28 July 2026, Volume 46 Issue 7
    

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  • Research progress on elemental content analysis of uranium-based nuclear fuel pellet
    DENG Chuandong, HUANG Xiaokang, SU Lei, ZHANG Dongping, TANG Yan ZHAO Feng, SUN Yongduo, LIAO Zhihai, WU Xiaoyong
    Metallurgical Analysis. 2026, 46(7): 1-12. https://doi.org/10.13228/j.boyuan.issn1000-7571.013077
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Accurate and rapid analysis of element content in uranium-based nuclear fuel pellet is crucial for the quality control of nuclear fuel.In this paper,the analysis methods for major metals,micro-trace metals and non-metallic impurity elements in uranium-based nuclear fuel pellet in recent years are reviewed from 3 aspects,including sample pretreatment,matrix separation and composition determination.The sample pretreatment methods mainly include acid dissolution,microwave digestion and direct pressed pellet.The matrix separation methods mainly include levextraction,extraction separation,liquid-solid phase separation method and high-temperature hydrolysis(PH).The composition determination methods mainly include titration,X-ray fluorescence spectrometry(XRF),inductively coupled plasma optical emission spectrometry(ICP-OES/AES),inductively coupled plasma mass spectrometry(ICP-MS),pulse melting thermal conductivity method,ion chromatography,oxidative combustion method,spectrophotometry and ion selective electrode method,etc.In tests,appropriate independent or combined analytical technologies can be selected according to the analysis requirements of different types of nuclear fuel pellets.Furthermore,the future development of elemental content analysis for uranium-based nuclear fuel pellets is prospected.
  • In-situ quantitative statistical distribution analysis of composition for spray-formed 2195 aluminum-lithium alloy ingot
    WU Dongxiao, LI Dongling, WANG Peng, YANG Jingwei, SONG Yifan, SHI Huachao
    Metallurgical Analysis. 2026, 46(7): 13-22. https://doi.org/10.13228/j.boyuan.issn1000-7571.013049
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    The chemical composition and process design of aluminum-lithium(Al-Li) alloy directly affect their microstructural distribution and overall service performance.The spray-formed aluminum alloy employs a relatively advanced smelting process,but the settings of its process parameters can significantly affect the composition distribution of the ingot.Consequently,the quantitative characterization of chemical composition distribution for spray-formed Al-Li alloy is of great significance for guiding the smelting processes.In this study,an in-situ quantitative statistical distribution characterization method for the composition of spray-formed 2195 Al-Li alloy was established based on microbeam X-ray fluorescence spectrometry(μ-XRF).Nondestructive in-situ quantitative distribution characterization was conducted for 5 major elements in 2195 Al-Li alloy,including Cu,Fe,Mg,Zr and Ag.The distribution regularity of each element from the core to the edge of ingot was systematically investigated.The results indicated that Cu exhibited obvious enrichment at the edge,followed by a secondary enrichment in the core region,while spot segregation was observed for both Fe and Mg.Continuous fixed-point analysis via spark discharge optical emission spectrometry(Spark-OES) further verified that the contents of Cu at the edge and core of the ingot were higher than that at the r/4 region (where r denotes the ingot radius),which was consistent with the quantitative distribution results obtained by μ-XRF.Scanning electron microscopy and energy dispersive spectroscopy(SEM/EDS) were also employed for the characterization of microstructures at different regions of ingot.Copper-rich phases were identified,which further clarified the formation mechanism of elemental segregation in the ingot.The in-situ quantitative statistical distribution analysis method based on μ-XRF had important significance for the detailed inspection and quality evaluation of spray-formed processes,and it was crucial for exploring and revealing the correlation among composition,microstructure and properties of spray-formed Al-Li alloy.
  • Research progress on intelligent metallographic analysis based on machine learning
    WANG Xiaoyong, ZHANG Jianing, SUN Chenxi, ZHANG Yanting, QI Zheng
    Metallurgical Analysis. 2026, 46(7): 23-30. https://doi.org/10.13228/j.boyuan.issn1000-7571.013109
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    This article systematically reviews the research progress and application status of machine learning in the field of metallographic analysis.It emphatically analyzes the technological breakthroughs of machine learning in key links,including grain size rating,microstructure identification,non-metallic inclusion analysis,case depth detection and intergranular corrosion assessment.Meanwhile,the existing issues are pointed out,such as uneven data quality,insufficient algorithm applicability and poor model interpretability.Combined with the development of artificial intelligence(AI) technology,future development directions are prospected,including the construction of standardized databases,the development of multimodal learning frameworks and the improvement of model interpretability.This study aims to promote the evolution of metallographic analysis towards intelligence and standardization,and provide stronger technical support for material research and quality control.
  • Determination of 10 major components in high-manganese iron ore by X-ray fluorescence spectrometry with fusion sample preparation
    YANG Xiaoli, LI Xiaodan, SHAO Xin, LU Shansong, QIU Xiaofei YANG Xiaoli, GUO Yuepin, ZENG Guanghua
    Metallurgical Analysis. 2026, 46(7): 31-39. https://doi.org/10.13228/j.boyuan.issn1000-7571.013056
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    When X-ray fluorescence spectrometry(XRF) is applied to the analysis of high-manganese iron ore,the abnormal manganese content(w(MnO)>2%) will cause negative deviation in Fe2O3 determination results.In addition,the conventional fusion preparation with a dilution ratio of 10∶1 easily leads to cracking of fused bead and poor molding difficulty.To address these issues,the calibration method,sample preparation conditions and interference correction were systematically optimized in this study.Firstly,a series of gradient calibration samples were prepared by proportionally mixing national first-grade certified reference materials of manganese ore and iron ore,which expanded the linear determination ranges for MnO and Fe2O3,and filled the calibration blank for high-manganese(w(MnO)>0.5%) and high-iron(w(Fe2O3)>30%) content intervals.Secondly,by optimizing the fusion preparation conditions such as dilution ratio,fusion temperature and time,the optimal fusion procedure was determined:a dilution ratio of 14∶1,addition of LiBr solution and NH4I solution as release agents,and fusion at 1 050 ℃ for 10 min.This procedure significantly improved the preparation quality and success rate of fused bead.Finally,the combination of theoretical α coefficient method and empirical coefficient method was adopted to correct the matrix effect.The overlapping interference of Mn Kβ spectral line on Fe Kβ spectral line was deducted,which effectively eliminated the distortion of Fe2O3 measurement results caused by high-manganese under high-iron background.The proposed method was used to determine 10 major components in high-manganese iron ore sample,including SiO2,Al2O3,Fe2O3,CaO,MgO,K2O,Na2O,TiO2,P2O5 and MnO.The relative standard deviations (RSD,n=6) of the results ranged from 0.29% to 8.3%.The RSD for the low-content Na2O component was relatively high,but all determination results could meet the requirements of DZ/T 0130-2006 The Specification of Testing Quality Management for Geological Laboratories.The trueness was further verified using reference materials iron ore.The determined values of each component were in good agreement with the standard values,and the relative errors could meet the specification requirements.Additionally,two high-iron high-manganese iron ore samples from a mining area were analyzed,and the results were compared with those obtained by national standard methods(gravimetry for SiO2;titrimetry for Al2O3,CaO,and MgO;spectrophotometry for Fe2O3,TiO2,and P2O5;atomic absorption spectrometry for Na2O,K2O,and MnO).The results showed good consistency between the two methods,and all errors conformed to the allowable range specified in DZG 93-07 Analytical Procedures for Iron Ores.The XRF analysis method for high-manganese iron ores established in this study successfully overcame the challenges of high-manganese matrix interference and sample preparation difficulties,and it was suitable for the analysis of actual samples.
  • Determination of gallium,vanadium and phosphorus in coal and gangue by inductively coupled plasma atomic emission spectrometry with acid dissolution oxidation
    ZHU Zhigang, LI Meili, WANG Zhengqi, LI Chao, A Lamusi, LI Guoxin
    Metallurgical Analysis. 2026, 46(7): 40-47. https://doi.org/10.13228/j.boyuan.issn1000-7571.013033
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    Accurate determination of gallium(Ga),vanadium(V) and phosphorus(P) contents in coal and gangue is of great significance for the resource utilization of associated elements,coal quality evaluation and environmental pollution assessment.Current national standard methods(GB/T 8208-2007,GB/T 19226-2003 and GB/T 216-2003) require high temperature ashing of samples at different temperatures,followed by separate determination of Ga,V and P via spectrophotometry.Such procedures are relatively cumbersome,and high temperature treatment easily causes volatile loss of partial elements,making simultaneous pretreatment and multi-element determination unavailable.In this study,based on the strong oxidation of HNO3,H2SO4,and H2O2,the organic matters in samples were oxidized and removed in the form of CO2,which effectively eliminated the adsorption and encapsulation of Ga,V and P by carbon-containing substances and avoided the carbon removal process by high temperature ignition.Furthermore,HF was introduced to form a mixed acid system together with HNO3 and H2SO4,which greatly improved the decomposition efficiency of silicon-bearing minerals.On this basis,a method for the simultaneous determination of Ga,V and P in coal and gangue sample by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established.The correlation coefficients(r) of calibration curves for all elements were 1.000 0.The limits of detection(LOD) of Ga,V and P ranged from 0.29 μg/g to 2.43 μg/g,and the limits of quantification(LOQ) were between 1.2 μg/g and 9.7 μg/g.The contents of Ga,V and P in coal and gangue were determined according to the experimental method,and the relative standard deviations(RSD,n=7) of the determination results were between 1.7% and 9.4%.The method comparison results indicated that there was no significant difference between the proposed method and national standard methods via t-test, demonstrating the accuracy and reliability of the established method.
  • Determination of micro additive in high-salinity nickel electrowinning electrolyte by high performance liquid chromatography with solid phase extraction
    LI Ruiji, ZHANG Fengrui, JIN Yan, WEI Hongsheng, LI Yijing TANG Qinghai, GUO Yong
    Metallurgical Analysis. 2026, 46(7): 48-53. https://doi.org/10.13228/j.boyuan.issn1000-7571.013048
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    A combined analytical method based on solid phase extraction and high performance liquid chromatography(SPE-HPLC) was established for the quantitative determination of micro additive in nickel electrowinning eletrolyte,including sodium salicylate(SS) and 2,5-dimethyl-3-hexyne-2,5-diol(HD-M).Through systematic optimization of pretreatment conditions,the hydrophilic-lipophilic balanced(HLB) solid phase extraction column was selected for enrichment and purification.The optimal sample loading volumes for SS and HD-M were 100 mL and 80 mL,respectively.The solution of formic acid-acetonitrile mixture (V∶V=8∶2) and methanol-water (V∶V=8∶2) was used as eluents.C18 chromatographic column coupled with ultraviolet detector was adopted for chromatographic analysis,achieving the effective separation and detection of two additives.Under optimized conditions,SS and HD-M exhibited good linear relationships within the ranges of 0.1-10 μg/mL and 0.2-10 μg/mL,respectively.The developed method presented high sensitivity.The limits of detection(LOD) for SS and HD-M were 0.03 μg/mL and 0.06 μg/mL,and the limits of quantification(LOQ) were 0.1 μg/mL and 0.2 μg/mL,respectively.The precision and standard addition recovery tests showed that the relative standard deviations(RSD,n=5) of SS and HD-M were 3.0%-6.1%,and the recoveries ranged from 83.36% to 95.35%.The proposed method was applied to the sample analysis in nickel electrowinning workshops.Both SS and HD-M were stably detected in catholyte(circulation port and diaphragm bag),but not detected in anolyte,which was consistent with the practical process expectation.This method could effectively eliminate the interference of high-salinity matrix and was suitable for real-time monitoring of additive concentrations during nickel electrowinning production.It provided a reliable analytical basis for process parameter optimization and product quality assurance.
  • Determination of low content cerium in high thermal conductivity and high strength magnesium alloy profile for lightweight automotive radiator by inductively coupled plasma atomic emission spectrometry
    XING Shudong, GAO Xiuhong, WANG Binqi, PENG Wei, ZHAO Jianfeng
    Metallurgical Analysis. 2026, 46(7): 54-59. https://doi.org/10.13228/j.boyuan.issn1000-7571.013060
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Cerium is a critical rare earth element for improving the comprehensive properties of high thermal conductivity and high strength magnesium alloy applied in lightweight automotive radiators.However,due to the large size and irregular shape of such structural components,the conventional analytical methods are difficult to realize the rapid and accurate determination of low content cerium.In this study,an analytical method based on inductively coupled plasma atomic emission spectrometry(ICP-AES) was established.The homogeneity of samples was verified by F-test.The sample was dissolved with 25 mL of hydrochloric acid(1+1),and the matrix matching method was adopted to eliminate the influence of matrix effect.Under the analytical spectral line of Ce 404.076 nm,cerium showed a good linear relationship in the range of 1.00-12.00 μg/mL,with a linear correlation coefficient(r) of 0.999 9.The limit of detection was 0.000 34%.The proposed method was applied for the determination of cerium in certified reference materials magnesium alloy,and the relative errors(RE) ranged from -0.89% to 3.16%.The content of cerium in high thermal conductivity and high strength magnesium alloy profile sample for lightweight automotive radiator was determined according to the experimental method.The relative standard deviations(RSD,n=6) were between 0.44% and 1.7%,and the recoveries were between 92.5% and 102.3%.This method was suitable for the accurate determination of low content cerium in magnesium alloy profile for radiators,and it provided a reliable analytical technique for material performance evaluation.
  • Determination of available phosphorus in neutral and alkaline soils by molybdenum-antimony-ascorbic acid spectrophotometry with ultrasonic extraction and centrifugal separation
    HAN Rui, CHEN Yajie, WANG Juan, FENG Lanhui, SHAN Weiyao SHI Lijuan, SUN Jia, ZHANG Lulu
    Metallurgical Analysis. 2026, 46(7): 60-66. https://doi.org/10.13228/j.boyuan.issn1000-7571.012930
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    To meet the high-throughput detection demand for available phosphorus in neutral and alkaline soils,a combined detection system integrating ultrasonic extraction,centrifugal separation and molybdenum-antimony-ascorbic acid spectrophotometry was established in this study.The key parameters including extractant concentration,ultrasonic extraction temperature,ultrasonic extraction duration and centrifugal separation time were optimized to determine the optimal extraction conditions.Based on the molybdenum-antimony-ascorbic acid chromogenic principle,the calibration curve was established at a wavelength of 880 nm.The linear correlation coefficient of the calibration curve was 0.999 8,and the apparent molar absorptivity was 1.75×104 L·mol-1·cm-1.The limit of detection(LOD) and limit of quantification(LOQ) of the method were 0.34 mg/kg and 1.36 mg/kg,respectively.The proposed method was applied for the determination of 4 certified reference materials(CRMs) for available nutrient analysis of soil available phosphorus.The relative standard deviations(RSD,n=6) of determination results ranged from 2.5% to 8.5%.The average values all fell within the uncertainty ranges of certified values,with relative errors(RE) of -4.61%-1.33%.The contents of available phosphorus in two typical soil samples from the Third National Soil Survey were determined according to the experimental method,and the recoveries were between 92% and 105%.Moreover,the available phosphorus contents in typical soil samples from the Third National Soil Survey were determined by the proposed method and the agricultural industry standard NY/T 1121.7-2014(the oscillation extraction is adopted for sample pretreatment),and the results of two methods were consistent.Compared with the standard method,this system presented significantly improved extraction efficiency,which provided efficient technical support for large-scale testing tasks such as national soil surveys.
  • Determination of low content of iron oxide in steelmaking promoter by inductively coupled plasma atomic emission spectrometry
    YANG Dongqi, WANG Zhaorui, XU Liang, YAN Sha, FENG Wenyan ZHU Jinbo, LI Yue, LI Tao
    Metallurgical Analysis. 2026, 46(7): 67-72. https://doi.org/10.13228/j.boyuan.issn1000-7571.013053
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    In view of the mismatch between the detection standard and product specification range for iron oxide in steelmaking promoter,as well as the deficiencies of current testing methods,an analytical method for the determination of low content of iron oxide (w≤5%) in steelmaking promoter by inductively coupled plasma atomic emission spectrometry(ICP-AES) was established.The sample was dissolved with hydrochloric acid by heating followed by filtration.The residue was ashed and subsequently fused with sodium carbonate-boric acid mixed flux (m∶m=2∶1).The melt was leached with hydrochloric acid,combined with the original filtrate,diluted to a constant volume,and then determined by instrumental analysis.The key conditions including sample digestion method and matrix interference were systematically investigated.The results showed that the combined acid dissolution and alkali fusion method achieved the best digestion effect for steelmaking promoter samples.The aluminum matrix had interference with the determination of iron oxide.The matrix matching method was adopted to prepare the calibration curve to eliminate the influence of matrix effect in this study,in other words,the aluminum matrix concentration in the standard solution series was basically consistent with that of the sample solution.The calibration curve exhibited good linearity when the iron oxide content(mass fraction) was in range of 0.01%-5.00%,and the correlation coefficient was 0.999 9.The limit of detection(LOD) was 0.003%.The content of iron oxide in steelmaking promoter samples was determined according to the experimental method.The relative standard deviation(RSD,n=7) was 0.46%-0.70%.The analytical results were in good agreement with those obtained by orthophenanthroline spectrophotometry.The results of F-test indicate that there is no significant difference between the two methods.Spiked recovery tests were performed on steelmaking promoter samples,and the recovery was between 95% and 100%.
  • Revision and evaluation of national standard GB/T 14949.7 for the determination of potassium and sodium in manganese ore
    YE Jinyan, YANG Shujie, ZHONG Junsong, LI Zhanjiang, TIAN Qiong, LIN Hai
    Metallurgical Analysis. 2026, 46(7): 73-78. https://doi.org/10.13228/j.boyuan.issn1000-7571.013044
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    To meet the refined requirements of raw material quality control in the development of manganese ore industry,this paper systematically evaluated and revised the method for the determination of potassium and sodium contents by flame atomic absorption spectrometry(FAAS) specified in the national standard GB/T 14949.7.This revision was developed on the basis of ISO 7969:1985 with joint participation of several laboratories.The revised national standard GB/T 14949.7-2024 mainly involved three key improvements:1)increasing the number of parallel determinations to enhance the precision and reliability of test results;2)clarifying the expression criteria of analytical results to ensure the data accuracy and comparability;3)simplifying and optimizing the preparation procedure of calibration curves to improve the detection efficiency and calibration precision.Multiple rounds of intra-laboratory validation confirmed that GB/T 14949.7-2024 provided accurate determination results and satisfactory precision for manganese ore samples with different content levels.
  • Determination of 11 components in high-chromium iron ore by X-ray fluorescence spectrometry with fusion sample preparation
    FENG Lili, ZHANG Yuesheng, HUANG Honghua, DANG Jiachen, GUAN Song
    Metallurgical Analysis. 2026, 46(7): 79-84. https://doi.org/10.13228/j.boyuan.issn1000-7571.013042
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    To address the difficulties in fusing chromium and the simultaneous accurate determination of sodium,phosphorus and other elements in high-chromium iron ore,a calibration series was established by combining various certified reference materials(CRM/RM) including high-chromium nickel iron ore,iron ore,chromite,lateritic nickel ore and nickel ore through mixed preparation.On this basis,the simultaneous determination of 11 components(sodium oxide,magnesium oxide,aluminum oxide,silicon dioxide,phosphorus pentoxide,potassium oxide,calcium oxide,titanium dioxide,chromium sesquioxide,manganese oxide and nickel oxide) in high-chromium iron ore by X-ray fluorescence spectrometry(XRF) with fusion sample preparation was realized.A mixed flux of lithium tetraborate-lithium metaborate(m∶m=12∶22) was adopted with a sample-to-flux dilution ratio of 1∶15.Ammonium iodide and lithium bromide solution was used as releasing agent.Uniform and transparent glass fused beads were obtained after fusion at 1 100 ℃ for 15 min.The built-in SPECTRAPLUS software was applied for matrix correction using theoretical α coefficient,which effectively eliminated the influence of matrix effect.The contents of 11 components in high-chromium iron ore were determined according to the experimental method,and the relative standard deviations(RSD,n=12) of determination results ranged from 0.10% to 4.8%.The t-test indicated that there was no significant difference between the results obtained by this method and those by traditional chemical methods.The measured values of three CRMs of high-chromium nickel iron ore and two synthetic samples prepared from CRM/RM were consistent with the certified or reference values.The proposed method was suitable for the comprehensive composition analysis of high-chromium iron ore.
  • Improvement of method for the determination of organic matter in electrolytic manganese residue by titration with potassium dichromate oxidation
    LI Zixin, YANG Binghong, ZOU Lang, XU Bin, WANG Chaowu, LIU Hui
    Metallurgical Analysis. 2026, 46(7): 85-92. https://doi.org/10.13228/j.boyuan.issn1000-7571.013029
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    Electrolytic manganese residue is the major solid waste generated in the electrolytic manganese industry,and its organic matter content is a critical parameter for environmental risk assessment and resource utilization potential evaluation.Aiming at the challenges encountered when potassium dichromate oxidation-titration is directly adopted for organic matter determination in electrolytic manganese residue,an improved analytical method suitable for electrolytic manganese residue samples was established through methodological modification and conditional optimization in this study.The interference behavior of Mn(Ⅱ) was emphatically investigated,and its allowable threshold was clarified.The experimental results indicated that Mn(Ⅱ) had no significant interference on the determination results when its mass fraction was lower than 5%.A self-assembled condensation reflux device was applied to effectively inhibit reagent volatilization in digestion process,thereby greatly improving the titration precision.After systematic optimization,the optimal reaction conditions were obtained as follows:reaction for 3.5 min from boiling in an oil bath at 170-190 ℃.The contents of organic matter in 5 electrolytic manganese residue samples were determined according to the experimental method.The relative standard deviations(RSD,n=11) of determination results were between 0.31% and 4.3%,and the recoveries ranged from 98.0% to 100.6%.The proposed method filled the gap in dedicated testing standards for organic matter in electrolytic manganese residue,and it provided reliable technical support for environmental compliance evaluation and safe resource utilization of electrolytic manganese residue.
  • Determination of nickel in lithium nickel cobalt manganese oxide by dimethylglyoxime gravimetry and zinc chloride back titration
    ZHANG Chuang, CHEN Xiongfei, GAO Lin, XU Qing, ZHANG Jing, XIAO Nana
    Metallurgical Analysis. 2026, 46(7): 93-99. https://doi.org/10.13228/j.boyuan.issn1000-7571.013028
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    Lithium nickel cobalt manganese oxide is a critical cathode material for new energy vehicles and consumer electronic products,in which the nickel content directly affects its electrochemical performance.The key conditions including precipitation pH,reagent dosage,aging temperature and time were systematically optimized in this study.Two chemical analytical methods for the determination of nickel(mass fraction:25.00%-55.00%) in lithium nickel cobalt manganese oxide were established,i.e.,the dimethylglyoxime gravimetry and the dimethylglyoxime precipitation separation-EDTA complexation-zinc chloride back titration.The optimal experimental conditions were confirmed as follows:the pH of solution for precipitation was 8.0-9.0;the dosage of both tartaric acid solution and ammonium acetate solution was 10 mL;the dosage of dimethylglyoxime ethanol solution for gravimetry and back titration was 50 mL and 30 mL,respectively;the precipitation aging temperature was 60-70 ℃,the aging time was 60 min,and 6 washing cycles were adopted;the dosage of acetic acid-sodium acetate buffer solution was 10 mL in back titration,and the pH of solution for titration was controlled at 5.0-6.0.The precision tests showed that the relative standard deviations(RSD,n=11) of the two methods for samples were 0.088% and 0.12%,respectively,indicating excellent repeatability. Statistical analysis was carried out on the consistency of nickel determination results for the same NCM622 lithium nickel cobalt manganese oxide sample using two methods,and the t-test showed no significant difference between the two methods.The certified reference material of GSB 04-3990-2022 was used for validation.It was found that the measured values of both methods fell within the standard value and uncertainty ranges,which further confirmed the reliability of proposed method.This method was suitable for the accurate determination of high content nickel in lithium nickel cobalt manganese oxide.
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