An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method(HPCD), is studied by an inductively coupled plasma optical emission spectrometry(ICP-OES) and an inductively coupled plasma mass spectrometry(ICP-MS). The operating parameters of the instruments are optimized, and the optimal analytical parameters are determined. The influences of optical spectrum and mass spectrum interferences, digestion methods and acid systems on the analytical results are investigated. The optimal spectral lines and isotopes are chosen, and internal standard element of rhodium is selected to compensate for matrix effects and analytical signals drifting. Compared with the methods of an electric heating plate digestion and a microwave digestion, a high-pressure closed digestion method is optimized with less acid, complete digestion,less damage for digestion process. The marine geological samples are dissolved completely by a HF-HCl-HNO_3 system, the relative error(RE) for the analytical results are all less than 6.0%. The method detection limits are 2–40μg/g by the ICP-OES, and 6–80 ng/g by ICP-MS. The methods are used to determine the marine sediment reference materials(GBW07309, GBW07311, GBW07313), rock reference materials(GBW07103, GBW07104,GBW07105), and cobalt-rich crust reference materials(GBW07337, GBW07338, GBW07339), the obtained analytical results are in agreement with the certified values, and both of the relative standard deviation(RSD) and the relative error(RE) are less than 6.0%. The analytical method meets the requirements for determining 52 elements contents of bulk marine geological samples. 相似文献
针对强电磁干扰极易掩盖微弱的大地电磁有用信号,本文结合奇异值分解在去噪方面的优越性,提出基于自适应多分辨率奇异值分解(Adaptive Multi-Resolution Singular Value Decomposition,AMRSVD)的大地电磁数据处理方法.首先对大地电磁数据构建Hankel矩阵,利用MRSVD得到不同分辨率的近似信号和细节信号;然后选用近似信号和细节信号的标准差差值,对大地电磁数据进行信噪辨识;接着结合MRSVD和相邻细节信号的标准差差值,提出先验信息未知情况下的AMRSVD法;最后对辨识出的强干扰运用AMRSVD去除噪声,重构有用信号.实验结果表明,该方法的处理效率高,能有效分离出相关性较强的噪声,时间序列和视电阻率-相位曲线均得到有效改善.