熔融制样-波长色散X射线荧光光谱法同时测定超基性岩中主、次及微量成分
|
摘要
采用熔融制样,以四硼酸锂(Li2B4O7)-偏硼酸锂(LiBO2)混合试剂(m:m=12:22)作为熔剂,稀释比为10:1,以硝酸锂(LiNO3)作为氧化剂,碘化铵(NH4I)为脱膜剂,1050℃熔融10 min制备熔片。采用超基性岩、滑石、水镁石、镍矿石、高铬镍铁矿、土壤、水系沉积物等标准物质,并通过上述标准物质的交叉配置得到具有合适梯度范围的系列校准样片。利用变化的理论α系数法对基体效应进行校正,建立了波长色散型X射线荧光光谱测定超基性岩中氧化镁、二氧化硅、三氧化二铁、三氧化二铬、氧化镍、三氧化二铝、氧化钙、氧化钴、氧化钾、氧化锰等10种成分的快速分析方法。采用实验方法对样品中各组分进行测定,结果的相对标准偏差为0. 53%～7. 0%(n=11),方法的测定值与标准物质推荐值一致。
A rapid detection method of magnesium oxide,silicon dioxide,ferric oxide,chromic oxide,nickel oxide,aluminum oxide,calcium oxide,cobalt oxide,potassium oxide and manganese oxide in ultrabasic rock was established by wavelength dispersive X-ray fluorescence spectrometry. The sample was prepared by the fusion method under the following conditions: Li2 B4 O7-Li BO2 mixture[m( Li2 B4 O7) : m( Li BO2) =12: 22]as flux,Li NO3 as oxidant,NH4 I as mold discharging agent,the dilution ratio of 10: 1 and fusion at 1050℃ for 10 min. The calibration curves were constructed by using the certified reference materials including ultrabasic rock,talcum,brucite,nickel ores,josephinite with high chromium,soils and stream sediments,as well as the synthesized samples by mixing them in a certain ratio,and the matrix effect was corrected by variable theoretical α influence coefficient method.The confirmatory experiment showed that the relative standard deviations( RSDs,n = 11) was 0. 53% ～7. 0%,and the results were consistent with the certified values of reference materials.
A rapid detection method of magnesium oxide,silicon dioxide,ferric oxide,chromic oxide,nickel oxide,aluminum oxide,calcium oxide,cobalt oxide,potassium oxide and manganese oxide in ultrabasic rock was established by wavelength dispersive X-ray fluorescence spectrometry. The sample was prepared by the fusion method under the following conditions: Li2 B4 O7-Li BO2 mixture[m( Li2 B4 O7) : m( Li BO2) =12: 22]as flux,Li NO3 as oxidant,NH4 I as mold discharging agent,the dilution ratio of 10: 1 and fusion at 1050℃ for 10 min. The calibration curves were constructed by using the certified reference materials including ultrabasic rock,talcum,brucite,nickel ores,josephinite with high chromium,soils and stream sediments,as well as the synthesized samples by mixing them in a certain ratio,and the matrix effect was corrected by variable theoretical α influence coefficient method.The confirmatory experiment showed that the relative standard deviations( RSDs,n = 11) was 0. 53% ～7. 0%,and the results were consistent with the certified values of reference materials.
引文
[1] Zeng M Y,Wang D M,Chen Y B,Yang M,Song S. Rock Miner. Anal.,2011,30(4):501曾美云,王迪民,陈燕波,杨梅,宋松.岩矿测试,2011,30(4):501
[2] Zhao L Z. Heilongjiang Sci.,2017,8(6):10赵立卓.黑龙江科学,2017,8(6):10
[3] Yuan C W. Xinjiang Nonferrous Met.,2017,40(3):97袁春伟.新疆有色金属,2017,40(3):97
[4] Feng X,Song X H,Duan Y W,Yang G X. Chin. J. Inorg. Anal. Chem.,2013,3(S1):20冯旭,宋晓红,段伟亚,杨桂香.中国无机分析化学,2013,3(S1):20
[5] Wang N. Xinjiang Nonferrous Met.,2013,(S1):148王娜.新疆有色金属,2013,(S1):148.
[6] Li F Q. Heilongjiang Sci&Technol. Inf.,2016,(13):88.李风琴.黑龙江科技信息,2016,(13):88.
[7] Bai W L,Zhang A F,Shi L,Ma H X,Liu J. Metall. Anal.,2016,36(10):40白万里,张爱芬,石磊,马慧侠,刘静.冶金分析,2016,36(10):40
[8] Zhong J H,Chen J F,Zhang Y Y,Zheng R J,Chen Q,Zhang Q X. Chin. J. Anal. Lab.,2016,35(7):826钟坚海,陈金凤,张艳燕,郑瑞娟,陈权,张奇勋.分析试验室,2016,35(7):826
[9] Zhu L,Wang J,Yin L H. Chin. J. Anal. Lab.,2017,36(9):1084朱俐,王瑾,尹利辉.分析试验室,2017,36(9):1084
[10] Ma J Z,liu H J,Wang F. Chin. J. Anal. Lab.,2016,35(11):1348马景治,刘恒杰,王峰.分析试验室,2016,35(11):1348
[11] Wang L,Zhang J Q,Hua B. Chin. J. Anal. Lab.,2017,36(6):738王凌,张家琪,华犇.分析试验室,2017,36(6):738.
[12] Fernand C,Jimmy S. B. Physics and Chemistry of Borate Melting,Translated by Zhuo S J. Shanghai:East China University of Science and Technology Press,2006:23Fernand C,Jimmy S. B.硼酸盐熔融的物理与化学.卓尚军译.上海:华东理工大学出版社,2006:23
[13] Xu Z B,Zhao C,Yuan L Z,Yang G H,Wang Z. Metall. Anal.,2015,35(7):27徐志彬,赵超,苑丽质,杨国辉,王钊.冶金分析,2015,35(7):27
[14] Li G H,Li X L. Metall. Anal.,2015,35(7):1李国会,李小莉.冶金分析,2015,35(7):1
[15] Dan J,Liu Y Q,Chen X Y,Li Z J,Liu L. Metall. Anal.,2015,35(7):48但娟,刘元清,陈小毅,李子敬,刘林.冶金分析,2015,35(7):48
[16] Wu Biao,Wen Jiankang,Wang Dianzuo. Chin J Rare Met,2017,41(6):720武彪,温建康,王淀佐.稀有金属,2017,41(6):720
[2] Zhao L Z. Heilongjiang Sci.,2017,8(6):10赵立卓.黑龙江科学,2017,8(6):10
[3] Yuan C W. Xinjiang Nonferrous Met.,2017,40(3):97袁春伟.新疆有色金属,2017,40(3):97
[4] Feng X,Song X H,Duan Y W,Yang G X. Chin. J. Inorg. Anal. Chem.,2013,3(S1):20冯旭,宋晓红,段伟亚,杨桂香.中国无机分析化学,2013,3(S1):20
[5] Wang N. Xinjiang Nonferrous Met.,2013,(S1):148王娜.新疆有色金属,2013,(S1):148.
[6] Li F Q. Heilongjiang Sci&Technol. Inf.,2016,(13):88.李风琴.黑龙江科技信息,2016,(13):88.
[7] Bai W L,Zhang A F,Shi L,Ma H X,Liu J. Metall. Anal.,2016,36(10):40白万里,张爱芬,石磊,马慧侠,刘静.冶金分析,2016,36(10):40
[8] Zhong J H,Chen J F,Zhang Y Y,Zheng R J,Chen Q,Zhang Q X. Chin. J. Anal. Lab.,2016,35(7):826钟坚海,陈金凤,张艳燕,郑瑞娟,陈权,张奇勋.分析试验室,2016,35(7):826
[9] Zhu L,Wang J,Yin L H. Chin. J. Anal. Lab.,2017,36(9):1084朱俐,王瑾,尹利辉.分析试验室,2017,36(9):1084
[10] Ma J Z,liu H J,Wang F. Chin. J. Anal. Lab.,2016,35(11):1348马景治,刘恒杰,王峰.分析试验室,2016,35(11):1348
[11] Wang L,Zhang J Q,Hua B. Chin. J. Anal. Lab.,2017,36(6):738王凌,张家琪,华犇.分析试验室,2017,36(6):738.
[12] Fernand C,Jimmy S. B. Physics and Chemistry of Borate Melting,Translated by Zhuo S J. Shanghai:East China University of Science and Technology Press,2006:23Fernand C,Jimmy S. B.硼酸盐熔融的物理与化学.卓尚军译.上海:华东理工大学出版社,2006:23
[13] Xu Z B,Zhao C,Yuan L Z,Yang G H,Wang Z. Metall. Anal.,2015,35(7):27徐志彬,赵超,苑丽质,杨国辉,王钊.冶金分析,2015,35(7):27
[14] Li G H,Li X L. Metall. Anal.,2015,35(7):1李国会,李小莉.冶金分析,2015,35(7):1
[15] Dan J,Liu Y Q,Chen X Y,Li Z J,Liu L. Metall. Anal.,2015,35(7):48但娟,刘元清,陈小毅,李子敬,刘林.冶金分析,2015,35(7):48
[16] Wu Biao,Wen Jiankang,Wang Dianzuo. Chin J Rare Met,2017,41(6):720武彪,温建康,王淀佐.稀有金属,2017,41(6):720