Determination of 15 major and minor components in manganese ore and marine polymetallic nodule by X-ray fluorescence spectrometry with fusion sample preparation
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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(Li2B4O7-LiBO2-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(w(Li2B4O7)∶m(LiBO2):w(LiF)=4.5:1:0.4)为熔剂,再分次加入2.000 0 g NH4NO3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、SiO2、Al2 O3、TFe2 O3、TiO2、CaO、K2 O、MgO、BaO、P2 O5、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 lithi-um fluoride(Li2B4O7-LiBO2-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(Li2B4O7)∶m(LiBO2)∶m(LiF)=4.5∶1∶0.4 was added as flux,2.000 0 g of NH4NO3 was added as oxidant,and the saturated solution of lithium bromide was se-lected as the release agent.The intact fusion pellet with good quality was prepared.The quantitative analy-sis method for the simultaneous determination of 15 components in manganese ore and marine polymetallic nodule(manganese nodule),including MnO,SiO2,Al2O3,TFe2O3,TiO2,CaO,K2O,MgO,BaO,P2O5,CuO,ZnO,PbO,NiO and CoO,was established.The proposed method was used for the analysis of national certi-fied reference materials(GBW07263 and GBW07296),and the relative standard deviations(RSD)of deter-mination results were between 0.11％and 4.8％.The analysis results of national primary certified refer-ence materials of marine polymetallic nodule GBW07295 and manganese ore GBW07265,which did not par-ticipate in the regression,were basically consistent with the certified values.
X-ray fluorescence spectrometry(XRF)fusion sample preparationmanganese oremarine poly-metallic nodulemajor and minor component
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