28 August 2025, Volume 45 Issue 8
    

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    Resource recycling
  • Technological advancements in safe and green resource utilization of aluminum ash residue
    LIU Chuanyi, XU Mujian, HONG Minghui, ZHANG Yueqing KONG Deyang, ZHANG Qingjian
    Metallurgical Analysis. 2025, 45(8): 1-9. https://doi.org/10.13228/j.boyuan.issn1000-7571.012824
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Aluminum ash residue has been listed in the National Catalogue of Hazardous Wastes for strict management due to its environmental hazards. However, with its high aluminum content, aluminum ash residue possesses significant recycling value. This paper tracks the latest environmental regulatory requirements for aluminum ash residue. It identifies its main components and environmental hazard characteristics, particularly heavy metal leaching toxicity and Al/AlN reactivity. The environmental risk sources associated with aluminum ash residue are analyzed, and its environmental and health risks are evaluated. The progress in both harmless disposal (including wet, thermal, and combined methods) and resource utilization (primarily in the production of water purification materials, building materials, and refractory materials) of aluminum ash residue is reviewed. Finally, key research directions for developing safe and green resource utilization technologies for aluminum ash residue are proposed, providing technical support for its future effective environmental management.
  • Enhanced phosphorus adsorption from water by mechanical ball-milling modified steel slag
    DU Xinran, YIN Chengyue, NIU Yating, GAO Shudan, HAN Haoran, BIAN Rongxing
    Metallurgical Analysis. 2025, 45(8): 10-18. https://doi.org/10.13228/j.boyuan.issn1000-7571.012920
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    Eutrophication of water bodies caused by excessive nitrogen and phosphorus is one of the water environment pollution problems worldwide. In this paper, the industrial by-product steel slag was selected as the research focus. The effects of initial pH, initial phosphorus mass concentration, steel slag dosage, and reaction time on the phosphorus removal by mechanical ball-milling modified steel slag were investigated. The phosphorus removal mechanism of steel slag was analyzed using scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR). The results showed that mechanical ball-milling could significantly enhance the specific surface area of steel slag, which increased from 0.78 m2/g before modification to 4.39 m2/g. The optimal conditions for phosphorus removal were determined as follows: pH=9, dosage of 1.0 g/L, and reaction time of 24 h. Under these conditions, the adsorption capacity was 7.64 mg/g. The adsorption of phosphorus by steel slag followed the pseudo-second-order kinetic model, and the adsorption isotherms conformed to the Langmuir model. The removal of phosphorus using mechanical ball-milling modified steel slag was controlled by dual factors, i.e., physical adsorption and chemical adsorption. Monolayer chemical adsorption was dominant, which was accompanied by chemical precipitation and surface complexation.
  • Process mineralogical study on blast furnace slag during high-temperature carbonization—low-temperature chlorination
    ZHONG Xiang, LÜ Xueming, SHI Zhixin, GAO Jian
    Metallurgical Analysis. 2025, 45(8): 19-26. https://doi.org/10.13228/j.boyuan.issn1000-7571.012814
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    The mineralogical characteristics of the integrated process from blast furnace slag to carbide slag to chlorinated residue, along with the occurrence and transformation behavior of titanium, were systematically studied using the AMICS automatic mineral analysis system. Results indicate that titanium in blast furnace slag primarily resides in perovskite (51.76%), titanium-rich pyroxene (26.96%), and titanian diopside (21.17%). Mineral crystallization followed the sequence: metallic iron > perovskite > titanium-rich pyroxene > titanian diopside. During high-temperature carbonization, titanium in perovskite transformed into titanium carbide. Titanium carbide particles (0.5-5 μm) were encapsulated within titanian augite, forming titanium carbide coatings surrounding metallic iron. The low-temperature chlorination process demonstrated significant selectivity: successful chlorination of most titanium carbide increased the titanian augite content in the residue to 94.90%(mass fraction, the same below). Unreacted titanium carbide (3.38%) concentrated within the core zones of titanian augite grains, and zones with well-developed fractures exhibited higher chlorination completeness. These findings elucidate the phase transformation mechanism of titanium during blast furnace slag valorization, providing a theoretical basis for enhancing titanium recycling efficiency.
  • Research progress on formation, pollution characteristics and mineral components resource utilization of municipal solid waste incineration fly ash
    LI Weiting, CHEN Xinlong, FENG Junli, LIN Jinyuan YI Jiaying, DAI Shijin, HE Hongping
    Metallurgical Analysis. 2025, 45(8): 27-37. https://doi.org/10.13228/j.boyuan.issn1000-7571.012818
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    Municipal solid waste incineration fly ash contains harmful substances such as heavy metals and dioxins (PCDD/Fs), so it is classified as hazardous waste. The common disposal method of fly ash is sanitary landfilling after solidification/stabilization treatment. However, this method occupies a large amount of land resources and poses a risk of secondary pollution, which cannot meet the requirements of urban sustainable development. The incineration fly ash is rich in effective mineral components such as CaCO3, SiO2, and Al2O3. With the rapid development of waste incineration technologies, resource utilization has become an important development trend. In this paper, the formation process, basic composition, and typical physical and chemical properties of incineration fly ash were systematically introduced. The main sources and migration and transformation mechanisms of heavy metals in fly ash were analyzed. Then the formation pathways of PCDD/Fs in fly ash were discussed. The differences in pollutant contents in fly ash across different regions and seasons were compared. Finally, the progresses on representative resource utilization disposal technologies and heavy metal separation-extraction technologies were summarized based on the main components of fly ash.
    • Solid waste identification
  • Solid waste identification of typical lead-containing smelting residues
    WU Suru, ZHU Jinbo, JING Xiangchao, CHEN Yan, LI Tao, WANG Zhaorui
    Metallurgical Analysis. 2025, 45(8): 38-44. https://doi.org/10.13228/j.boyuan.issn1000-7571.012838
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    The solid waste attributes of two samples declared as "lead concentrate powder" and "lead-zinc ore" were identified and analyzed. Based on characteristics such as element content, phase composition, microscopic morphology, and particle size distribution, it was concluded that the two samples were lead-containing fume and lead pyrometallurgical slag, respectively. The main elements in the "lead concentrate powder" sample were lead, sulfur, zinc, tin, chlorine and copper, and the main phases were lead sulfate, basic lead chloride and zinc stannate. The particle size was very fine, and the microscopic morphology consisted of extremely fine spherical particle aggregates. These features are inconsistent with the characteristics of common lead ores, indicating it is lead-containing fume produced during pollution control processes. The main elements in the "lead-zinc ore" sample were silicon, zinc, iron, calcium, aluminum and lead, and its main phases were hardystonite, willemite, calcium zinc silicate and gatena. Its microscopic morphology showed a honeycomb-like microporous structure, consistent with lead pyrometallurgical slag. According to GB 34330-2017, both samples were identified as solid wastes.
  • Multi-technique approach for solid waste identification of imported copper rice
    ZHOU Junlong, TANG Zhikun, LIN Chunmei, LI Quanzhong ZHAO Quan, CHEN Yihao, XIAO Dahui
    Metallurgical Analysis. 2025, 45(8): 45-49. https://doi.org/10.13228/j.boyuan.issn1000-7571.012850
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    This study established a method for identifying the solid waste attributes of "imported copper rice" by integrating visual inspection with ultra-depth-of-field microscopy for morphological analysis, X-ray fluorescence (XRF), X-ray diffraction (XRD) and inductively coupled plasma atomic emission spectrometry (ICP-AES) for inclusion composition/phase/element characterization, infrared carbon/sulfur analysis for graphite quantification, as well as high-frequency melting to assess direct usability as premium recycled copper feedstock. Results revealed: black flaky appearance; 6.0% deep-black undersize fraction (<120 mesh); wrinkled morphology with surface-adhered black substances and embedded particles; predominant graphite, copper and trace lithium nickelate via multi-technique detection; open flames/thick smoke during melting, yielding excessive slag without consolidated copper ingot formation (metal recovery rate: 58.7%). These characteristics contradicted GB/T 38471-2023 Recycled Copper Raw Materials while exhibiting fundamental deviations from conventional recycled copper, with inclusions exactly matching characteristic markers of graphite anodes in lithium-ion batteries. Based on copper foil current collector recycling process and GB 34330-2017 General Rules for Solid Waste Identification, the material is classified as solid waste derived from copper foil current collectors of graphite anodes in recycled lithium batteries.
    • Analytical testing
  • Determination of 10 elements in toxicity leachate from zinc smelting by-product gypsum slag by inductively coupled plasma atomic emission spectrometry
    LONG Xingjie, YANG Ping, LIU Chuanshi, WEI Wei, YANG Juncheng
    Metallurgical Analysis. 2025, 45(8): 50-57. https://doi.org/10.13228/j.boyuan.issn1000-7571.012811
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    Gypsum slag represents the highest-yield residue in hydrometallurgical zinc smelting, with characterization of its leaching toxicity being critical for scientific management and resource utilization. This study employed the sulfuric acid-nitric acid method for toxicity leaching tests on zinc smelting by-product gypsum slag. Filtered leachates (0.45 μm microporous membrane) underwent acid digestion with nitric acid; samples were analyzed in radial viewing mode via inductively coupled plasma atomic emission spectrometry (ICP-AES) to quantify 10 target elements (As, Ba, Cd, Cr, Cu, Ni, Pb, Se, Hg, Zn). This established a validated determination method for these elements in toxicity leachates, demonstrating: and the linear correlation coefficients were all no less than 0.999 9, The limits of detection of the elements ranged from 0.000 92 to 0.006 4 mg/L. Ten elements in the toxicity leaching solution of zinc smelting by-product gypsum slag were determined according to the experimental method. The relative standard deviations (RSD, n=11) of the determination results were between 1.1% and 9.9%, and the spiked recoveries were between 90%-115%. The contents of ten elements in the toxicity leaching solution of zinc smelting by-product gypsum slag were determined using the developed method and inductively coupled plasma mass spectrometry (ICP-MS). The results showed that the measured values from the two methods remained consistent.
  • Determination of platinum, palladium and rhodium in waste ternary catalysts by hydrogen reduction-microwave digestion-inductively coupled plasma atomic emission spectrometry
    LIU Qiuxiang, YAN Fangping, LOU Caiying, YE Xiangyu, WEI Qing
    Metallurgical Analysis. 2025, 45(8): 58-65. https://doi.org/10.13228/j.boyuan.issn1000-7571.012830
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    Accurate determination of Pt, Pd and Rh in waste ternary catalysts is crucial for precious metal catalyst recycling. Surface oxidation of precious metals under complex service conditions hinders complete dissolution of their oxides even with microwave digestion, resulting in underestimated Pt, Pd and Rh determinations. This study introduced hydrogen reduction to convert metal oxides into metallic Pt, Pd and Rh. Subsequent digestion employed a 15 mL HCl-3 mL H2O2 mixed acid system via microwave digestion, followed by indutively coupled plasma atomic emission spectrometry (ICP-AES) determination. This established a hydrogen reduction-microwave digestion-ICP-AES method for Pt, Pd and Rh determination in waste ternary catalysts. Optimized digestion at 180 °C for 30 min achieved complete dissolution. A linear relationship was observed between the emission spectral intensity and the mass concentration of Pt, Pd, and Rh within the range of 1-20 mg/L; the linear correlation coefficients of the calibration curves were not less than 0.999 9. The limits of detection for Pt, Pd and Rh by this method were 0.000 08%-0.000 11% (mass fraction, the same below), and the limits of quantification were 0.000 25%-0.000 38%. According to the experimental method, the determined contents of Pt, Pd and Rh in the waste ternary catalyst showed relative standard deviations (RSD,n=7) not more than 2.0%, and the spike recoveries were in the range of 96%-104%. The same waste ternary catalyst sample was analyzed for Pt, Pd, and Rh by this method in three different laboratories, and the results were in agreement.
  • Determination of platinum, palladium and rhodium in waste automotive exhaust catalysts by nickel sulfide fire assay preconcentration-inductively coupled plasma atomic emission spectrometry
    MA Xiaohui, XIAN Yun
    Metallurgical Analysis. 2025, 45(8): 66-72. https://doi.org/10.13228/j.boyuan.issn1000-7571.012844
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    With the surge in scrapped automobiles, the concentrations of platinum group metals (including platinum, palladium and rhodium) in the exhaust catalysts, known as "urban mines", are far higher than those in primary ore. Therefore, accurate determination of platinum, palladium and rhodium contents is essential for optimizing the recovery process, avoiding metal loss, unlocking economic value, and ensuring resource security. In this study, the sample was roasted at 600 ℃ for 4 h, then mixed with a flux (containing 0.7 g of nickel powder, 0.35 g of sulfur powder, 1.5 g of ferrous sulfide, 40 g of sodium carbonate, 5 g of silicon dioxide, 40 g of borax, and 1 g of flour). The mixture was melted at 1 050 ℃ for 60 min. After coprecipitation separation by adding 1.0 mg of tellurium, the contents of platinum, palladium and rhodium were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). This established a method for the determination of platinum, palladium and rhodium in waste automotive exhaust catalysts by nickel sulfide fire assay preconcentration combined with ICP-AES. Applying this method to waste catalyst samples, the relative standard deviations (RSD,n=11) were less than or equal to 5.5% and the spiked recoveries ranged from 99.8% to 100.4%. Analysis of the international certified reference material for automobile catalysts (SRM2556) yielded results for platinum, palladium and rhodium that were in good agreement with the certified values. The method employs a small-scale nickel sulfide fire assay technique, which ensures efficient capture of platinum, palladium and rhodium while significantly reducing nickel powder consumption. The resulting small nickel sulfide button exhibited favorable pulverization and dissolution properties. Following dissolution with aqua regia and employing tellurium coprecipitation and stannous chloride separation to effectively eliminate interference from base metals, the ICP-AES detection significantly enhanced the accuracy of precious metal determination.
  • Determination of aluminum,manganese,iron,chromium,titanium, silicon and lead in welding fumes by inductively coupled plasma atomic emission spectrometry
    JIANG Shiqin, ZHANG Fengyong, LIU Manyu, HONG Ye, LI Lin, WANG Qizhao
    Metallurgical Analysis. 2025, 45(8): 73-79. https://doi.org/10.13228/j.boyuan.issn1000-7571.012867
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    Welding fumes exhibit complex composition and cannot be completely dissolved with inorganic acids. When alkali fusion digestion is employed, matrix effects from high salt content cause significant result fluctuations. This study subjected samples to alkali fusion at 740 ℃. After acidification, aliquots of the mother liquor were diluted to reduce salt concentration. Matrix-matched standard solutions with NaCl effectively eliminated matrix effects, establishing an inductively coupled plasma atomic emission spectrometry (ICP-AES) method for determining aluminum, manganese, iron, chromium, titanium, silicon and lead in welding fumes. Coexisting elements caused no spectral interference.The linear correlation coefficients of calibration curves for each element were all higher than 0.999 9. The limits of detection for the elements ranged from 0.000 6% to 0.016 2%, and the limits of quantification from 0.003% to 0.081%. The contents of aluminum, manganese, iron, chromium, titanium, silicon and lead in a welding fume sample were determined according to the experimental method. The relative standard deviations (RSD, n=11) were between 0.66% and 1.3%, and the spiked recoveries were between 99% and 110%.
  • Determination of silicon dioxide in silica fume by coagulation gravimetry combined with inductively coupled plasma atomic emission spectrometry
    MU Yinghua, WANG Yapeng, HU Weizhu
    Metallurgical Analysis. 2025, 45(8): 80-85. https://doi.org/10.13228/j.boyuan.issn1000-7571.012914
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    Silica fume, a solid waste from metallurgical processes with high silicon dioxide content, requires accurate quantification of silicon dioxide to enable effective reuse. In this method, 0.300 0 g of sample was fused at 1 000 ℃ for 30 min with 2.0 g of sodium carbonate-boric acid-sodium peroxide mixed flux. After acidification with hydrochloric acid, all silicon dioxide was converted to silicic acid. The silicic acid was coagulated using 15 mL of 0.50 g/L polyethylene oxide solution, followed by filtration, calcination, and gravimetric determination of the precipitated silicon dioxide. Trace residual silicon in the filtrate was quantified by inductively coupled plasma atomic emission spectrometry (ICP-AES). The total silicon dioxide content was obtained by summing both values. For three silica fume samples, the relative standard deviations (RSD,n=7) of determination results were 0.19%-0.23%. The determination result of siliceous sandstone certified reference material GBW03114 was 89.50%, which was consistent with certified value of 89.59%. Low reagent cost and minimal waste discharge comply with green development principles.
  • Determination of fluorine and chlorine in typical copper/zinc-containing materials by combustion furnace-ion chromatography
    LI Yijun, CHEN Tingxin, WANG Bisheng, ZHONG Jianhai WANG Fengrong, ZHENG Ruijuan, ZHANG Yanyan, FENG Junli
    Metallurgical Analysis. 2025, 45(8): 86-92. https://doi.org/10.13228/j.boyuan.issn1000-7571.012858
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    As a major consumer of copper and zinc, China imports substantial quantities of copper/zinc-containing materials. Accurate determination of fluorine and chlorine contents is vital for ecological security and equipment protection. This study establishes a combustion furnace-ion chromatography method for determining fluorine and chlorine in typical copper/zinc-containing materials. Optimized combustion conditions include: sample mass of 30 mg, mass ratio of tungsten trioxide combustion accelerator to sample of 1∶1, combustion temperature of 1 100 ℃, combustion time of 300 s, and water feeding rate of 0.2 L/min. The results showed that the mass concentration of fluorine and chlorine in the range of 0.20-4.0 μg/mL and 0.10-2.0 μg/mL exhibited good linear relationships with their corresponding peak areas, respectively. The limits of detection of fluorine and chlorine in this study were 7.71 mg/kg and 2.86 mg/kg, and the limits of quantification were 25.71 mg/kg and 9.52 mg/kg, respectively. The proposed method was applied for the determination of fluorine and chlorine in three copper/zinc-containing material samples, and the relative standard deviations (RSD,n=11) of the results were between 0.74% and 2.1%. The contents of fluorine and chlorine in certified reference materials of copper ore/concentrate were determined according to the experimental method, and the measured results were consistent with the certified/reference values. The contents of fluorine and chlorine in standard samples of zinc oxide concentrate (SYDK101, SYDK102) were determined according to the experimental method, and the measured results were consistent with the standard values. This method allowed for the direct sample introduction of copper/zinc-containing samples with continuous automation of combustion, absorption, and determination processes. It provided technical support for the rapid determination of imported copper and zinc-containing materials.
  • Determination of silver in zinc hydrometallurgy leaching residue by flame atomic absorption spectrometry
    LUO Kailiang, CAI Hongxin, LI Benfen
    Metallurgical Analysis. 2025, 45(8): 93-98. https://doi.org/10.13228/j.boyuan.issn1000-7571.012928
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    Silver content in zinc hydrometallurgy leaching residue is a critical trade settlement indicator, necessitating accurate determination. After multistage processing, the residue exhibits strong chemical stability and high insolubility, resisting complete decomposition by conventional aqua regia. This study employed an ammonium fluoride-hydrochloric acid-nitric acid-perchloric acid digestion system. Silver was determined by flarne atomic absorption spectrometry (FAAS) in 10% hydrochloric acid matrix using air-acetylene flame at 328.1 nm. 5 mL of saturated ammonium fluoride solution effectively removed silicon dioxide. The linear range of silver in calibration curve was 0.25-1.50 μg/mL, and the linear correlation coefficient of the calibration curve was r=0.999 6. The limit of detection of method was 6.08 mg/kg and the limit of quantification was 20.0 mg/kg. The content of silver in actual sample of zinc hydrometallurgy leaching residue was determined according to the experimental method. The relative standard deviations (RSD,n=11) of determination results were between 1.2% and 1.8%, and the spiked recoveries were between 96% and 103%. Results agreed with fire assayenrichment-gravimetric method.
  • Determination of 5 components in recycled product from smelting iron-containing solid waste by X-ray fluorescence spectrometry with fusion sample preparation
    PANG Zhenxing, JIAO Li, JIA Xiaohong, YAO Ruixue, DU Shiyi, WANG Guiyu
    Metallurgical Analysis. 2025, 45(8): 99-105. https://doi.org/10.13228/j.boyuan.issn1000-7571.012892
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    With accelerated resource utilization of steel solid wastes, conventional wet chemical analysis struggles to meet industrial demands for rapid and accurate detection due to inefficiency and operational complexity. In this study, a method based on fusion sample preparation combined with X-ray fluorescence spectrometry (XRF) was established for the determination of five components(TFe, SiO2, CaO, MgO, and Al2O3) in recycled product from smelting iron-containing solid wastes. The sample was first pretreated by ignition at 800 ℃ for 120 min. Subsequently, it was mixed with a flux (w(Li2B4O7)∶w(LiBO2)=2∶1) at a sample-to-flux dilution ratio of 1∶12 and fused at 1 050 ℃ for 12 min. Cobalt oxide was added as an internal standard to correct for high iron content and eliminate matrix effects on its determination. The linear correlation coefficients (r) of the calibration curves for all components exceeded 0.998. The proposed method was applied to determine the components in kiln slag, iron slag powder, ball-milled iron powder, and cold-pressed pellet samples. The relative standard deviations (RSD, n=5) of the determination results were all less than 1.5%. The results were in excellent agreement with those obtained by dichromate titration (GB/T 6730.65-2009) for TFe, and inductively coupled plasma atomic emission spectrometry (ICP-AES, GB/T 6730.63-2024) for SiO2, CaO, MgO and Al2O3. The proposed method provides an efficient and accurate technological approach for monitoring composition in steel solid waste resource recovery.
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