28 September 2025, Volume 45 Issue 9
    

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  • Bibliometric study of X-ray fluorescence spectrometry in past 65 years in China
    DENG Saiwen, WANG Yiya, WANG Yimin, GAO Xinhua, LI Song, LIU Chenghai
    Metallurgical Analysis. 2025, 45(9): 1-14. https://doi.org/10.13228/j.boyuan.issn1000-7571.012885
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    The development of X-ray fluorescence spectrometry (XRF) has undergone 65 years in China,and the quantity of relevant technical literatures has exceeded 14 000. In 2019, the publication of paper Bibliometric analysis on research trend of X-ray fluorescence spectrometry based on CNKI and the book The literature index of X-ray fluorescence spectrometry analysis in China (1960-2015) opened up the statistical and quantitative research on the X-ray fluorescence spectrometry(XRF) literatures in China.On the basis of above two literatures and referring to the recently published review papers,this paper summarized the basic situation of Chinese XRF literatures from 1960 to 2024 in terms of bibliometric statistics,review papers and monographs(translated works),as well as the development process of technology and new technologies and applications.The section of literature metrology and statistics briefly introduced the types of XRF literatures in China,and focused on the main achievements of statistical research,which mainly included the annual distribution of total number of literatures,the overall distribution of journal literatures and the top 10 journals with the largest number of literatures.The section of paper review compiled 226 various review papers published over a span of 65 years from 1960 to 2024.The papers were reviewed according to the categorization of comprehensive reviews,annual reviews,and thematic reviews.The thematic reviews included the instrument (devices) and core components,software and sample preparation techniques,advancements in various application fields.The evaluations of these advancements included geological sample analysis,metallurgy and non-ferrous metals,environment and materials science,agriculture,food, and biomedicine,petrochemicals and process analysis,scientific archaeology and criminal investigation,precious metal jewelry and gemstones testing,and standard methods.The section of specialized(translated) works collected 31 specialized(translated) works officially published in China since the development of X-ray fluorescence spectrometry analysis,and provided a brief introduction by category.
  • Literature review on detection and X-ray fluorescence spectrometry analysis technique of silicon-based ferroalloy
    BAO Xibo, ZHAO Jing
    Metallurgical Analysis. 2025, 45(9): 15-28. https://doi.org/10.13228/j.boyuan.issn1000-7571.012925
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    Silicon-based ferroalloys are widely used in the steel metallurgy and casting industries as deoxidizers,alloying agents and inoculants.For the scientific guidance of production and application,it is of great significance to accurately and rapidly detect the main and trace alloy components in silicon-based ferroalloys.Due to the advantages of high precision,high sensitivity,accuracy,rapidity and high degree of automation,X-ray fluorescence spectrometry(XRF) analysis has played a crucial role in many fields such as on-site quality control in production,research and development of new materials,exploration of physical and mineral resources,environmental protection and cultural relic identification.As an important analytical method for characterizing the chemical composition and properties of substances,XRF has gradually been deeply studied and widely applied in the composition detection of silicon-based ferroalloys since the 1990s.The author has retrieved that 4 monographs related to the analysis of silicon-based ferroalloys have been compiled by chemical detection technicians in China. 30 classic chemical analysis standard methods and 27 modern instrumental analysis standard methods for silicon-based ferroalloys were studied and formulated.A total of 44 research papers on the analysis of the chemical composition and technology of silicon-based ferroalloys by XRF method have been published in various journals,magazines and national industry conference paper collections,including 21 papers on the analysis of silicon-based ferroalloys by XRF with pressed powder pellet and 23 papers on the analysis of silicon-based ferroalloys by XRF method with fusion sample preparation.The sample preparation technology,the selection of reference materials,the calibration of working curves,the scientific nature of detection data and the application prospects of silicon-based ferroalloys analyzed by XRF were briefly reviewed in this paper. Total 105 articles were cited.
  • On-site analysis of 9 inorganic elements in nickel ore sample by total reflection X-ray fluorescence spectrometry
    LIU Xiao, FAN Xingtao, ZHAN Xiuchun
    Metallurgical Analysis. 2025, 45(9): 29-34. https://doi.org/10.13228/j.boyuan.issn1000-7571.012851
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    The sample was prepared into suspension,and the effects of factors such as the dispersant and sample mass concentration in suspension on the analytical results by total reflection X-ray fluorescence spectrometry(TXRF) were investigated.The method for the determination of Ca,Ti,Cr,Mn,Fe,Co,Ni,Cu,and Zn in nickel ore samples by TXRF was established.The proposed method was applied for on-site application demonstration in Chengde,Hebei Province.The experimental results showed that the quantitative analysis accuracy of Zn would be affected when Ga or Ge was used as the internal standard element because the spectral peaks of Ga and Ge were close to those of the measured element Zn.Therefore,Se was selected as the internal standard element in experiments.The recoveries of elements were closer to 100% when ultrapure water was used as the dispersant.As the sample mass concentration in suspension increased,the recoveries of elements first showed an upward trend,then gradually stabilized at 100%,and then significantly decreased and seriously deviated from 100%.In order to obtain accurate measurement results,the sample mass concentration should be controlled in range of 10-20 mg/mL.The limits of detection were between 0.009 0 μg/g and 0.068 μg/g,and the relative standard deviations(RSD) were better than 15%.3 certified reference materials laterite nickel ore were determined according to the experimental method.The found results of TXRF analysis were consistent with the certified values and those obtained by inductively coupled plasma mass spectrometry(ICP-MS),which could meet the requirements of on-site analysis.The on-site analysis of nickel ore samples by TXRF was conducted in Chengde,Hebei Province,and the analysis results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry(ICP-AES) or ICP-MS.The absolute values of relative error for most data were less than 20%,which proved the reliability of suspension sample preparation and on-site analysis of nickel ore samples. The proposed method provided technical support for the on-site exploration of nickel ore.
  • Study on the origin traceability of imported iron ore based on multi-element analysis combined with machine learning algorithms
    LI Tao, WEI Bingyan, ZHAO Jiangyong, YAN Sha, ZHENG Yunlong, FENG Shuang
    Metallurgical Analysis. 2025, 45(9): 35-41. https://doi.org/10.13228/j.boyuan.issn1000-7571.012913
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    The price and quality of imported iron ore are affected by the origin.The iron ore from different origins has unique elemental contents due to the difference of metallogenic environment and mineral associated characteristics.To deal with the problem of misrepresentation of the origin for imported iron ores,this study aimed to construct an origin traceability model,which integrated the machine learning algorithms and X-ray fluorescence spectrometry(XRF),to achieve precise classification of imported iron ores from 6 countries including Australia and Brazil.This study could provide technical support for trade supervision to avoid trade fraud.Total 610 batches of imported iron ore samples were collected,and 15 items were detected,including the contents of Fe,SiO2,Al2O3P,K2O,TiO2,MgO,CaO,Mn and Cu(determined by XRF),Hg,F,Cl and S(determined by other technologies) as well as the loss on ignition (L.O.I).Data preprocessing and sample balancing were performed using Python.6 models including C5.0 decision tree,CART decision tree,neural network,support vector machine,logistic regression and discriminant analysis were employed to analyze the correlation between elemental characteristics and origins.The key variables were screened to validate the model performance.The results showed that the neural network model achieved the highest test-set accuracy rate of 98.92%,while the C5.0 decision tree model based on 5 key variables(Al2O3,Fe,S,Hg content and L.O.I) achieved an accuracy rate of 97.85%,which was significantly higher than the traditional linear model(e.g.,logistic regression of 88.71%).The integration of XRF and machine learning broke through the linear limitation of conventional elemental analysis.The models such as C5.0 decision tree demonstrated superior performance in variable utilization efficiency and classification accuracy,which offered an efficient solution for origin traceability of iron ore.
  • Determination of major and minor components in copper-cobalt mixed concentrate by X-ray fluorescence spectrometry with fusion sample preparation
    ZHOU Cunkuan, YU Xue, SU Liming, QIN Qun
    Metallurgical Analysis. 2025, 45(9): 42-47. https://doi.org/10.13228/j.boyuan.issn1000-7571.012888
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    In view of the low content of Co in domestic reference materials copper concentrate, the content range of Co was expanded in experiments by adding spectrally pure substance Co2O3.The calibration curves were established using 17 certified reference materials/reference materials copper concentrate,and 5 artificially synthesized copper-cobalt mixed concentrate calibration samples.The determination of 15 components(Cu,Co,S,Pb,Zn,Mn,Ni,As,Bi,SiO2,Al2O3,TFe,K2O,CaO and MgO) in copper-cobalt mixed concentrate was achieved by X-ray fluorescence spectrometry(XRF) with fusion sample preparation.The conditions for fusion sample preparation were optimized:0.200 0 g of sample and 1.500 0 g of LiNO3 were fully ground and mixed in agate mortar,and then encapsulated in 6.000 0 g of Li2B4O7-LiBO2 mixed flux.The mixture was pre-oxidized at 650 ℃ to effectively inhibit the volatilization of S.Then 4 drops of 500 g/L LiBr solution were added as the release agent.The fused bead was prepared by rotating and fusion at 1 050 ℃ for 10 min.The theoretical α coefficient method was used to correct the matrix effect,and interference correction was required for the elements with spectral line overlapping.The correlation coefficients of calibration curves were all higher than 0.999,and the limits of detection were between 12 μg/g and 255 μg/g.One copper-cobalt mixed concentrate sample was used for precision test,and the relative standard deviations(RSD,n=11) of determination results of components ranged from 0.32% to 8.9%.The trueness tests were conducted using reference material copper concentrate(GBW(E)070199) without participation of regression correction,artificial synthesized calibration sample(NK#) and production samples(1# and 2#).The found results by this method were basically consistent with the certified values/reference values and the results determined by national standard methods.The proposed method had certain guiding significance for the determination of copper concentrate sample with high content of Co.
  • Determination of 8 components in red mud with high content of iron by X-ray fluorescence spectrometry with fusion sample preparation
    PENG Zhan, LIU Jing, MA Huixia
    Metallurgical Analysis. 2025, 45(9): 48-55. https://doi.org/10.13228/j.boyuan.issn1000-7571.012775
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    The content of iron oxide in red mud with high content of iron is up to 75%(mass fraction),and it has high-sodium and high-calcium characteristics which are different from iron ore. There is a problem in lack of corresponding reference materials to draw calibration curves when X-ray fluorescence spectrometry (XRF) is used for determination.In experiments,the mixed flux (the mass ratio of Li2B4O7 to LiBO2 was 12∶22) and cobalt internal standard flux (the mass ratio of mixed flux to Co2O3 was 10∶1) were mixed with red mud sample(with high content of iron) with dilution ratio of 1∶14. The fused bead was prepared after fusion at 1 070 ℃ for 13 min.The calibration curve was prepared by mixing high-purity/spectroscopically pure substances and primary standard substances in reference materials to prepare the artificially synthesized calibration samples.The cobalt internal standard was used for the calibration of iron.The method for the determination of 8 components(including Al2O3,SiO2,Fe2O3,TiO2,K2O,Na2O,CaO and MgO) in red mud with high content of iron by XRF was established.The content of 8 components in 2 red mud samples with high content of iron was determined according to the experimental method.The relative standard deviations(RSD,n=11) of determination results were between 0.14% and 10%.The content of 8 components in reference material iron ore GSBD31005a and artificially synthesized calibration sample of red mud was determined according to the experimental method.The found results were consistent with the standard/reference values.
  • Determination of aluminum oxide,strontium oxide,europium oxide and dysprosium oxide in phosphors by wavelength dispersive X-ray fluorescence spectrometry with fusion sample preparation
    CHEN Xin, WANG Nan, YANG Yu, GAO Xiaoyuan, ZENG Ze, FU Yao
    Metallurgical Analysis. 2025, 45(9): 56-61. https://doi.org/10.13228/j.boyuan.issn1000-7571.012778
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    It is very important to determine the content of each component in the production process of phosphors,which can provide powerful guidance to adjust the ingredient proportion of product.Moreover,the content of components in phosphors is also required in the customs import and export commodity supervision to determine the commodity tax number.Therefore,it is necessary to establish a method for the determination of components in phosphors.In experiment, the phosphors sample was firstly calcined at 1 000 ℃ for 1 h.Lithium tetraborate was used as the flux,and dilution ratio was 1∶40.Sodium iodide solution was selected as the release agent.After melting at 1 080 ℃ for 20 min,the fused glass sheet was prepared for the determination by wavelength dispersive X-ray fluorescence spectrometry(WD-XRF).Consequently,the determination of aluminum oxide,strontium oxide,europium oxide and dysprosium oxide in phosphors by WD-XRF with fusion sample preparation was realized.The calibration sample series were artificially synthesized using spectroscopically pure strontium aluminate,aluminum oxide,strontium nitrate,europium oxide and dysprosium oxide.The matrix effect correction and absorption enhancement effect was conducted by theoretical α coefficient method in the instrument software.The linearity of calibration curves of each component was good with correlation coefficients not less than 0.998 9.The limit of detection of aluminum oxide,strontium oxide,europium oxide and dysprosium oxide was 0.038%,0.064%,0.012% and 0.009 6%,respectively.4 components in phosphor were determined according to the experimental method,and the relative standard deviations(RSD, n=11) of determination results were between 0.20% and 1.2%.The measured results were consistent with the theoretical values.
  • Determination of copper,iron,lead and zinc in copper concentrate by microwave digestion-energy dispersive X-ray fluorescence spectrometry
    WANG Lili, WANG Lei, ZHAO Chao, LIU Qi, LIU Zhiying, RAO Jinwu SHAO Yating, AI Yuanhua
    Metallurgical Analysis. 2025, 45(9): 62-68. https://doi.org/10.13228/j.boyuan.issn1000-7571.012820
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    Copper concentrate is kind of smelting raw material produced from low-grade copper bearing raw ore by grinding,ball milling and reagent flotation to enrich copper minerals.At present,the element detection in copper concentrate is mainly based on GB/T 3884 standard series.However,these standard methods have some shortcomings,for example,the main and trace elements are hardly determined synchronously,and the pretreatment is complex with long testing period.In this study,copper concentrate was quickly digested into solution by microwave digestion with 8 mL of reversed aqua regia and 0.1 mL of hydrofluoric acid mixed acid system to eliminate the sample heterogeneity and particle size effect.The standard solution series were prepared to draw calibration curve.A method for the determination of copper,iron,lead and zinc in copper concentrate by energy dispersive X-ray fluorescence spectrometry(EDXRF) was established.The determination range of copper and iron was 10%-40% (mass fraction,the same below),and 1%-10% for lead and zinc.The linear correlation coefficients of calibration curves were all greater than 0.998.The proposed method was applied for the determination of copper,iron,lead and zinc in 3 copper concentrate samples,and the relative standard deviations(RSD,n=11) of determination results were less than 0.2%.The content of copper,iron,lead and zinc in 4 certified reference materials copper concentrate(ZBK337,ZBK338,ZBK340 and 116#) were determined according to the experimental method,and the found results were consistent with the standard values.The content of copper,iron,lead and zinc in 2 copper concentrate samples was determined by this method and GB/T 3884 standard method series(iodimetry for copper,potassium dichromate titration for iron,and inductively coupled plasma atomic emission spectrometry(ICP-AES) for lead and zinc). The difference could meet the requirements of reproducibility tolerance in GB/T 3884.
  • Determination of tin and lead in tin-lead alloy by X-ray fluorescence spectrometry
    ZHANG Yingwen, TIAN Lunfu, DAI Yichun
    Metallurgical Analysis. 2025, 45(9): 69-73. https://doi.org/10.13228/j.boyuan.issn1000-7571.012870
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    Tin-lead alloy is an important soldering metal,and its welding performance is directly affected by the elemental composition.Therefore,the determination of tin and lead content in tin-lead alloy is of great significance.In order to address the lack of certified reference materials tin-lead alloy,a set of tin-lead alloys with gradient compositions were self-prepared and then used as calibration samples after measurement by chemical titration.The content of tin and lead in tin-lead alloy was determined by X-ray fluorescence spectrometry(XRF).During the establishment of calibration curves,it was found that the linear calibration curve could not adequately fit the relationship between X-ray fluorescence spectral intensity and content due to the strong absorption-enhancement effect between tin and lead.Consequently,the quadratic curve was adopted to establish calibration curves for Sn Kα and Pb Lα spectral lines,which could increase the determination coefficients to 0.999 4 with better fitting performance.Presion test was conducted on tin-lead alloy sample,and the relative standard deviations(RSD,n=7) were below 0.1%.The found results of tin-lead alloy sample by XRF were consistent with those obtained by chemical titration.This method was suitable for detecting 55%-75%(mass fraction,the same below) tin and 25%-45% lead in tin-lead alloy,which could meet the requirements of production and detection.
  • Determination of 9 major and minor components in matte by X-ray fluorescence spectrometry with fusion sample preparation
    LIU Tianyi, LI Tengfei
    Metallurgical Analysis. 2025, 45(9): 74-80. https://doi.org/10.13228/j.boyuan.issn1000-7571.012912
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    The traditional chemical analysis methods for matte are cumbersome and time-consuming in operation.The method for simultaneous determination of 9 major and minor components in matte(including Cu,S,Fe,SiO2,CaO,Al2O3,Pb,As and Zn) by X-ray fluorescence spectrometry(XRF) with fusion sample preparation was established.Anhydrous Li2B4O7-LiBO2 (m∶m=12∶22) was selected as the mixed flux for sample fusion.NaNO3 was used as oxidant and LiBr was used as release agent.A fully automatic electric heating sample fusion machine integrating pre-oxidation and fusion functions was used to prepare the fusion beads,which improved the safety and efficiency of sample preparation.The optimal experimental conditions were determined as follows:the mass ratio of sample to NaNO3 was 1∶2,and the dilution ratio of mixed flux to sample was 20∶1.Fusion sample preparation could significantly reduce the X-ray fluorescence counting rate and avoid intensity overload.The calibration samples were prepared by manually mixing actual matte sample,reference material and primary standard substance.After calibrating the values by standard methods,the calibration curves were drawn.The matrix effect and spectral line interference were corrected by combining theoretical α coefficient method with empirical coefficient method in this method.Except for major components including Cu,S and Fe,the limits of detection of other components were in range of 0.004%-0.017%.The precision test of was conducted,and the relative standard deviations(RSD,n=11) of determination results of each component in matte sample were between 0.04% and 2.4%.Meanwhile,3 matte production control samples were analyzed according to the experimental method,and the relative errors between the measured results and the reference values ranged from -1.88% to 4.00%.
  • Determination of 16 major and minor components in soil and stream sediment by X-ray fluorescence spectrometry with fusion sample preparation
    REN Nan, WANG Xuewei, CHEN Na
    Metallurgical Analysis. 2025, 45(9): 81-88. https://doi.org/10.13228/j.boyuan.issn1000-7571.012893
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    The quantitative analytical method for 16 major and minor components(SiO2,Al2O3,Fe2O3,CaO,MgO,K2O,Na2O,Ti,P,Mn,Cr,Cu,Ba,Sr,Zn and Zr) in soil and stream sediment by wavelength dispersive X-ray fluorescence spectrometry(WDXRF) with fusion sample preparation was established in this study.The fusion sample preparation parameters were optimized:the ratio of flux to sample was 1∶10;the ignition temperature was 600 ℃;the fusion temperature was 1 050 ℃;0.5 mL of LiBr solution was used as release agent.The fused beads with good surface flatness and optical homogeneity were prepared,which effectively eliminating the influence of matrix effect and particle size effect on the analytical results.In experiments,the calibration curves were drawn using the certified reference materials soil and stream sediment as well as the calibration samples prepared.The calibration curve ranges covered the high content components such as SiO2(12%-75%),Al2O3(3%-28%) and Fe2O3(2%-15%).The matrix effect was corrected by theoretical α coefficient method,empirical coefficient method and Compton scattering internal standard method.The experimental results showed that the limits of detection were in range of 1-20 μg/g excepted for major components.The accuracy test was conducted using the certified reference materials soil(GBW07980) and stream sediment(GBW07360).The relative standard deviations(RSD,n=6) of determination results of 16 components were less than 5%,and the absolute value of relative errors(RE) were controlled within 5%.Compared to the traditional chemical analysis methods,the proposed method exhibited significant advantages such as short analytical cycle (less than 3 h per sample),strong adaptability to matrix and environmental friendliness(avoiding strong acid digestion).It could provide technical support for efficient analysis of regional geochemical surveys and soil pollution surveys.
  • Determination of 14 components in iron-bearing dust and sludge by X-ray fluorescence spectrometry with secondary oxidation fusion sample preparation
    DENG Junhua, XU Qiang, HU Zhongxin, KANG Dehua, YANG Jie
    Metallurgical Analysis. 2025, 45(9): 89-95. https://doi.org/10.13228/j.boyuan.issn1000-7571.012815
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    As a typical solid waste generated from dust removal process in iron and steel metallurgy,the iron-bearing dust and sludge faces challenges in resource utilization due to its compositional complexity and the scarcity of reference materials.To address the problems of inefficiency and severe matrix interference of traditional wet chemical analysis method,a composite flux system (m(Li2B4O7)∶m(LiBO2)=67∶33) incorporating secondary low-temperature pre-treatment oxidation was developed in this study.The fusion sample preparation was conducted at 1 050 ℃ with dilution ratio of 12.5∶1.The synthetic calibration sample system was established based on gradient-mixed reference material iron ore,iron concentrate and primary standard substance,which successfully met the broad-range calibration requirements of 14 components such as TFe (1.20%-69.5%), SiO2 (1.00%-48.50%),and Zn (0.10%-10.76%).The influence caused by mass difference were eliminated via fused bead mass correction,and the spectral interferences among components were corrected using the empirical coefficient method TL(Traill-Lachance) model.Under the optimized experimental parameters,a method for determination of 14 components in iron-bearing dust and sludge(including TFe,SiO2,CaO,MgO,Al2O3,MnO,P,TiO2,Cr,Ni,V2O5,Zn,Co and K2O) by X-ray fluorescence spectrometry(XRF) was established.Wherein TFe,SiO2,CaO,MgO,Al2O3 and MnO were analyzed using fixed channels.The experimental results demonstrated that the linear correlation coefficients of all calibration curves were not less than 0.999 3.The relative standard deviations(RSD,n=8) of determination results were between 0.14% and 3.8%.The proposed method was compared with other methods using the certified reference materials. Method comparison tests were conducted on reference material iron-bearing dust and sludge and actural sample,the results showed that measured values were consistent with standard values and those obtained by other methods.The detection accuracy of TFe was comparable to that of the conventional cobalt internal standard method.The proposed method was applied for the analysis of iron-bearing dust and sludge waste solid,realizing the accurate determination of multi-components. It provided reliable technical support for the high-value utilization of metallurgical solid wastes and met the detection demands of routine scientific research.
  • Determination of silver and copper in silver-copper based brazing filler metal by X-ray fluorescence spectrometry
    WANG Zhanming, XU Junhui, FAN Min, WANG Lisha
    Metallurgical Analysis. 2025, 45(9): 96-101. https://doi.org/10.13228/j.boyuan.issn1000-7571.012866
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    During the determination of silver and copper content in silver-copper based brazing filler metal by traditional silver chloride precipitation-flame atomic absorption spectrometry(FAAS),the operation is cumbersome and time-consuming.In this study,the silver-copper based brazing filler metal sample was dissolved with nitric acid,and the content of silver and copper in solution was determined by X-ray fluorescence spectrometry(XRF).The influence of nitric acid concentration in sample solution on the determination results of silver and copper was explored in experiments.The interference of acid was eliminated by removing acid and steaming dry.The effect of solution volume on the determination results of silver and copper was also discussed,and 10 mL was selected as the optimal measurement volume.The spectral lines were examined,and AgKα and CuKα was selected as the analytical line for silver and copper,respectively.Cu 200 μm was selected as the AgKα spectral line filter,and 0.46° collimator was used for the measurement of CuKα spectral line.The correlation coefficients of calibration curves for silver and copper were both higher than 0.999 9.The proposed method was applied for the determination of silver and copper in silver-copper based brazing filler metal sample, and the relative standard deviation (RSD, n=6) of determination results was 0.16% and 0.21%, respectively. The content of silver and copper in simulation sample of silver-copper based brazing filler metal was determined according to the experimental method.The absolute value of relative error(RE) of measurement results was not more than 0.5%.The recoveries of silver and copper were 99.5%-100.3% and 99.5%-100.5%,respectively.The proposed method solved the problem of no solid referende materials,and it could effectively meet the demands of chemical composition analysis of silver-copper based brazing filler metal in welding processes.
  • Determination of molybdenum in uranium-molybdenum alloy by X-ray fluorescence spectrometry with binary ratio method
    YANG Yongming, YUAN Cuihong, HAN Shuzhen, ZHANG Qingming
    Metallurgical Analysis. 2025, 45(9): 102-107. https://doi.org/10.13228/j.boyuan.issn1000-7571.012833
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    Uranium-molybdenum(U-Mo) alloy is a kind of novel metal nuclear fuel,wherein the technical requirements for Mo content become more and more strict.The surface roughness of U-Mo alloy samples after grinding by metallographic sand paper with different specifications was investigated.It was found that the surface roughness of sample was below 2 μm when the specification of sand paper was not less than P400,which had no influence on the determination of Mo by X-ray fluorescence spectrometry(XRF).The sample was processed to $\phi$25 mm×5 mm specimens.The X-ray fluorescence intensity of Mo on upper and lower surfaces was basically consistent.The F test and t test results proved that there was no significant difference between two groups of data.The uniformity of sample was good and it could be used for direct determination by XRF.In addition,it was found that the surface oxidation extent of U-Mo alloy increased with increasing time,leading to the decrease of X-ray fluorescence intensity of both U and Mo.However,the ratio of the intensity of U to Mo was basically stable.Therefore,the calibration curves were drawn by binary ratio method using the self-prepared U-Mo alloy quality control samples.U-Lα and Mo-Kβ were selected as the analytical line to eliminate the influence of surface oxidation of U-Mo alloy on the determination of Mo.One U-Mo alloy quality control sample and one production sample were used for precision test.The relative standard deviations(RSD, n=6) of determination results were not more than 0.15%.The same U-Mo alloy sample was determined by XRF and inductively coupled plasma atomic emission spectrometry(ICP-AES).The comparison indicated that the determination of solid sample by XRF exhibited better precision.Moreover,the confidence interval of determination results was narrower at 95% confidence,which was more suitable for the detection of U-Mo alloy samples with strict technical requirements.
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