在海洋的地质的样品决定 52 专业,未成年者和踪迹元素的内容的一个改进分析方法用有一个高压的关上的消化方法( HPCD )的一个 HF-HCl-HNO3 酸系统,被诱导地联合的血浆学习光排放 spectrometry ( ICP-OES )和诱导地联合的血浆团 spectrometry ( ICPMS )。仪器的操作参数被优化,并且最佳的分析参数是坚定的。分析结果上的光光谱和集体光谱干扰,消化方法和酸系统的影响被调查。最佳光谱线和同位素被选择,并且金老的内部标准元素被选择补偿漂流的矩阵效果和分析信号。与电的加热板消化和微波消化的方法相比,一个高压的关上的消化方法与更少的酸的、完全的消化被优化,为消化过程的更少的损坏。海洋的地质的样品被一个 HF-HCl-HNO3 系统完全溶解,为分析结果的相对错误(RE ) 都是不到 6.0% 。方法察觉限制由 ICPMS 是由 ICP-OES,和 6-80 ng/g 的 2-40 g/g。方法被用来决定海洋的沉积参考材料( GBW07309 , GBW07311 , GBW07313 ),岩石参考材料( GBW07103 , GBW07104 , GBW07105 ),并且充满钴的外壳参考材料( GBW07337 , GBW07338 , GBW07339 ),获得的分析结果与证明价值一致,并且两相对标准差( RSD )和相对错误( RE )是不到6.0%。分析方法满足要求因为决定 52 个元素体积水兵满足地质的样品。
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.