ICP-MS测定高硅矿物中铌、钽及稀土
|
摘要
采用ICP-MS法测定了高硅矿物中铌、钽及稀土含量。针对花岗岩的特性,试验了硝氟酸溶解分离与氟化氢铵焙烧分离2种有效分离硅的方法,消除了硅对分析结果的影响,并对方法进行了验证,较不分离硅,该方法的准确度、精密度均有大幅提升,适用于花岗岩等高硅矿床中稀土及铌、钽的分析,值得推广。
Niobium,tantalum and rare earth elements in high-silicon rocks were determined by ICP-MS. According to the characteristcs of granite,tests for separation of silicon were conducted by dissolving the sample in nitro-fluoric acid and roasting the sample with ammonium bifuoride,respectively.The effect of silicon on the determination of Nb,Ta and rare earth was eliminated.The method is rapid and accurate. It is suitable for determination of rare earth,niobium and tantalum in high silicon rocks.
Niobium,tantalum and rare earth elements in high-silicon rocks were determined by ICP-MS. According to the characteristcs of granite,tests for separation of silicon were conducted by dissolving the sample in nitro-fluoric acid and roasting the sample with ammonium bifuoride,respectively.The effect of silicon on the determination of Nb,Ta and rare earth was eliminated.The method is rapid and accurate. It is suitable for determination of rare earth,niobium and tantalum in high silicon rocks.
引文
[1] Simandl G J.Geology and market-dependent significance of rare earth element resources[J].Mineralium Deposita,2014,49(8):889-904.
[2] 侯振宇,何扬.我国稀土资源概况及应用前景[J].内蒙古科技与经济,2017,(7):28-30.Hou Z Y,He Y.General situation and application prospect of rare earth resources in China[J].Inner Mongolia Science technology & Economy,2017,(7):28-30.
[3] GB/T 6730.23-2006.稀土总量的测定.萃取分离-偶氮氯膦mA分光光度法[S].GB/T 6730.23-2006.Determination of total rare earths with extraction separation-chlorophosphonazo mA by spectrophotometric method[S].
[4] 杨枝,李伯平,罗明标,宋金如,刘维.微色谱柱分离-光度法测定高稀土铁矿石中的微量钍[J].分析试验室,2008,27(3):52-55.Yang Z,Li B P,Luo M B,Song J R,Liu W.Separation of thorium in lanthanon-iron ore samples by microcolumn of HD-8 resin and determination by spectrophotometry[J].Chinese Journal of Analysis Laboratory,2008,27(3):52-55.
[5] GB/T 6730.24-2006,稀土总量的测定.草酸盐重量法[S] .GB/T 6730.24-2006,Determination of total rare earths by oxalate gravimetric method[S] .
[6] 杨瑞瑛,贾秀琴.中子活化法研究中祁连清水沟蛇绿岩中稀土元素的地球化学特征[J].同位素,2006,19(2):65-69.Yang R Y,Jia X Q.Geochemical characteristics of rocks from qingshuigou of middle qilian ophiolete by NAA[J].Journal of Isotopes,2006,19(2):65-69.
[7] Brunfelt A O,Roelandts I,Steinnes E.Determination of rubidium,caesium,barium and eight rare earth elements in ultramafic rocks by neutron-activation analysis[J].Analyst,1974,99:277-284.
[8] Djingova R,Ivanova J.Determination of rare earth elements in soils and sediments by inductively coupled plasma atomic emission spectrometry after cation-exchange separation[J].Talanta,2002,57:821-829.
[9] 吴石头,王亚平,孙德忠,温宏利,许春雪,王伟.电感耦合等离子体发射光谱法测定稀土矿石中15种稀土元素-四种前处理方法的比较[J].岩矿测试,2014,1:12-19.Wu S T,Wang Y P,Sun D Z,Wen H L,Xu C X,Wang W.Determination of 15 rare earth elements in rare earth ores by inductively coupled plasma-atomic emission spectrometry:A Comparison of Four Different Pretreatment Methods[J].Rock and Mineral Analysis,2014,1:12-19.
[10] Beata Z,Katarzyna P,Barbara F,Marzena P,Andrzej K,Rafal S.Determination of rare earth elements by spectroscopic techniques:A review[J].Journal of Analytical Atomic Spectrometry,2011,26 (12):2373-2390.
[11] Frederico G P,Rainerio E J,Tatiana D S.Sample preparation for determination of rare earth elements in geological samples by ICP-MS:A critical review[J].Analytical Letters,2012,45(12):1537-1556.
[12] Tinggi U,Gianduzzo T,Francis R.Determination of selenium in red blood cells by ICP-MS after microwave digestion.Journal of Radioanalytical and Nuclear Chemistry,2004,259(3):469-472
[13] 李小莉,张勤.粉末压片-X射线荧光光谱法测定土壤、水系沉积物和岩石样品中15种稀土元素[J].冶金分析,2013,33(7):35-40.Li X L,Zhang Q.Determination of fifteen rare earth elements in soil,stream sediment and rock samples byX-ray fluorescence spectrometry with pressed powderpellet[J].Metallurgical Analysis,2013,33(7):35-40.
[14] 周伟,曾梦,王健,张磊,李迎春.熔融制样-X射线荧光光谱法测定稀土矿石中的主量元素和稀土元素[J].岩矿测试,2018,20(3):42-45.Zhou W,Zeng M,Wang J,Zhang L,Li Y C.Determination of major and rare earth elements in rare earth ores by X-ray fluorescence spectrometry with fusion sample preparation[J].Rock and Mineral Analysis,2018,37(3):298-305.
[15] Legkodymov A A,Kuper K E,Nazmov V P,et al.Applying hard X-rays to determination of the minimum detection levels of rare earth element by the XRFA-SRmethod[J].Bulletin of the Russian Academy of Sciences Physics,2015,79(1):103-108.
[16] 岩石矿物分析编写组.岩石矿物分析[M].第三分册.第四版.北京:地质出版社,2011.376.The Editorial Committee of Rock and Mineral Analysis[M].Rock and Mineral Analysis (Third Edition:Volume IV).Beijing:Geological Publishing House,2011:376.
[2] 侯振宇,何扬.我国稀土资源概况及应用前景[J].内蒙古科技与经济,2017,(7):28-30.Hou Z Y,He Y.General situation and application prospect of rare earth resources in China[J].Inner Mongolia Science technology & Economy,2017,(7):28-30.
[3] GB/T 6730.23-2006.稀土总量的测定.萃取分离-偶氮氯膦mA分光光度法[S].GB/T 6730.23-2006.Determination of total rare earths with extraction separation-chlorophosphonazo mA by spectrophotometric method[S].
[4] 杨枝,李伯平,罗明标,宋金如,刘维.微色谱柱分离-光度法测定高稀土铁矿石中的微量钍[J].分析试验室,2008,27(3):52-55.Yang Z,Li B P,Luo M B,Song J R,Liu W.Separation of thorium in lanthanon-iron ore samples by microcolumn of HD-8 resin and determination by spectrophotometry[J].Chinese Journal of Analysis Laboratory,2008,27(3):52-55.
[5] GB/T 6730.24-2006,稀土总量的测定.草酸盐重量法[S] .GB/T 6730.24-2006,Determination of total rare earths by oxalate gravimetric method[S] .
[6] 杨瑞瑛,贾秀琴.中子活化法研究中祁连清水沟蛇绿岩中稀土元素的地球化学特征[J].同位素,2006,19(2):65-69.Yang R Y,Jia X Q.Geochemical characteristics of rocks from qingshuigou of middle qilian ophiolete by NAA[J].Journal of Isotopes,2006,19(2):65-69.
[7] Brunfelt A O,Roelandts I,Steinnes E.Determination of rubidium,caesium,barium and eight rare earth elements in ultramafic rocks by neutron-activation analysis[J].Analyst,1974,99:277-284.
[8] Djingova R,Ivanova J.Determination of rare earth elements in soils and sediments by inductively coupled plasma atomic emission spectrometry after cation-exchange separation[J].Talanta,2002,57:821-829.
[9] 吴石头,王亚平,孙德忠,温宏利,许春雪,王伟.电感耦合等离子体发射光谱法测定稀土矿石中15种稀土元素-四种前处理方法的比较[J].岩矿测试,2014,1:12-19.Wu S T,Wang Y P,Sun D Z,Wen H L,Xu C X,Wang W.Determination of 15 rare earth elements in rare earth ores by inductively coupled plasma-atomic emission spectrometry:A Comparison of Four Different Pretreatment Methods[J].Rock and Mineral Analysis,2014,1:12-19.
[10] Beata Z,Katarzyna P,Barbara F,Marzena P,Andrzej K,Rafal S.Determination of rare earth elements by spectroscopic techniques:A review[J].Journal of Analytical Atomic Spectrometry,2011,26 (12):2373-2390.
[11] Frederico G P,Rainerio E J,Tatiana D S.Sample preparation for determination of rare earth elements in geological samples by ICP-MS:A critical review[J].Analytical Letters,2012,45(12):1537-1556.
[12] Tinggi U,Gianduzzo T,Francis R.Determination of selenium in red blood cells by ICP-MS after microwave digestion.Journal of Radioanalytical and Nuclear Chemistry,2004,259(3):469-472
[13] 李小莉,张勤.粉末压片-X射线荧光光谱法测定土壤、水系沉积物和岩石样品中15种稀土元素[J].冶金分析,2013,33(7):35-40.Li X L,Zhang Q.Determination of fifteen rare earth elements in soil,stream sediment and rock samples byX-ray fluorescence spectrometry with pressed powderpellet[J].Metallurgical Analysis,2013,33(7):35-40.
[14] 周伟,曾梦,王健,张磊,李迎春.熔融制样-X射线荧光光谱法测定稀土矿石中的主量元素和稀土元素[J].岩矿测试,2018,20(3):42-45.Zhou W,Zeng M,Wang J,Zhang L,Li Y C.Determination of major and rare earth elements in rare earth ores by X-ray fluorescence spectrometry with fusion sample preparation[J].Rock and Mineral Analysis,2018,37(3):298-305.
[15] Legkodymov A A,Kuper K E,Nazmov V P,et al.Applying hard X-rays to determination of the minimum detection levels of rare earth element by the XRFA-SRmethod[J].Bulletin of the Russian Academy of Sciences Physics,2015,79(1):103-108.
[16] 岩石矿物分析编写组.岩石矿物分析[M].第三分册.第四版.北京:地质出版社,2011.376.The Editorial Committee of Rock and Mineral Analysis[M].Rock and Mineral Analysis (Third Edition:Volume IV).Beijing:Geological Publishing House,2011:376.