Determination of zirconium,niobium,hafnium,tantalum and rare earth elements in geological sample by inductively coupled plasma mass spectrometry with sodium peroxide alkali fusion
The determination of Zr,Nb,Hf,Ta,and rare earth elements in geological samples has important significance for exploration and utilization of rare earth mineral resources as well as the geological environ-ment researches such as geochemistry and petrogenesis.The sample was melted with Na2O2 at 750 ℃ for 8 min followed by leaching with boiling water.After filtration,the hydroxide precipitates were dissolved with HCl-H2O2 mixed solution in stages.The interferences of oxides or hydroxides of light rare earth ele-ments with heavy rare earth elements were overcome by selecting He collision cell mode and interference correction equation.Rh was used to correct Zr,Nb,Sc,Y,La,Ce,Pr,Nd and Sm,and Re was used to correct Hf,Ta,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb and Lu.Consequently,a method for simultaneous de-termination of Zr,Nb,Hf,Ta and rare earth elements in geological sample was established by inductively coupled plasma mass spectrometry(ICP-MS).Under the optimized experimental conditions,the linear cor-relation coefficients of calibration curves of 20 elements were all not less than 0.999 2.The limits of detec-tion were in range of 0.03-2.69 μg/g,and the limits of quantitation were in range of 0.09-8.07 μg/g.The contents of Zr,Nb,Hf,Ta and rare earth elements in certified reference materials of stream sediment and rock were determined according to the proposed method,and the relative errors(RE)between the results and certified values were all not more than 6.7％,which could meet the allowable limit requirements of relative error in industry standard of DZ/T 0130-2006.The relative standard deviations(RSD,n=12)were all not more than 4.8％.The proposed method was applied for determination of Zr,Nb,Hf,Ta and rare earth elements in soil,stream sediment and rock samples,and the RSDs(n=6)of determination re-sults were between 0.5％and 4.8％.
sodium peroxidealkali fusioninductively coupled plasma mass spectrometry(ICP-MS)geo-logical samplezirconiumniobiumhafniumtantalumrare earth element
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