高压密闭消解-电感耦合等离子体质谱法测定海洋沉积物中稀土元素

高晶晶; 刘季花; 张辉; 白亚之; 崔菁菁; 何连花

高压密闭消解-电感耦合等离子体质谱法测定海洋沉积物中稀土元素

1.
国家海洋局第一海洋研究所, 山东青岛 266061
2.
海洋沉积与环境地质国家海洋局重点实验室, 山东青岛 266061
3.
国家海洋局第一海洋研究所, 山东青岛 266061
4.
海洋沉积与环境地质国家海洋局重点实验室, 山东青岛 266061
5.
国家海洋局第一海洋研究所, 山东青岛 266061
6.
海洋沉积与环境地质国家海洋局重点实验室, 山东青岛 266061
7.
国家海洋局第一海洋研究所, 山东青岛 266061
8.
海洋沉积与环境地质国家海洋局重点实验室, 山东青岛 266061
9.
国家海洋局第一海洋研究所, 山东青岛 266061
10.
海洋沉积与环境地质国家海洋局重点实验室, 山东青岛 266061
11.
国家海洋局第一海洋研究所, 山东青岛 266061
12.
海洋沉积与环境地质国家海洋局重点实验室, 山东青岛 266061

基金项目:

国家自然科学基金项目(40976038)

国家海洋局第一海洋研究所基本科研业务费项目(GY02-2009G22)

海洋公益性行业科研专项经费项目(201105003)

国家海洋局青年海洋科学基金项目(2012325)

计量
- 文章访问数: 7023
- HTML全文浏览量: 0
- PDF下载量: 1339
出版历程
- 收稿日期: 2011-07-27
- 修回日期: 2011-12-15

Determination of Rare Earth Elements in the Marine Sediments by Inductively Coupled Plasma-Mass Spectrometry with High-pressure Closed Digestion

1.
First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China
2.
Key Laboratory of Marine Sedimentology and Environmental Geology, State Oceanic Administration, Qingdao 266061, China
3.
First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China
4.
Key Laboratory of Marine Sedimentology and Environmental Geology, State Oceanic Administration, Qingdao 266061, China
5.
First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China
6.
Key Laboratory of Marine Sedimentology and Environmental Geology, State Oceanic Administration, Qingdao 266061, China
7.
First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China
8.
Key Laboratory of Marine Sedimentology and Environmental Geology, State Oceanic Administration, Qingdao 266061, China
9.
First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China
10.
Key Laboratory of Marine Sedimentology and Environmental Geology, State Oceanic Administration, Qingdao 266061, China
11.
First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China
12.
Key Laboratory of Marine Sedimentology and Environmental Geology, State Oceanic Administration, Qingdao 266061, China

摘要

摘要: 样品用HNO₃-HF高压密闭消解,电感耦合等离子体质谱测定海洋沉积物中15种稀土元素。研究了消解方法、酸体系和质谱干扰对稀土元素测定的影响。结果表明,相比于电热板消解和微波消解,高压密闭消解具有酸用量少、消解完全、消解过程损失少等优点;HNO₃-HF体系能有效地分解海洋沉积物样品;利用干扰离子校正方程,能有效地校正Ba和轻稀土元素所形成的多原子离子干扰。15种稀土元素的方法检出限为3~15 ng/g。使用水系沉积物标准物质GBW 07309和GBW 07311、海底沉积物标准物质GBW 07313进行验证,测定值与标准值基本吻合,相对标准偏差和相对误差均低于5%。方法用于长江口沉积物样品的测定,精密度(RSD,n=6)小于5%,加标回收率为95.8%~104%。该方法检出限低,精密度和准确度高,适用于大批海洋沉积物样品的分析。
- 海洋沉积物 /
- 稀土元素 /
- 高压密闭消解 /
- 电感耦合等离子体质谱法
Abstract: Using a HF-HNO₃ system with high-pressure closed digestion, a method to determine concentrations of fifteen rare earth elements (REEs) in marine sediments was studied by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). Experimental conditions such as mass spectrum interferences, digestion methods and acid systems have been investigated. Compared to electric heating plate digestion and microwave digestion, high-pressure closed digestion has the advantages of using less acid, achieving complete digestion and causing less damage to the digestion process. The correction equation effectively calibrated polyatomic ions interferences formed by Ba and light rare earth elements. The marine sediment samples were dissolved completely by HF-HNO₃ system, and the relative error (RE) was less than 5%. The method detection limits were 3-15 ng/g. The proposed method was validated by the marine sediment reference materials GBW 07309, GBW 07311 and GBW 07313. The results were consistent with certified values, and the relative standard deviation (RSD) and relative error were both less than 5%. The determination precision (RSD, n=6) of the Yangtze River estuary sediment samples was less than 5%, and the recoveries were 95.8%-104%. This method has a low detection limit with high precision and accuracy, all of which meet the requirements to analyze a large number of marine sediment samples.
- marine /
- sediment /
- rare /
- earth

HTML全文

参考文献(22)

王中刚,于学元,赵振华.稀土元素地球化学[M].北京:科学出版社,1989.

赵振华.微量元素地球化学原理[M].北京:科学出版社,1997.

蓝先洪,申顺喜.南黄海中部沉积岩心的稀土元素地球化学特征[J].海洋通报,2002,21(5): 46-53.

曹煊,李景喜,俞晶晶,于振花,陈维余,杨黄浩.电感耦合等离子体质谱法测定井间示踪剂中稀土元素[J].岩矿测试,2009,28(2): 91-96.

杨社锋,方维萱,胡瑞忠,王思德,魏宁.老挝Boloven高原玄武岩风化壳中稀土元素富集与主量元素关系[J].中国稀土学报,2007,25(4): 461-469.

吴波英,黄少文.ICP-AES在稀土元素分析中的抗干扰技术的应用及进展[J].稀土,2005,26(5): 17-22.

田晓娅,张宏志.ICP-AES法同时测定岩石、矿物、土壤等样品中十五种稀土元素的方法研究[J].光谱实验室,1996,13(5): 57-63.

富玉,刘金霞,王彦芬,黄志荣.无滤共沉淀富集-等离子体原子发射光谱法测定痕量稀土元素[J].分析试验室,2007,26(3): 91-94.

胡圣虹,林守麟,刘勇胜,高山.等离子体质谱法测定地质样品中痕量稀土元素的基体效应及多原子离子干扰的校正研究[J].高等学校化学学报,2000,21(3): 368-372.

黄慧萍,李艳玲,陶德刚,熊采华,方金东.电感耦合等离子体质谱法测定铬铁矿单矿物中痕量稀土元素[J].冶金分析,2005,25(6): 42-45.

贾维斯,格雷,霍克.电感耦合等离子体质谱手册[M].尹明,李冰,译.北京: 原子能出版社,1997.

林立,陈光,陈玉红.电感耦合等离子体质谱法测定茶叶中的16种稀土元素[J].环境化学,2007,26(4): 555-558.

李冰,尹明.电感耦合等离子体质谱法测定生物样品中超痕量稀土时氧化物干扰的研究[J].岩矿测试,2000,19(2): 101-105.

帅琴,杨薇,胡圣虹,卢爱明,郑楚光.微波消解-电感耦合等离子体质谱测定大气颗粒物中痕量稀土元素[J].分析科学学报,2005,21(4): 375-377.

王君玉,吴葆存,李志伟,韩敏,钟莅湘.敞口酸溶-电感耦合等离子体质谱法同时测定地质样品中45个元素[J].岩矿测试,2011,30(4): 440-445.

周国兴,刘玺祥,崔德送.碱熔ICP-MS法测定岩石中稀土等28种金属元素[J].质谱学报,2010,31(2): 120-124.

陈永欣,黎香荣,韦新红,吕泽娥,谢毓群,蔡维专.微波消解-电感耦合等离子体质谱法测定土壤和沉积物中痕量稀土元素[J].岩矿测试,2011,30(5): 560-565.

吴淑芳,姜玉梅,刘燕,刘永林.电感耦合等离子体质谱法测定土壤中可溶态稀土元素[J].南昌大学学报: 理学版,2007,31(4): 377-379.

王小如.电感耦合等离子体质谱应用实例[M].北京: 化学工业出版社,2005.

刘虎生,邵宏翔.电感耦合等离子体质谱技术与应用[M].北京: 化学工业出版社,2005.

Song Y H, Choi M S. REE geochemistry of fine-grained sediments from major rivers around the Yellow Sea[J]. Chemical Geology, 2009, 266: 328-342.

Singh P. Major, trace and REE geochemistry of the Ganga River sediments: Influence of provenance and sedimentary processes [J]. Chemical Geology, 2009, 266: 242-255.

施引文献

资源附件(0)

计量

文章访问数: 7023
HTML全文浏览量: 0
PDF下载量: 1339
被引次数: 0

高压密闭消解-电感耦合等离子体质谱法测定海洋沉积物中稀土元素

计量

出版历程

Determination of Rare Earth Elements in the Marine Sediments by Inductively Coupled Plasma-Mass Spectrometry with High-pressure Closed Digestion

计量

出版历程

目录