熔融制样-X射线荧光光谱法测定锰矿石及大洋多金属结核中15种主次成分  

Determination of 15 major and minor components in manganese ore and marine polymetallic nodule by X-ray fluorescence spectrometry with fusion sample preparation

作　　者：苏建芝 罗学辉 邓华 李海东 满玉凯 胡雪冰 SU Jianzhi;LUO Xuehui;DENG Hua;LI Haidong;MAN Yukai;HU Xuebing(Hebei Oriental University,Langfang 065000,China;Langfang Natural Resources Comprehensive Survey Center of China Geological Survey,Langfang 065000,China)

机构地区：[1]河北东方学院,河北廊坊065000 [2]中国地质调查局廊坊自然资源综合调查中心,河北廊坊065000

出　　处：《冶金分析》2024年第7期62-67,共6页Metallurgical Analysis

基　　金：战略性矿产勘查岩矿测试技术支撑(廊坊中心)(DD20242943)。

摘　　要：本文基于锰矿石和大洋多金属结核这两种重要锰资源基体和物相具有高度相似性,以四硼酸锂-偏硼酸锂-氟化锂(Li_(2)B_(4)O_(7)-LiBO_(2)-LiF)为熔剂,为解决高含量铜的大洋多金属结核样品在熔融时易脆裂和出现裂痕的问题,经过试验确定稀释比为30∶1,以(m(Li_(2)B_(4)O_(7))∶m(LiBO_(2))∶m(LiF)=4.5∶1∶0.4)为熔剂,再分次加入2.0000 g NH_(4)NO_(3)为氧化剂,以饱和溴化锂饱和溶液为脱模剂,制备出完整的高质量熔融片。建立了同时测定锰矿石及大洋多金属结核(锰结核)中MnO、SiO_(2)、Al_(2)O_(3)、TFe_(2)O_(3)、TiO_(2)、CaO、K_(2)O、MgO、BaO、P_(2)O_(5)、CuO、ZnO、PbO、NiO、CoO 15种组分的定量分析方法。用此方法分析国家标准物质GBW07263、GBW07296,各组分测定结果的相对标准偏差(RSD)为0.11%~4.8%;分析不参加回归的国家一级大洋多金属结核标准物质GBW07295和锰矿石标准物质GBW07265,测试值与认定值相符。Manganese ore and marine polymetallic nodule are two important manganese resources and their phases have high similarity.In this study,the mixture of lithium tetraborate,lithium metaborate and lithium fluoride(Li_(2)B_(4)O_(7)-LiBO_(2)-LiF)was used as flux.In order to solve the problem of embrittlement and cracking of marine polymetallic nodule sample with high copper content during fusion,the dilution ratio of 30∶1 was determined by experiments.Then m(Li_(2)B_(4)O_(7))∶m(LiBO_(2))∶m(LiF)=4.5∶1∶0.4 was added as flux,2.0000 g of NH_(4)NO_(3) was added as oxidant,and the saturated solution of lithium bromide was selected as the release agent.The intact fusion pellet with good quality was prepared.The quantitative analysis method for the simultaneous determination of 15 components in manganese ore and marine polymetallic nodule(manganese nodule),including MnO,SiO_(2)、Al_(2)O_(3)、TFe_(2)O_(3)、TiO_(2)、CaO、K_(2)O、MgO、BaO、P_(2)O_(5)、CuO、ZnO、PbO、NiO and CoO,was established.The proposed method was used for the analysis of national certified reference materials(GBW07263 and GBW07296),and the relative standard deviations(RSD)of determination results were between 0.11%and 4.8%.The analysis results of national primary certified reference materials of marine polymetallic nodule GBW07295 and manganese ore GBW07265,which did not participate in the regression,were basically consistent with the certified values.

关 键 词：X射线荧光光谱法(XRF) 熔融制样 锰矿石 大洋多金属结核 主次成分 

分 类 号：O657.34[理学—分析化学]