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微波消解辅助小体积过滤-流动注射电感耦合等离子体质谱法同时测定海水中悬浮颗粒态痕量金属(钴、镍、铜、锌、镉和铅)

Simultaneous determination of suspended particulate trace metals (Co, Ni, Cu, Zn, Cd and Pb) in seawater with small volume filtration assisted by microwave digestion and flow injection inductively coupled plasma mass spectrometer.

作者信息

Nakatsuka Seiji, Okamura Kei, Norisuye Kazuhiro, Sohrin Yoshiki

机构信息

Institute for Chemical Research, Kyoto University, Uji, Kyoto 611-0011, Japan.

出版信息

Anal Chim Acta. 2007 Jun 26;594(1):52-60. doi: 10.1016/j.aca.2007.04.057. Epub 2007 May 3.

Abstract

A new technique for the determination of suspended particulate trace metals (P-metals >0.2 microm), such as Co, Ni, Cu, Zn, Cd and Pb, in open ocean seawater has been developed by using microwave digestion coupled with flow injection inductively coupled plasma mass spectrometry (FI-ICP-MS). Suspended particulate matter (SPM) was collected from 500 mL of seawater on a Nuclepore filter (0.2 microm) using a closed filtration system. Both the SPM and filter were completely dissolved by microwave digestion. Reagents for the digestion were evaporated using a clean evaporation system, and the metals were redissolved in 0.8 M HNO3. The solution was diluted with buffer solution to give pH 5.0 and the metals were determined by FI-ICP-MS using a chelating adsorbent of 8-hydroxyquinoline immobilized on fluorinated metal alkoxide glass (MAF-8HQ). The procedure blanks with a filter were found to be 0.048+/-0.008, 10.3+/-0.3, 0.27+/-0.05, 3.3+/-1.8, 0.02+/-0.03 and 0.85+/-0.09 ng L(-1) for Co, Ni, Cu, Zn, Cd and Pb, respectively (n=14). Detection limits defined as 3 times the standard deviation of the blanks were 0.023, 0.90, 0.14, 5.3, 0.078 and 0.28 ng L(-1) for Co, Ni, Cu, Zn, Cd and Pb, respectively. Accuracy was evaluated using certified reference materials of chlorella (NES CRM No. 3) and marine sediment (HISS-1). The method was applied to the determination of vertical distributions for P-Co, Ni, Cu, Zn, Cd and Pb in the Western North Pacific.

摘要

一种用于测定开阔海洋海水中悬浮颗粒痕量金属(粒径大于0.2微米的颗粒态金属,即P - 金属,如钴、镍、铜、锌、镉和铅)的新技术已被开发出来,该技术采用微波消解结合流动注射电感耦合等离子体质谱法(FI - ICP - MS)。使用封闭过滤系统,通过0.2微米的核孔滤膜从500毫升海水中收集悬浮颗粒物(SPM)。SPM和滤膜均通过微波消解完全溶解。消解试剂使用清洁蒸发系统蒸发,金属重新溶解于0.8 M硝酸中。用缓冲溶液将溶液稀释至pH 5.0,然后使用固定在氟化金属醇盐玻璃(MAF - 8HQ)上的8 - 羟基喹啉螯合吸附剂通过FI - ICP - MS测定金属含量。发现带滤膜的程序空白值对于钴、镍、铜、锌、镉和铅分别为0.048±0.008、10.3±0.3、0.27±0.05、3.3±1.8、0.02±0.03和0.85±0.09纳克/升(n = 14)。定义为空白值标准偏差3倍的检测限对于钴、镍、铜、锌、镉和铅分别为0.023、0.90、0.14、5.3、0.078和0.28纳克/升。使用小球藻(NES CRM No. 3)和海洋沉积物(HISS - 1)的有证标准物质评估了准确度。该方法应用于测定北太平洋西部P - 钴、镍、铜、锌、镉和铅 的垂直分布。

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