in water by hydride atom-ic fluorescence spectrometry so as to provide a reference for achieving a standardized operational procedure for sample di-gestion.Methods In the process of performing constant temperature oxidation-reduction reaction hydride atomic fluo-rescence spectrometry,10.00 mL of water sample was taken into a conical tube,and a polypropylene conical tube was used.Nitric acid was added to the water sample,selenium was dissolved in water at 110 C for 15 minutes,reducing agents hydrochloric acid and thiourea solution were added,and dissolved at 110 ℃ for 35 minutes.After cooling,water was added to the mark to complete the sample digestion.Determine the detection limit,precision,spiked recovery rate,calculate the relative standard deviation(RSD),and perform standard substance determination.After determining the optimal experi-mental conditions,the total selenium content was determined using hydride atomic fluorescence spectrometry.Results Under optimized conditions,the linear range of tetravalent selenium was 1.00-10.00 μ g/L,r=0.999 7.The recovery rate of tetravalent selenium spiked ranged from 97.98%-101.00%,and the relative standard deviation(RSD)was 0.99%-1.28%.The recovery rate of hexavalent selenium spiked was 96.32%to 98.82%,with RSD ranging from 0.84%to 1.44%.The measured values of standard substances were within a reliable range.The minimum detection limit was 0.20 μg/L.Conclusion After optimizing the method for determining tetravalent selenium and hexavalent selenium in water u-sing hydride atomic fluorescence spectrometry in this experiment,the linearity,detection limit,precision,and accuracy of the measurement results all meet the methodological requirements.The constant temperature digestion method can accu-rately determine the total selenium content in water,and the operation is simple.

Total seleniumThioureaREDOX reactionHydride atomic fluorescence spectrometry

车燕妮、郭琴

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威海市疾病预防控制中心理化检验科,山东 264200

总硒 硫脲 氧化还原反应 氢化物原子荧光光谱法

2024

预防医学论坛
中华预防医学会

预防医学论坛

影响因子:0.645
ISSN:1672-9153
年,卷(期):2024.30(8)