Determination of Trace Lead and Copper in Seawater by Inductively Coupled Plasma-Mass Spectrometry with Coconut Shell Biochar Enrichment
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摘要:
海洋环境中的重金属污染备受关注，准确测定海水中的痕量重金属，对保护海洋环境和人类健康具有重要意义。海水样品的高盐和重金属痕量浓度等特点给仪器分析带来巨大挑战，直接准确测定高盐基质中的低含量重金属元素是非常困难的，须经前处理去除海水中的大量盐分，并对待测元素进行富集，从而消除基体干扰，降低检出限。为实现海水中的痕量铅和铜的绿色分离与快速检测，本文采用吸附脱附的方式，将海水中铅和铜富集在椰壳生物炭上，再用超纯水反复冲洗生物炭，除去盐分基质，经硝酸溶解脱附，脱附液用0.45μm滤膜过滤后利用电感耦合等离子体质谱法(ICP-MS)测定，建立了生物炭富集ICP-MS测定海水中铅和铜含量的方法。两种金属元素在0.10～100μg/L范围内线性关系良好，线性相关系数均大于0.9995。海水中铅和铜，方法检出限分别为0.005μg/L和0.006μg/L，测定下限分别为0.020μg/L和0.024μg/L，满足《海水、海洋沉积物和海洋生物质量评价技术规范》(HJ 1300—2023)规定的海水质量评价要求。海水样品加标回收率在96.1%～102.3%范围内，相对标准偏差小于5%。本方法操作简便、分析成本低、绿色环保，更适合于基层海洋监测应用，也可用于高矿化度基体样品的水质监测。
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关键词:
- 椰壳生物炭 /
- 富集 /
- 电感耦合等离子体质谱法 /
- 海水 /
- 重金属
Abstract:The high salt in seawater samples brings great challenges for analyzing trace heavy metals. To achieve the green separation and rapid detection of trace lead and copper in seawater, a method of coconut shell biochar enrichment was established. By using the method of adsorption and desorption, lead and copper elements in seawater were enriched on coconut shell biochar, and the coconut shell biochar powder was repeatedly washed with pure water to remove the salt matrix in seawater. The desorption was dissolved with 7.5% HNO3, and the desorption solution was filtered with 0.45μm filter membranes and analyzed by ICP-MS. Two metal elements showed good linear relationships within the range of 0.10−100μg/L, and the linear correlation coefficients were greater than 0.9995. The method had a detection limit of 0.005μg/L for Pb and 0.006μg/L for Cu, meeting the evaluation requirements of seawater quality assessment stipulated in Technical Specification for Assessment of Sea Water, Marine Sediment and Marine Biological Quality (HJ1300—2023). The spiked recovery rates for seawater samples were between 96.1% and 102.3%, with the relative standard deviation less than 5%. This method had the advantages of simple operation, low costs, environmental protection, and high reliability and sensitivity.
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Key words:
- coconut shell biochar /
- enrichment /
- ICP-MS /
- seawater /
- heavy metals
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表 1 海水中重金属元素质控样品的测定结果
Table 1. Analytical results of quality control samples for heavy metal elements in seawater
重金属
元素BWQ7001-2016(北方伟业) TMQC0129(坛墨质检) 标准值
(μg/L)实际测定值
(μg/L)标准值
(μg/L)实际测定值
(μg/L)Pb 10.0±0.6 9.92 10.2±0.6 10.23 Cu 5.0±0.4 5.05 5.6±0.5 5.57 
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