瞿翠兰 张兵 钟仕花

摘 要：应用微波消解技术，采用电感耦合等离子体质谱仪（ICP-MS），建立了海湾沉积物中稀土元素的检测方法，对比3种不同酸消解体系和3种不同赶酸温度对14种元素回收率的影响。结果表明：在3种不同酸消解体系中，HNO3 6mL+HCl 3mL+HF 2mL+HClO4 2mL酸解体系消化后，回收率达到最佳效果且均能满足相关标准要求;经过微波消解后，在3种不同赶酸温度中，（150+200）℃组合温度下赶酸，其回收率效果最佳且均能满足相关标准要求。经ICP-MS进行定量分析，14种组分在各自浓度范围内的线性关系均大于0.995，平均回收率在74.9%～113%。相对标准偏差为2.1%～4.2%，14种稀土元素的方法检出限范围为0.02～0.04μg/kg。表明该方法具有良好的准确度和精密度，可以满足海湾沉积物中14种稀土元素的检测要求，从而为海湾沉积物中稀土元素的检测提供了新途径。

关键词：酸消解体系;赶酸温度;海湾沉积物

中图分类号 X833文献标识码 A文章编号 1007-7731（2020）15-0115-04

Abstract： A method for the determination of rare earth elements in bay sediments was established by microwave digestion technique and inductively coupled plasma mass spectrometry （ICP-MS）.The effects of three different acid digestion systems and three different acid removal temperatures on the recovery of 14 elements were compared.The experimental results show that：three different acid digestion systems were set up， among them the recovery rate of HNO3 6mL+HCl 3mL+HF 2mL+HClO4 2mL acidizing system can reach the best effect;and three different acid removal temperatures are set after microwave digestion， among them acid is driven out at the combined temperature of 150℃ and 200℃， the recovery rate is the best and can meet the requirements of the relevant standards.Quantitative analysis by ICP-MS showed that ： the linear relationship of the 14 components was more than 0.995 in the range of their respective concentrations， and the average recovery was 74.9% ～113%.The relative standard deviation is 2.1～4.2%.The detection limit of 14 rare earth elements is 0.02～0.04μg/kg.The method has good accuracy and precision and can meet the requirements of 14 rare earth elements in Gulf sediments.It provides a new way for the detection of rare earth elements in bay sediments.

Key words：Acid digestion system; Acid driving temperature; Bay sediment

海灣作为衔接海洋与陆地的核心区域，可以为海岸带地区提供双重生态价值，也是最容易受到人类活动影响和生态极其脆弱的区域[1]。深圳作为国际化程度很高的大都市，海湾生态条件对深圳城市经济的发展具有重要的支撑作用。深圳自成立经济特区以来，经过近40年的高速发展，对土地、海域、环境等高强度的过度开发利用，对深圳海域的水动力条件、生态环境等都产生了深远的影响。以深圳湾为例，海域面积减少近25km2，湿地面积减小约50%，填海后深圳湾面积减少近1/3[2]，湾内断面缩窄，过水断面减小，水动力减弱，湾内淤积严重，近河口位置初步估计深圳河口淤积量达0.2亿m3以上。……