氟化氢铵和过氧化氢消解多金属结核和富钴结壳的方法研究

发布时间：2018-06-24 07:27

本文选题：多金属结核 + 富钴结壳　；参考：《中国地质大学(北京)》2016年硕士论文

【摘要】：海洋中的多金属结核和富钻结壳富含大量有价值的元素,其中锰、钴、镍、铜等金属元素的储量,相当于陆地储量的几十至几千倍,因此成为目前的一个研究热点。目前所使用的大洋多金属结核化学分析方法较为复杂,需进行大量实验才可获得结核中各元素的含量。本论文针对结核和结壳的消解方法进行研究,使用氟化氢铵或过氧化氢作为主要消解试剂,电烘箱、微波消解仪、电热板等仪器作为加热手段,所得样品采用ICP-MS和ICP-OES联机检测,考察其消解效果,最终为找到一种高效的多元素同时分析方法提供数据支撑。主要研究成果如下：1、建立了氟化氢铵消解-盐酸提取-电感耦合等离子体质谱、光谱联机检测多金属结核和富钴结壳的方法。此方法整个流程时间大大缩短,Mn、Fe、Co、 Ni、HREE等元素的回收率能够达到90%以上；Ti、Cr、Mn、Ni、Cu、Zn、Mo的测定下限为2.15-47.4μg·gl,其它元素为0.003-0.881μg·g-1,精密度(RSD, n=3)5%。2、使用硝酸-盐酸-过氧化氢消解结核和结壳,不经赶酸、复溶,直接定容上机检测,结果显示部分元素(Mn、Fe、Ni、Cd、HREE、Bi、U)的回收率达到90%。此方法Ti、Mn、Ni、Cu、Zn、Sr、Sn、Sb、Ba的测定下限为1.067～29.53μg·g-1,其它元素为0.010-0.621μg·g-1,精密度(RSD, n=3)除Cr、Ga、Nb、Sb、W高于10%外其它元素均低于10%。3、对ICP-MS检测结果中出现的内标下降结果随之上升、ICP-OES检测结果中空白值为负的问题进行了研究。对样品溶液进行稀释、减少单次测量样品数量、进行校准计算、选用更加合理的标准溶液等手段能够改善这些问题。4、微波消解速度较快,但结果不稳定,尚不能作为准确检测多金属结核和富钴结壳的加热手段。
[Abstract]:Polymetallic nodules and rich drilling crusts in the ocean are rich in a large number of valuable elements, of which manganese, cobalt, nickel, copper and other metal elements, which are tens to thousands of times the reserves on land, have become a research hotspot at present. The chemical analysis methods of oceanic polymetallic nodules used at present are more complicated, and a large number of experiments are needed to obtain the contents of various elements in nodules. In this paper, the digestion methods of nodules and crusts were studied. Ammonium bicarbonate or hydrogen peroxide was used as the main digestion reagent, electric oven, microwave digestion instrument and electric heating plate were used as heating means. The samples were detected by ICP-MS and ICP-OES on-line. Finally, it provides data support for finding an efficient multielement simultaneous analysis method. The main research results are as follows: 1. A new method for the determination of polymetallic nodules and cobalt-rich crusts by inductively coupled plasma mass spectrometry (ICP-MS) with ammonium hydrofluoride digestion, hydrochloric acid extraction, and cobalt-rich crusts has been established. The whole process time of this method is greatly shortened. The recovery rate of NiHREE and other elements can reach more than 90%. The lower limit of determination of TiCrCr-MnMn-NiCuOZZN Mo is 2.15-47.4 渭 g gl.Other elements are 0.003-0.881 渭 g g-1, precision (RSD-N3) 5..2, using nitric acid hydrochloric acid-hydrogen peroxide to dissolve nodule and crust, without acid catching, redissolving, and so on, the recovery rate of RSD-HREE and so on can reach 90%, and the determination limit is 2.15-47.4 渭 g / g 路g ~ (-1), and the precision (RSD, n _ 3) _ 5 路2. The results showed that the recovery rate of some elements (MnOFeFeHREEU) was 90%. In this method, the lower limit of determination is 1.067 ~ (29.53) 渭 g g ~ (-1), other elements are 0.010 ~ (-0.621) 渭 g / g ~ (-1), the precision (RSD, n ~ (3) is lower than 10.3 except for CrGaGaNbSbN _ W > 10%, and the decrease of internal standard in ICP-MS is increased. The blank value of ICP-OES is negative. The problem is studied. Diluting the sample solution, reducing the number of samples measured at a single time, calibrating calculation, selecting more reasonable standard solution can improve these problems. The microwave digestion speed is faster, but the results are unstable. It can not be used as a heating method for accurate detection of polymetallic nodules and cobalt-rich crusts.
【学位授予单位】：中国地质大学(北京)
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：P744

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