电感耦合等离子体原子发射光谱法(ICP-OES)测定含钒尾渣中钒的含量

以氢氟酸、硝酸消解样品,然后加入硫酸络合钛避免其在低酸度介质中水解,并且加热至产生三氧化硫烟以驱赶氢氟酸,以水稀释定容后采用电感耦合等离子体原子发射光谱法（ICP-OES）直接测定含钒尾渣中钒的含量。实验考察了在共存含有铁、钛、铝、铬、锰、钒等元素的含钒尾渣复杂基体中,基体效应、光谱干扰以及背景噪音等影响因素对钒测定的干扰,方法通过优选元素分析谱线、背景校正区域以及光谱仪工作条件,并且采用基体匹配法和同步背景校正法相结合的方式,消除了构成复杂且变化无常的样品基体对测定的影响。结果表明,方法可用于测定0.01%~6.0%的钒,并且样品基体在含20%~40%铁,5%~30%钛时,铝、铬、锰、钠、硅、钙、镁各元素1%~10%的变化对测定无影响,检测下限可达0.0009%;精密度RSD〈3%,加标回收率94%~106%,与高锰酸钾氧化-硫酸亚铁铵滴定化学分析法的测定结果对照一致。     

Thermal analysis of carbide slag solutions

A model of slag refining processes and a method of determining the reduction capability of slag solutions are presented. Carbide slags were analysed by DTA methods.     

Analytical study by SEM/EDX and metallographic techniques of materials used in the iron production process during the iberian period

This work is the archaeometric study of different types of materials used in iron production in the Iberian Period (6th-2nd century b.c.). The materials were recovered in several archaeological digs (which makes it possible to date the archaeological remains) on different sites in the Levante area of the Iberian Peninsula. The samples selected for this study belong to different materials used in the ancient iron production process such as ores, slags, finished objects, etc. The use of scanning electron microscopy (SEM) is proposed to observe surface images of the samples to determine their morphological, microstructural and topographic characteristics to obtain valuable information on the materials studied. The study also proposes chemical analysis of the elements in the sample by X-ray microanalysis (SEM/EDX) which provides both qualitative and quantitative information. The archaeometric study suggests that the iron obtained was very good quality, but the process was not economically efficient when viewed from today's perspective. Furthermore, the slag produced in the furnace can be related with the slag or impurities contained in the iron. It has also been possible to relate the ores and slag, some furnace conditions, the use of fluxes and also to differentiate types of slag.     

Hot particles in industrial waste and mining tailings

Industrial waste was studied concerning its radioactive pollution. Using known properties of the solid state nuclear track detector CR-39 we found among a high concentration of more or less homogeneously distributed single α-tracks discrete spots of very high enrichments of α-particles created by so called hot particles. We will report about the α-activity, the concentration of hot particles and about their ability to be air borne.     

无机物高温下微结构的研究

上海市钢铁冶金新技术开发应用重点实验室 ( SELF)的 U- 1 0 0 0型 Raman谱仪经过改造已能用两种方式在高温下进行测定。其一是由共焦显微镜 -显微加热台构成的“空间分辨法”。其二是利用电阻炉加热的“时间分辨法”。SELF正在进行冶金熔渣的微结构研究。这类物质的物性 (从冶金学考虑 ,首先是熔渣中的组元活度 )数据已有不少报道 ,但为了促进技术的发展 ,急需鉴别它们的可靠程度。并且 ,还有大量未定值的物性 (例如 :粘度、表面张力、介电常数、扩散系数等 )有待预测。而打通微观结构和宏观物性之间的渠道 ,则是解决上述问题的根本途径。本文介绍了 SELF在 <2 0 0 0 K条件下的 HTRS(高温 Raman谱 )实测和 DFT- MD计算机模拟两种研究手段 ,定量分析冶金熔渣微结构的基本思路以及若干初步的结果。事实上 ,冶金熔渣、地学中的岩浆、玻璃和陶瓷 ,乃致某些宝石都可认为是一大物类 ,所以 SEL F同时也正在进行着烯土类熔盐和功能晶体的研究。     

过滤用镁渣多孔陶瓷的制备与渗透性能

本文以镁渣,粉煤灰等为原料制备了镁渣基多孔陶瓷,评价了多孔陶瓷的孔隙参数,烧结性能,力学性能,渗透性能等,观察了多孔陶瓷的微观结构,研究了烧结温度、成型压力、原料配比和添加剂等因素等对多孔陶瓷理化性能的影响.结果表明,烧结温度1150℃,保温4 h可制得固废掺比为90;的镁渣基多孔陶瓷,成型压力对多孔陶瓷的气孔率、吸水率和体积密度具有较大影响.镁渣和粉煤灰的配比为7:2时,多孔陶瓷产品的综合性能较好.添加电石渣和碳粉为造孔剂能够匀化气孔分布,细化孔径,提高多孔陶瓷的气孔率和气体过滤性能.     

模拟熔融态黄磷炉渣制备微晶玻璃析晶规律研究

以SiO2-Al2O3、Na2O-SiO2-Al2O3 、K2O-SiO2-Al2O3、CaO-SiO2-Al2O3和MgO-SiO2-Al2O3五种混合辅料为研究对象,采用液-固混合法与热态黄磷炉渣进行高温混熔直接制CaO-Al2O3-SiO2系微晶玻璃.通过Factsage、差热分析和X射线衍射,并利用修正后的Johnson-Mehl-Avrami (JMA)方程,分析了不同辅料在高温下与热态黄磷炉渣混熔制备微晶玻璃的析晶规律.结果表明:混合辅料SiO2-Al2O3出现液相的最低温度为1595℃,而当加入碱金属或碱土金属作助熔剂时辅料的熔融液相温度均大幅降低.添加Na2O-SiO2-Al2O3辅料后制备出的微晶玻璃析晶活化能E为192.8718 kJ/mol,而添加K2O-SiO2-Al2O3辅料后其析晶活化能明显增加为306.4335 kJ/mol.当助熔剂为CaO和MgO时,其析晶活化能接近,分别为376.7427 kJ/mol和372.0462 kJ/mol.在五种混合辅料直接添加到热态黄磷炉渣制备微晶玻璃过程中,K2O-SiO2-Al2O3和CaO-SiO2-Al2O3辅料均出现目标主晶相为硅灰石(CaSiO3)的物相.综合考虑析晶活化能和物相组成,以K2O-SiO2-Al2O3为混合辅料直接加入热态黄磷炉渣制备出的微晶玻璃优于其它混合辅料的直接添加.     

不同冷却方式黄磷炉渣微晶玻璃析晶动力学研究

以水淬黄磷炉渣和自然冷却态黄磷炉渣为研究对象,采用熔融法制备CaO-Al2O3-SiO2系微晶玻璃.通过差热分析、X射线衍射和扫描电镜,并利用修正后的Johnson-Mehl-Avrami (JMA)方程和Augis-Bennett方程,分析了不同冷却方式下黄磷炉渣制备微晶玻璃的析晶规律.结果表明:不同冷却方式对微晶玻璃的析晶行为有所不同,水淬黄磷炉渣微晶玻璃的析晶活化能E为352.609 kJ/mol,自然冷却黄磷炉渣微晶玻璃的析晶活化能E为405.685kJ/mol;两种不同冷却方式的黄磷炉渣微晶玻璃的晶化机制均为三维体积晶化.水淬黄磷炉渣微晶玻璃中主晶相为硅灰石(CaSiO3)并含有少量的石英矿物;自然冷却黄磷炉渣微晶玻璃中主晶相为钙蔷薇辉石类(Ca(Mn2,Ca)Si2O6)和含铁硅灰石类固溶体((Ca,Fe) SiO3).以自然冷却渣制备的微晶玻璃性能优于水淬渣制备出的微晶玻璃.     

Use of Taguchi approach for synthesis of calcite particles from calcium carbide slag for CO2 fixation by accelerated mineral carbonation

This study is focused on the conversion of harmful materials (calcium carbide slag [CCS] and flue gas) into CaCO₃ particles through an accelerated mineral carbonation process. The influences of reaction temperature, amount of Na-oleate, solid-to-liquid ratio, and stirring speed on the properties of CaCO₃ particles were determined using XRF, XRD, SEM, FTIR, TG, and contact angle measurements. Experiments were designed based on an orthogonal array L9 (3⁴) of the Taguchi approach. The gas mixture of CO₂/N₂ (16.3% of CO₂ cons.) gas was used to represent the flue gas for each experiment. The formation of CaCO₃ particles from CCS depending on time was monitored via SEM. Experiments showed that the presence of Na-oleate in the slurry played a curial role in the carbonation process, and the conversion ratio of CO₂ into a solid carbonate phase was higher than that in the experiments conducted without Na-oleate. The crystallite size of CaCO₃ particles varied between 11.55 and 38.11 nm depending on the production conditions. Each obtained CaCO₃ particles were identified as calcite (cubic-like rhombohedral), which is in high demand in many industrial applications.     

Microchemical investigation of early iron metallurgy slags

A group of slags, dating back to Iron Age II (Aramean period, 800-720 B.C.), that appeared to be iron-smelting by-products, have been found at Tell Afis (North-Western Syria). The microchemistry of these materials has been studied by means of small-area X-ray photoelectron spectroscopy (XPS), X-ray induced Auger electron spectroscopy (XAES), scanning electron microscopy (SEM), electron-probe microanalysis (EPMA) and optical microscopy (OM). The results indicate that the slags can be associated with an iron-smelting process and show the presence of large amounts of Fe(II) and Fe(III) oxides and hydroxides mixed with different glassy and crystalline silicon compounds. The latter consist essentially of quartz and various silicates, such as wollastonite, melilite, Mg[SiO₄] or Mg[SiO₆] compounds and other complex aluminosilicates. This chemical information is used to elucidate some aspects of the early ironmaking process.