偏振激发能量色散X射线荧光光谱仪在野外矿区现场实验室的应用探讨
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摘要
为提高野外找矿人员工作效率,探索测试设备直接在野外现场服务地质找矿事业的问题,项目组在辽宁丹东野外Fe-Cu-Co矿区以集装箱改造房作为实验测试场所,以小型偏振激发能量色散X射线荧光光谱仪(P-EDXRF)为测试手段,配备相应的电力供应系统、碎样系统以及配套相应的野外测试方法和样品前处理方法,建立了可独立工作的野外现场分析实验室。利用该矿区两个样品,现场进行精密度实验,Fe、Cu、Co 3种元素相对标准偏差(RSD)都在6%以下;利用标准样品GBW07233、GBW07296、GBW07306进行正确度实验,3种元素相对误差在10%以下。将野外现场分析实验室测试数据与找矿单位提供的30件矿区样品中Fe、Cu、Co 3个元素的室内实验室测试数据进行比较,Fe、Cu符合度较高,可以进行定量测试,Co的测试效果相对较差,建议只提供半定量数据,但均可以对其异常区进行准确圈定。研究表明,该类型实验室可以在野外条件下独立承担多种元素的测试工作,达到快速圈定元素异常区的目的,为野外找矿工作发挥现场技术支撑作用。
In order to improve the work efficiency of prospecting persons in field,the direct application of test equipment in field service of prospecting was explored.The project team built a test place in field in Fe-Cu-Co mining area of Liaoning Dandong based on one container reconstruction house.The minitype polarization excitation energy dispersive X-ray fluorescence spectrometer(P-EDXRF)was employed.The corresponding power supply system and sample smashing system were equipped.The field test method and sample pretreatment method were also matched.The laboratory for on-site analysis in field which could be independently operated was established.Two samples from this mining area were used for precision test.The relative standard deviations(RSD)for Fe,Cu and Co were all less than 6%.National standard samples(GBW07233,GBW07296 and GBW07306)were used for trueness test.The relative errors of three elements were less than 10%.The measuring results of 30 samples in laboratory in field were compared with those obtained by other indoor laboratories.It was found that the conformity of Fe and Cu was high and the proposed method could be applied for quantitative analysis.The test results of Co were relatively bad.It suggested providing semi-quantitative data.However,the abnormal areas could be accurately delineated.The experiments showed that this type of on-site laboratory could independently undertake the testing of several elements for the rapid delineation of abnormal areas.The proposed study provided technical support for the prospecting in field.
In order to improve the work efficiency of prospecting persons in field,the direct application of test equipment in field service of prospecting was explored.The project team built a test place in field in Fe-Cu-Co mining area of Liaoning Dandong based on one container reconstruction house.The minitype polarization excitation energy dispersive X-ray fluorescence spectrometer(P-EDXRF)was employed.The corresponding power supply system and sample smashing system were equipped.The field test method and sample pretreatment method were also matched.The laboratory for on-site analysis in field which could be independently operated was established.Two samples from this mining area were used for precision test.The relative standard deviations(RSD)for Fe,Cu and Co were all less than 6%.National standard samples(GBW07233,GBW07296 and GBW07306)were used for trueness test.The relative errors of three elements were less than 10%.The measuring results of 30 samples in laboratory in field were compared with those obtained by other indoor laboratories.It was found that the conformity of Fe and Cu was high and the proposed method could be applied for quantitative analysis.The test results of Co were relatively bad.It suggested providing semi-quantitative data.However,the abnormal areas could be accurately delineated.The experiments showed that this type of on-site laboratory could independently undertake the testing of several elements for the rapid delineation of abnormal areas.The proposed study provided technical support for the prospecting in field.
引文
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[12]焦距,詹秀春,翟磊,等.无外接电源富集装置-手持式XRF现场分析水体中重金属[J].光谱学与光谱分析,2017,37(1):267-272.JIAO Ju,ZHAN Xiu-chun,ZHAI Lei,et al.On-site analysis of heavy metals in water with handheld X-ray fluorescence and pre-concentration device without external power supply[J].Spectroscopy and Spectral Analysis,2017,37(1):267-272.
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[16]Heckel J.Using Barkla polarized X-ray radiation in energy dispersive X-ray fluorescence analysis(EDXRF)[J].Journal of Trace and Microprobe Techniques,1995,13(2):97-108.
[17]Kramar U.Advances in energy-dispersive X-ray fluorescence[J].Journal of Geochemical Exploration,1997,58(1):73-80.
[18]张素荣,杨帆,张华,等.青藏高原条件下现场分析方法的适应性[J].物探与化探,2014,38(1):100-105.ZHANG Su-rong,YANG Fan,ZHANG Hua,et al.The suitability of field analytical methods under the special conditions of Tibetan Plateau[J].Geophysical and Geochemical Exploration,2014,38(1):100-105.
[19]李强,张学华.手持式X射线荧光光谱仪测定富钴结壳样品中锰铁钴镍铜锌[J].岩矿测试,2013,32(5):724-728.LI Qiang,ZHANG Xue-hua.Determination of Mn,Fe,Co,Ni,Cu and Zn in cobalt-rich crusts by portable X-ray fluorescence spectrometry[J].Rock and Mineral A-nalysis,2013,32(5):724-728.
[20]Weider S Z,Nittler L R,Starr R D,et al.Evidence for geochemical terranes on mercury:Global mapping of major elements with MESSENGER′s X-ray spectrometer[J].Earth and Planetary Science Letters,2015,416:109-120.
[21]Escárate P,Bailo D,Guesalaga A,et al.Energy dispersive X-ray diffraction spectroscopy for rapid estimation of calcite in copper ores[J].Minerals Engineering,2009,22:566-571.
[22]张鹏,张寿庭,邹灏,等.便携式X荧光分析仪在萤石矿勘查中的应用[J].物探与化探,2012,36(5):718-722.ZHANG Peng,ZHANG Shou-ting,ZOU Hao,et al.The application of portable X-ray fluorescence analyzer to fluorite prospecting[J].Geophysical and Geochemical Exploration,2012,36(5):718-722.
[23]樊兴涛,李迎春,王广,等.车载台式能量色散X射线荧光光谱仪在地球化学勘查现场分析中的应用[J].岩矿测试,2011,30(2):155-159.FAN Xing-tao,LI Ying-chun,WANG Guang,et al.On-site geochemical exploration analysis by vehicle-loaded energy dispersive X-ray fluorescence spectrometry[J].Rock and Mineral Analysis,2011,30(2):155-159.
[24]詹秀春,樊兴涛,李迎春,等.直接粉末制样-小型偏振激发能量色散X射线荧光光谱法分析地质样品中多元素[J].岩矿测试,2009,28(6):501-506.ZHAN Xiu-chun,FAN Xing-tao,LI Ying-chun,et al.Multi-element determination in geological materials by bench-top polarized energy dispersive X-ray fluorescence spectrometry coupled with directly pressed powder sample preparation technique[J].Rock and Mineral Analysis,2009,28(6):501-506.
[2]Lanson B,Ferrage E,Hubert F,et al.Experimental aluminization of vermiculite interlayers:An X-ray diffraction perspective on crystal chemistry and structural mechanisms[J].Geoderma,2015,249-250:28-39.
[3]Ortolano G,Zappal L,Mazzoleni P.X-ray map analyser:A new ArcGIS based tool for the quantitative statistical data handling of X-ray maps(geo-and material-science applications)[J].Computers and Geosciences,2014,72:49-64.
[4]赵琦.X荧光测量在区域化探异常检查中的应用[J].四川地质学报,2000,20(2):158-160.ZHAO Qi.The application of X-ray fluorescence analysis to regional geochemical anomaly exploration[J].Acta Geologica Sichuan,2000,20(2):158-160.
[5]蒯丽君,樊兴涛,詹秀春,等.酸消解-车载偏振能量色散X射线荧光法现场测定祁曼塔格多金属矿中高品位铜铅锌[J].岩矿测试,2013,32(4):538-546.KUAI Li-jun,FAN Xing-tao,ZHAN Xiu-chun,et al.On-site analysis of Cu,Pb and Zn in polymetallic ores from Qimantage area by vehicle-loaded polarized energy dispersive X-ray fluorescence spectrometer with acid digestion[J].Rock and Mineral Analysis,2013,32(4):538-546.
[6]Kaniu M I,Angeyo K H.Challenges in rapid soil quality assessment and opportunities presented by multivariate chemometric energy dispersive X-ray fluorescence and scattering spectroscopy[J].Geoderma,2015,241-242:32-40.
[7]Kaniu M I,Angeyo K H,Mwala A K,et al.Direct rapid analysis of trace bioavailable soil macronutrients by chemometrics-assisted energy dispersive X-ray fluorescence and scattering spectrometry[J].Analytica Chimica Acta,2012,729:21-25.
[8]Paulette L,Man T,Weindorf D C,et al.Rapid assessment of soil and contaminant variability via portable X-ray fluorescence spectroscopy:Copsa Mic,Romania[J].Geoderma,2015,243-244:130-140.
[9]Zhu Y D,Weindorf D C,Zhang W T.Characterizing soils using aportable X-ray fluorescence spectrometer:1.Soil texture[J].Geoderma,2011,167-168:167-177.
[10]方哲,陈吉文,胡少成,等.基于X射线荧光光谱技术的燃煤电厂烟气重金属铅的在线监测方法应用[J].冶金分析,2016,36(2):1-6.FANG Zhe,CHEN Ji-wen,HU Shao-cheng,et al.Application of on-line monitoring method of heavy metal lead in coal burning power plant flue gas based on X-ray fluorescence spectrometry[J].Metallurgical Analysis,2016,36(2):1-6.
[11]方哲,陈吉文.基于X射线荧光光谱的大气重金属在线分析方法的评估及应用[J].冶金分析,2015,35(3):1-6.FANG Zhe,CHEN Ji-wen.Evaluation and application of the analysis method of atmospheric heavy metal online based on X-ray fluorescence spectrometry[J].Metallurgical Analysis,2015,35(3):1-6.
[12]焦距,詹秀春,翟磊,等.无外接电源富集装置-手持式XRF现场分析水体中重金属[J].光谱学与光谱分析,2017,37(1):267-272.JIAO Ju,ZHAN Xiu-chun,ZHAI Lei,et al.On-site analysis of heavy metals in water with handheld X-ray fluorescence and pre-concentration device without external power supply[J].Spectroscopy and Spectral Analysis,2017,37(1):267-272.
[13]Poen S O,John N R.A focusing X-ray polarizer for energy-dispersive analysis[J].X-Ray Spectrometry,1978,7(4):241-248.
[14]Wobrauschek P,Aiginger H.X-ray fluorescence analysis using intensive linear polarized monochromatic X-ray after Bragg reflection[J].X-Ray Spectrometry,1980,9(2):57-59.
[15]Heckel J,Brumme M,Weinert A,et al.Multi-element trace analysis of rocks and soils by EDXRF using polarized radiation[J].X-Ray Spectrometry,1991,20:287-292.
[16]Heckel J.Using Barkla polarized X-ray radiation in energy dispersive X-ray fluorescence analysis(EDXRF)[J].Journal of Trace and Microprobe Techniques,1995,13(2):97-108.
[17]Kramar U.Advances in energy-dispersive X-ray fluorescence[J].Journal of Geochemical Exploration,1997,58(1):73-80.
[18]张素荣,杨帆,张华,等.青藏高原条件下现场分析方法的适应性[J].物探与化探,2014,38(1):100-105.ZHANG Su-rong,YANG Fan,ZHANG Hua,et al.The suitability of field analytical methods under the special conditions of Tibetan Plateau[J].Geophysical and Geochemical Exploration,2014,38(1):100-105.
[19]李强,张学华.手持式X射线荧光光谱仪测定富钴结壳样品中锰铁钴镍铜锌[J].岩矿测试,2013,32(5):724-728.LI Qiang,ZHANG Xue-hua.Determination of Mn,Fe,Co,Ni,Cu and Zn in cobalt-rich crusts by portable X-ray fluorescence spectrometry[J].Rock and Mineral A-nalysis,2013,32(5):724-728.
[20]Weider S Z,Nittler L R,Starr R D,et al.Evidence for geochemical terranes on mercury:Global mapping of major elements with MESSENGER′s X-ray spectrometer[J].Earth and Planetary Science Letters,2015,416:109-120.
[21]Escárate P,Bailo D,Guesalaga A,et al.Energy dispersive X-ray diffraction spectroscopy for rapid estimation of calcite in copper ores[J].Minerals Engineering,2009,22:566-571.
[22]张鹏,张寿庭,邹灏,等.便携式X荧光分析仪在萤石矿勘查中的应用[J].物探与化探,2012,36(5):718-722.ZHANG Peng,ZHANG Shou-ting,ZOU Hao,et al.The application of portable X-ray fluorescence analyzer to fluorite prospecting[J].Geophysical and Geochemical Exploration,2012,36(5):718-722.
[23]樊兴涛,李迎春,王广,等.车载台式能量色散X射线荧光光谱仪在地球化学勘查现场分析中的应用[J].岩矿测试,2011,30(2):155-159.FAN Xing-tao,LI Ying-chun,WANG Guang,et al.On-site geochemical exploration analysis by vehicle-loaded energy dispersive X-ray fluorescence spectrometry[J].Rock and Mineral Analysis,2011,30(2):155-159.
[24]詹秀春,樊兴涛,李迎春,等.直接粉末制样-小型偏振激发能量色散X射线荧光光谱法分析地质样品中多元素[J].岩矿测试,2009,28(6):501-506.ZHAN Xiu-chun,FAN Xing-tao,LI Ying-chun,et al.Multi-element determination in geological materials by bench-top polarized energy dispersive X-ray fluorescence spectrometry coupled with directly pressed powder sample preparation technique[J].Rock and Mineral Analysis,2009,28(6):501-506.
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