28 October 2026, Volume 46 Issue 10
    

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  • Miao Lede, Zhang Yi, Chen Min
    Metallurgical Analysis. 2026, 46(10): 1-8. https://doi.org/10.13228/j.boyuan.issn1000-7571.013132
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    The precipitation strengthening of 9Cr1Mo heat-resistant steel is mainly attributed to the M23C6 and M2X phases.In addition,a Mo-rich intermetallic Laves phase can form during high-temperature aging and creep processes.The effect of Laves phase precipitation on creep resistance remains debatable,while the particle size and distribution of precipitated phases also significantly affect the creep resistance and impact toughness of the steel.To investigate the evolution behavior of precipitated phases in 9Cr1Mo heat resistant steel under different creep durations,the structure,morphology,and size of the precipitated phases were characterized by laser particle size analyzer,scanning electron microscope (SEM),and transmission electron microscope (TEM) in this study.Furthermore,X-ray diffraction (XRD) coupled with the Rietveld full-spectrum fitting method was employed for qualitative and quantitative analysis to discuss the influence of creep duration on precipitates and their correlation with high-temperature service failure.The results showed that three types of precipitated phases,namely M23C6,M2X,and Laves phase,were present in 9Cr1Mo steel after high-temperature creep.The precipitated phases in the tempered specimens were dominated by M23C6 and M2X.At 600 ℃,the specimens fractured at 52 h and 242 h under constant stresses of 108 MPa and 93 MPa,respectively,and the types of precipitated phases remained essentially unchanged.When the constant stress was reduced to 79 MPa,the Laves phase began to appear at fracture after 1 990 h of creep.With decreasing stress and extending creep time,the mass fraction of the Laves phase increased from 0.20% at 1 990 h to 0.64% at 10 060 h.
  • Shi Zhixin, Luo Huihua, Liu Liwei, Li Hongqiang, Gao Jian
    Metallurgical Analysis. 2026, 46(10): 9-18. https://doi.org/10.13228/j.boyuan.issn1000-7571.013102
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    To clarify the evolution of V-bearing phases and the migration behavior of V during the self-activated roasting of low-calcium vanadium slag,X-ray diffraction (XRD),scanning electron microscope (SEM),and electron probe micro-analyzer (EPMA),along with other characterization techniques,were employed to investigate the roasting reaction behaviors of vanadium-iron spinel with five additives (TiO2,SiO2,CaO,MgO,and MnO),as well as the solid-solution behavior of V in different valence states within the Ti-Fe-O system.The results showed that oxidative decomposition of vanadium iron spinel occurred during roasting with TiO2 and SiO2,respectively.TiO2 reacted with the decomposition products to form a V-containing Fe2TiO5 solid solution,which was hardly leached by sulfuric acid.In contrast,SiO2 did not react with the decomposition products.When vanadium-iron spinel was roasted with MgO,CaO,and MnO,respectively,acid-soluble phases,namely Mg2V2O7,CaV2O6,Ca2V2O7,and Mn2V2O7,were formed by reacting with the decomposition products.V did not form a solid solution in the decomposition product Fe2O3.When V in different valence states entered the Ti-Fe-O system,V(Ⅲ) dissolved more readily in the Fe2TiO5 phase than V(Ⅳ).V(Ⅴ) could not form a solid solution with Fe2TiO5,but reacted with it to form FeVO4.This study systematically elucidates the phase-formation mechanism between vanadium-iron spinel and the main slag components in the self-activated roasting system of vanadium slag,providing a theoretical basis for the process and helping to improve the resource utilization efficiency of vanadium slag.
  • Sun Fangfang, Li Yanxiang, Li Baoyu, Zhang Di, Lin Peijun
    Metallurgical Analysis. 2026, 46(10): 19-26. https://doi.org/10.13228/j.boyuan.issn1000-7571.013127
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    The determination of phosphorus and sulfur in geochemical samples is of great significance for the research of diagenetic and mineralization processes,ecological environment as well as soil fertility.The main challenges lie in the accurate determination of low-content samples and the effective elimination of complex matrix interferences.In this study,an analytical method was established for the simultaneous determination of phosphorus and sulfur in regional geochemical samples (soils,stream sediments and rocks) by inductively coupled plasma tandem mass spectrometry (ICP-MS/MS).The sample was subjected to open-vessel digestion with a mixed four-acid system of nitric acid,hydrochloric acid,hydrofluoric acid,and perchloric acid.Then oxygen was introduced into the collision/reaction cell (OCR),where 31P+ and 32S+ were converted into 31P16O+ and 32S16O+.The mass-shift mode was adopted for measurement,which effectively eliminated polyatomic ion interferences originating from complex matrices.The calibration curves of phosphorus and sulfur exhibited good linearity within the range of 1.00-1 000 μg/L,and the correlation coefficients were both higher than 0.999.The limits of detection for method were 0.60 μg/g for phosphorus and 1.76 μg/g for sulfur,respectively.Multiple national primary geochemical reference materials were determined,and the results were in good agreement with the certified values.The relative standard deviations (RSD,n=6) were 1.0%-2.0% for phosphorus and 1.8%-4.2% for sulfur.Compared with the results obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS),the proposed method showed remarkable advantages in terms of precision and accuracy.The standard addition method was applied for method validation of low-content phosphorus and sulfur.The spiked recoveries were 82%-86% and 79%-88%,with RSD (n=6) of 4.1%-7.2% and 5.2%-9.4%,respectively.These results demonstrated that the proposed method maintained excellent accuracy and precision even at trace levels close to the detection limit.This method was suitable for the efficient analysis of phosphorus and sulfur in large batches of regional geochemical samples.
  • Ji Yuping, Lin Ding, Yang Tianfu
    Metallurgical Analysis. 2026, 46(10): 27-35. https://doi.org/10.13228/j.boyuan.issn1000-7571.013133
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    Phenolic compounds such as alkylphenols and bisphenols are mostly toxic and bioaccumulative,which threaten ecosystem balance and human health.In order to achieve accurate determination of phenolic compounds in soil,an analytical method was established in this study for the simultaneous detection of 23 phenolic compounds (including alkylphenols,bisphenols,nitrophenols and chlorophenols) in soil by pressurized liquid extraction (PLE) combined with acetic anhydride derivatization-gas chromatography-tandem mass spectrometry (GC-MS/MS).The soil samples were extracted by PLE using n-hexane-acetone (1∶1,V/V) as extraction solvent.After concentrating the extract to 1.0 mL,5 mL of isopropanol was added and the solution was transferred into 100 mL of 0.4 mol/L potassium carbonate solution.3.0 mL of triethylamine was used as a catalyst for the derivatization reaction with 2.0 mL of acetic anhydride to form volatile and thermally stable acetate derivatives.After liquid-liquid extraction with dichloromethane,qualitative and quantitative analysis was conducted by GC-MS/MS under multiple reaction monitoring (MRM) mode.Under optimized conditions,the calibration curves of 23 phenolic compounds exhibited good linearity within the range of 10.0-500 μg/L.The correlation coefficients (r) were between 0.999 1 and 0.999 9.The relative standard deviations (RSD) of response factors ranged from 1.87% to 10.2%.The limits of detection (LOD) of this method were 0.18-0.28 μg/kg,and the limits of quantification (LOQ) were 0.72-1.12 μg/kg,respectively.At four spiked levels of 1.00,10.0,20.0 and 50.0 μg/kg,the spiked recoveries of the target 23 compounds were between 75.3% and 113%,and the corresponding RSDs(n=7) were between 2.47% and 11.3%.Forty actual soil samples were analyzed,and all 23 phenolic compounds were detected in varying degrees.The relative deviations of parallel samples were 0.08%-14.3%,and the spiked recoveries were 70.8%-116%.Repeatability tests on two actual samples revealed that the RSD(n=6) was 3.43%-14.0%.The proposed method could meet the detection requirements for 23 phenolic compounds in soil.
  • Wu Shu, Wang Quanhua, Zhu Xi, Luo Xiaoyun, Tang Yong
    Metallurgical Analysis. 2026, 46(10): 36-43. https://doi.org/10.13228/j.boyuan.issn1000-7571.013136
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    The extensive application of high-purity titanium in high-end fields such as aerospace and medical care imposes strict requirements on its purity.However,the traditional detection methods suffer from low efficiency and the risk of introducing foreign impurities,which cannot meet the current analytical demands.Accordingly,an analytical method based on glow discharge mass spectrometry (GDMS) was established for the determination of 23 impurity elements (Li,B,Na,Mg,Al,Si,Cl,K,Ca,V,Cr,Mn,Fe,Ni,Co,Cu,Zn,Zr,Mo,Ag,Sn,W,Pb) in high-purity titanium.Through systematic experiments,the optimal detection isotopes and instrument working parameters (i.e.,discharge current of 2.0 mA,discharge voltage of 980 V,and pre-sputtering time of 20 min) for each element were determined.High-purity titanium sample was used for validation,and it was found that the relative standard deviations (RSD,n=6) of determination results for tested elements were all less than 30% with good repeatability.Except for Na,V,and Zn,the detection results of the other elements were basically consistent with those obtained by inductively coupled plasma mass spectrometry (ICP-MS).Due to the restriction of matrix-matched certified reference materials,the matrix matching correction of relative sensitivity factors (RSF) was only conducted for Al,Sn,Mo,Si,Ni,Cr,Mn,Fe and Cu.After correction,the absolute relative biases of determination results of these elements compared to ICP-MS method were controlled within 30%.The limits of detection of the proposed method reached the level of 10 ng/g or even 1 ng/g for most elements,which could meet the detection requirements of trace impurity elements in 4 N-grade (99.99% purity) and higher-grade high-purity titanium.
  • Quan Xueling, Jin Chuanwei, Zhang Jiming
    Metallurgical Analysis. 2026, 46(10): 44-50. https://doi.org/10.13228/j.boyuan.issn1000-7571.013128
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    An automatic statistical method for precipitated phases in steel was investigated by means of field emission scanning electron microscope (FE-SEM) and energy-dispersive spectroscopy software Feature taking pipeline steel and non-oriented silicon steel as research objects.The key factors including sample preparation,substrate selection and parameter setting for electron microscope measurement were systematically examined.The results showed that the optimal experimental conditions were as follows: the precipitated phases were obtained by a secondary replication technique; carbon substrate was adopted to support carbon film for eliminating background interference; the accelerating voltage was 10 kV,and the current was 5 nA.Under these conditions,the automatic statistics of precipitated phases not less than 10 nm could be realized.Experimental results of X65MS pipeline steel and non-oriented silicon steel demonstrated that the statistical results obtained by FE-SEM were consistent with those of transmission electron microscope(TEM) for small-area statistics,with a difference less than 0.7 counts/μm2.Large-area statistics revealed the inhomogeneous distribution of precipitated phases and a decrease in number per unit area,which could better reflect the actual distribution.A large number of Ti containing precipitates were detected in high-Ti non-oriented silicon steel,whereas no-Ti containing precipitates were observed in low-Ti non-oriented silicon steel.
  • Li Shaowen, Zhang Yanbo, Yue Haofeng, Xie Liyun, Liu Pan
    Metallurgical Analysis. 2026, 46(10): 51-58. https://doi.org/10.13228/j.boyuan.issn1000-7571.013349
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    Standardization of chemical analysis methods for copper and copper alloys has attracted great attention from countries around the world and relevant organizations.China,the United States,the European Union,Japan and the International Organization for Standardization (ISO) have developed a series of corresponding analytical method standards.In this study,the current status of Chinese standards for chemical analysis of copper and copper alloys was systematically reviewed and compared with relevant standards issued by ISO,American Society for Testing and Materials (ASTM),European Committee for Standardization (CEN) and Japanese Industrial Standards Committee (JISC).The advantages and disadvantages of domestic standards were analyzed from multiple dimensions including method applicability and testing requirements.In general,Chinese standards for chemical analysis methods of copper and copper alloys are at an internationally leading level and can basically meet domestic inspection requirements.Nevertheless,there are still some problems and shortcomings in element type coverage,determination range,standard structural optimization and timeliness of adopting international standards.Based on the above analysis,some suggestions for improving the relevant method standard system in China have been proposed.
  • Zhang Xiaoyi, Li Jiyun, Alniyaz Tursun, Zhang Miao, Zhang Chaoqing, Zhang Hang, Yu Lei
    Metallurgical Analysis. 2026, 46(10): 59-66. https://doi.org/10.13228/j.boyuan.issn1000-7571.013355
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    X-ray fluorescence spectrometry (XRF) is one of the core techniques for multi-element analysis of geological samples.Powder pellet sample preparation is widely adopted due to its advantages of high efficiency,low cost,and environmental friendliness.Nevertheless,the conventional low-pressure (200-400 kN) powder pellet preparation suffers from poor adhesion and poor formability of high silicon samples,pellet cracking and powder shedding,as well as significant particle size and mineral effects,which severely restrict analytical performance.High-pressure (600-3 200 kN) powder pellet sample preparation can effectively improve the pellet quality and reduce physical effects by greatly increasing compaction pressure,and it has become an important development direction in the field of XRF sample preparation.In this study,the pressing mechanism and equipment development of high-pressure powder pellet preparation were systematically elaborated.The optimization strategies of key parameters,including pressure,holding time,sample particle size,sample mass and film-coating procedure,as well as their influences on analytical performance,were discussed in detail.On this basis,the research progress and application performance of this technique for various matrices were summarized,including silicate rocks,soils,stream sediments,polymetallic ores,bauxite,marine sediments,cobalt-rich crusts,coal and biological samples.Moreover,the technical indicators such as sensitivity,precision,accuracy and limit of detection were compared and analyzed.At the same time,some innovative derivative technologies such as high-pressure film-coating sample preparation and calibration based on artificial intelligence (genetic algorithm-back propagation (GA-BP) neural network) were introduced.Finally,the future development trends of this technique were prospected in the fields of standardization system construction,intelligent equipment research and development,and combination with ultrafine grinding.
  • Zhou Hao, Peng Yuanlun, He Cuiying, Chen Junbo, Zhao Jiali Shi Weipeng, Lu Xiaoming
    Metallurgical Analysis. 2026, 46(10): 67-72. https://doi.org/10.13228/j.boyuan.issn1000-7571.013226
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    Traditional detection methods for components in molybdenum concentrate are wet chemical methods,which usually require long analysis cycles.In this study,3 mL of HNO3 (w=65%) was used as oxidant to react with MoS2 in 0.300 0 g of molybdenum concentrate powder.Sulfur (S) was oxidized to high valence state so as to prevent corrosion of platinum-gold crucibles and volatilization during fusion.After optimization,the fusion conditions were obtained as follows: mixed flux of Li2B4O7-LiBO2 (m∶m=50∶50),dilution ratio of 26.67∶1,fusion temperature of 1 050 ℃,static fusion for 3 min followed by swinging-rotating fusion for 12 min.And 0.40 mL of 250 g/L LiBr solution was elected as the releasing agent.Homogeneous glass beads were successfully prepared.Accordingly,a method for determination of nine components (including Mo,Al2O3,SiO2,Fe2O3,CaO,Pb,Cu,K2O and S) in molybdenum concentrate by X-ray fluorescence spectrometry (XRF) was established.Calibration samples were prepared and calibration curves were plotted by mixing molybdenum ore with certified reference materials of molybdenum concentrate,or mixing certified reference materials of molybdenum concentrate with pure reagents,which broadened the determination ranges for each component.Spectral overlapping interference of MoLα with SKα could be eliminated by instrumental software correction.The precision tests showed that the relative standard deviations (RSD,n=7) for nine components in molybdenum concentrate ranged from 0.18% to 4.7%.The accuracy tests verified that the measured values of certified reference materials and production samples of molybdenum concentrate by the proposed method were in good agreement with the certified values or those obtained by the wet chemical method.
  • Sun Huiying, Li Xiaohui, Hao Shengtao, Chen Chongke, Sun Ruihai, Sun Jia, Zhang Lulu
    Metallurgical Analysis. 2026, 46(10): 73-78. https://doi.org/10.13228/j.boyuan.issn1000-7571.013078
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    Accurate and efficient determination of ammonia nitrogen content in landfill leachate is of great significance for the treatment of landfill leachate.In this study,the sample was pretreated by flocculation precipitation and then directly determined after pressure filtration with a 0.45 μm microfiltration membrane without predistillation.The sample pH,chromogenic reagent combination and instrumental parameters were optimized.The determination of ammonia nitrogen in landfill leachate by spectrophotometry was achieved using a fully-automatic flow injection analyzer.The results showed that the mass concentration of ammonia nitrogen in the range of 0.005 0-10.0 mg/L exhibited an excellent linear relationship with the signal intensity,with a correlation coefficient of r=0.999 9.The limit of detection of this method was 0.001 mg/L.The CRMs environment were determined according to the experimental method,and two actual samples were analyzed by the method in National Environmental Protection Standard HJ 666-2013 for comparison.The relative errors (RE) of the determination results of certified reference materials (CRMs) and actual samples were between -1.21% and 3.37%.The relative standard deviations (RSD,n=6) of determination results of certified reference materials and actual samples were between 0.81% and 3.7%.The proposed method was suitable for the rapid analysis of ammonia nitrogen in batches of landfill leachate samples.
  • Wei Xin, Men Qianni, Feng Xiaojuan, Sun Sha, Liao Binbin, Xue Yuhao, Wang Xiao
    Metallurgical Analysis. 2026, 46(10): 79-85. https://doi.org/10.13228/j.boyuan.issn1000-7571.013108
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    Chromite is an important strategic mineral resource,and its silicon content directly affects the efficiency of smelting processes and the quality of final products.Aiming at the drawbacks of conventional analytical methods for silicon detection in chromite (e.g.,gravimetric method),including cumbersome operations,time-consuming procedures and high cost,a rapid method for the determination of silicon content (expressed as silicon dioxide) in chromite was established based on microwave digestion-boric acid complexation-inductively coupled plasma atomic emission spectrometry (ICP-AES).The sample was treated by microwave digestion in a closed system with nitric acid hydrochloric acid-hydrofluoric acid mixture.The residual fluoride ions (F-) were complexed with boric acid to prevent the corrosion of quartz sample injection system.The effects of dosages of hydrochloric acid,nitric acid and hydrofluoric acid,as well as digestion temperature,digestion time and boric acid dosage on measurement results were systematically investigated.The optimal pretreatment conditions were determined as follows: 0.200 0 g of sample was treated in 3 mL of hydrochloric acid,1 mL of nitric acid and 2.5 mL of hydrofluoric acid by microwave digestion at 160 ℃ for 25 min to achieve complete dissolution of silicon dioxide.After digestion,10 mL of boric acid solution was added to fully complex the excess F- ions.Si 251.611 nm was selected as the analytical spectral line for silicon.The limit of detection (LOD) of this method was 0.000 092 4% (mass fraction,the same below) for silicon dioxide,and the determination range was 0.25%-25.0%.The proposed method was applied to the determination of silicon dioxide in certified reference materials chromite GBW07819,GBW07820,GBW07821,GBW(E)070134 and GBW(E)070135.The measured values were in good agreement with the certified values,with relative errors (RE) of -0.34%-2.53%.The relative standard deviations (RSD,n=7) of determination results were between 0.42% and 3.1%.The proposed method had the advantages of simple operation and high analytical efficiency,and it provided a reliable new approach for the determination of silicon dioxide in chromite and other similar refractory minerals.
  • Zhu Chunyao, Qin Jian, Zhang Jiming, Xie Yanjia
    Metallurgical Analysis. 2026, 46(10): 86-91. https://doi.org/10.13228/j.boyuan.issn1000-7571.013261
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    The accurate and rapid determination of silicon and boron in iron-silicon-boron (Fe-Si-B) amorphous alloys is crucial for material quality control.Nevertheless,the volatile loss of silicon and boron during acid digestion restricts the combined application of acid-dissolution pretreatment with inductively coupled plasma atomic emission spectrometry (ICP-AES).In this study,a method for the simultaneous determination of high content silicon and boron in Fe-Si-B amorphous alloys by acid-dissolution ICP-AES was established.The sample pretreatment and testing conditions were optimized as follows:0.10 g of sample was weighed,and then 5.0 mL of 20 g/L mannitol solution and 15 mL of nitric acid (1+2) were added sequentially; the solution was heated at low temperature to digest the sample.After complete dissolution,the solution was cooled to room temperature.Then 5.0 mL of hydrofluoric acid was added dropwise with continuous shaking until the white precipitate was completely dissolved,and the remaining hydrofluoric acid was supplemented subsequently.Since boron forms stable complexes with mannitol under acidic conditions,the loss of boron in BF3 is effectively prevented.The solution temperature was controlled below 80 ℃ during hydrofluoric acid addition to avoid silicon volatilization in acid treatment procedures.Si 185.067 nm and B 182.591 nm were selected as the analytical spectral lines for silicon and boron,respectively.The calibration curve was plotted by matrix matching method.The linear correlation coefficients of calibration curves for silicon and boron were both greater than 0.999 8.The limits of detection (LOD) of this method for silicon and boron were 0.012% and 0.000 2% (mass fraction,the same below),and the limits of quantification (LOQ) were 0.040% and 0.000 6%,respectively.The proposed method was applied to the determination of silicon and boron in two Fe-Si-B amorphous alloy samples.The relative standard deviations (RSD,n=6) were 0.53%-0.74% for silicon and 0.71%-0.81% for boron.The determination results were basically consistent with those obtained by national standard methods of GB/T 223.60-2024 and GB/T 223.6-2025.The proposed method is accurate and reliable,and it is suitable for the simultaneous and rapid determination of high content silicon and boron in Fe-Si-B amorphous alloys.
  • Wang Quanhua, Wu Shu, Zhu Xi, Luo Xiaoyun, Tang Yong, Liu Fengjun
    Metallurgical Analysis. 2026, 46(10): 92-98. https://doi.org/10.13228/j.boyuan.issn1000-7571.013120
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    Lead-bismuth alloy is widely employed as a coolant material in fourth-generation nuclear energy systems due to its superior neutronics performance,high thermal conductivity,high boiling point,and excellent chemical stability.The impurity elements such as carbon and sulfur significantly affect the properties and safety of lead-bismuth alloys.However,there is no standard method established at home and abroad for the determination of carbon and sulfur contents in such alloys to date.In this study,the experimental conditions for measuring carbon and sulfur contents in lead-bismuth alloy by high-frequency combustion-infrared absorption method were systematically investigated.Some key parameters including flux blank,flux type and amount,and sample mass were studied.The results showed that the blank value was greatly reduced without interfering with the measurement after tin flux was cleaned with dilute hydrochloric acid followed by drying,and tungsten flux was treated at 400 ℃ for 4 h.The optimized analytical procedures were described as follows: 0.50 g of sample was accurately weighed; then 0.20 g of tin granules and 1.30 g of tungsten granules were added as composite flux.The calibration curves were established using certified reference materials/standard samples of steel.The linear correlation coefficients of calibration curves for carbon and sulfur were 0.999 8 and 0.999 7,respectively,indicating high reliability of the calibration curves.The limits of detection (LOD) for carbon and sulfur were 0.000 3% and 0.000 03% (mass fraction,the same below),and the limits of quantification (LOQ) were 0.001 0% and 0.000 1%,respectively.The contents of carbon and sulfur in lead-bismuth alloy sample were determined according to the experimental method,and the relative standard deviations (RSD,n=6) of measurement results were 3.3%-4.6% for carbon and 6.3%-11% for sulfur.The spiked recoveries were 99%-107% and 102%,respectively.The proposed method was accurate and rapid with good repeatability,which was suitable for the efficient determination of trace carbon and sulfur in lead-bismuth alloys.This study provided technical support for quality control and safety assessment in nuclear energy applications.
  • Zhang Yingying, Liu Wenjing, Xue Ya’nan
    Metallurgical Analysis. 2026, 46(10): 99-104. https://doi.org/10.13228/j.boyuan.issn1000-7571.013121
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    The contents of sodium oxide and potassium oxide in aluminum oxide directly affect the aluminum electrolysis process and product quality.The development of an accurate and sensitive determination method is of great significance for product quality control.In this study,a method for the determination of sodium oxide and potassium oxide in aluminum oxide by sulfuric acid-microwave digestion-flame atomic absorption spectrometry (FAAS) was established.The acid medium,matrix effect,and interferences of coexisting components were systematically investigated.Sulfuric acid was selected as the digestion medium,and microwave digestion in a closed system was adopted for sample pretreatment.The influence of the aluminum matrix on the measurement was effectively eliminated by matrix matching.Under the optimal conditions,the analytical wavelengths for sodium and potassium were 589.0 nm and 766.5 nm,respectively.The linear correlation coefficients of the calibration curves for sodium oxide and potassium oxide were both greater than 0.995.The limits of detection (LOD) for sodium oxide and potassium oxide were 0.000 2% and 0.000 5% (mass fraction,the same below),and the limits of quantification (LOQ) were 0.000 7% and 0.001 8%,respectively.The contents of sodium oxide and potassium oxide in aluminum oxide samples were determined according to the experimental method,and the relative standard deviations (RSD,n=11) of the measurement results were between 1.1% and 4.4%.The proposed method was applied to the determination of sodium oxide and potassium oxide in certifired reference materials (CRMs) and actual samples of aluminum oxide,and the measured results were consistent with the standard values or those obtained by inductively coupled plasma mass spectrometry (ICP-MS).The proposed method combines the high efficiency and cleanliness of microwave digestion with the high sensitivity of FAAS,and it is suitable for the accurate determination of trace sodium oxide and potassium oxide in aluminum oxide.
  • Long Xingjie
    Metallurgical Analysis. 2026, 46(10): 105-112. https://doi.org/10.13228/j.boyuan.issn1000-7571.013100
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    Hydrometallurgical zinc electrolyte contains high-concentration zinc (45-60 g/L) and magnesium (15-20 g/L),as well as low-concentration calcium (0.5-1 g/L).The traditional EDTA titration method makes it difficult to separately determine calcium and magnesium under high zinc matrix.The flame atomic absorption spectrometry (FAAS) requires multiple dilutions and the addition of lanthanum salt releasing agent,resulting in cumbersome operations and failing to achieve the continuous and rapid analysis of the three elements.In this study,a combined analytical method was proposed.Based on an improved Cu-PAN indicator system,the contents of zinc and total calcium and magnesium were sequentially titrated under controlled pH conditions; then the content of calcium was accurately determined by inductively coupled plasma atomic emission spectrometry (ICP-AES); finally,the content of magnesium was calculated by the subtraction method.The proposed method effectively eliminated the interference of preferential zinc complexation with magnesium determination,and avoided the problems such as ambiguous endpoint judgment and complex operations in traditional methods.Two hydrometallurgical zinc electrolyte samples were analyzed according to the experimental method,and the relative standard deviations (RSD,n=6) of determination results for zinc,calcium,and magnesium were between 0.40% and 1.2%,with spiked recoveries ranging from 98.0% to 106.7%.This method was compared with EDTA titration and FAAS,and it was found that the determination results showed good consistency.The proposed method was simple to operate and the results were accurate,realizing the continuous determination of zinc,calcium and magnesium with one single sample aliquot.It provided an efficient and reliable analytical technical support for the control of acid-zinc ratio and the early warning of calcium-magnesium enrichment in hydrometallurgical zinc electrolytes.
  • Yu Zhilong, Yang Zhong
    Metallurgical Analysis. 2026, 46(10): 113-118. https://doi.org/10.13228/j.boyuan.issn1000-7571.013086
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    Sponge cadmium is an important industrial raw material.The accurate and rapid determination of cadmium and zinc in sponge cadmium is of great significance for the production quality control.Aiming at the problems of cumbersome operation and many interference factors in traditional analytical methods,a method for the rapid and simultaneous determination of cadmium and zinc in sponge cadmium was established based on EDTA titration.The dosage of masking agent and the pH condition at titration endpoint were systematically optimized.The optimal conditions were obtained as follows: 0.20 g of ascorbic acid,1.0 g of potassium fluoride and 10 mL of saturated thiourea solution.The coexisting ions such as Fe36,Al3+,Sn4+ and Cu2+ could be effectively masked under these conditions.The pH at first endpoint (for determination of total cadmium and zinc) and second endpoint (for replacement titration of cadmium) was 6.0 and 5.8-5.9,respectively.The contents of cadmium and zinc in sponge cadmium sample were determined according to the experimental method under optimized conditions,and the relative standard deviations (RSD,n=9) of measurement results were 0.09% and 2.1%,respectively.The determination results were consistent with those obtained by EDTA titration method (for determination of cadmium) in Appendix A of GB/T 26042-2010 and inductively coupled plasma atomic emission spectrometry (for determination of zinc).The proposed method had advantages of sharp color change at endpoint,simple operation and high accuracy,and it was suitable for the routine analysis of zinc and cadmium content in sponge cadmium.