X射线管辐射谱线分析

经Ni滤波片过滤的CuKa射线，并非为真正的单色X射线，其中含部分白色X射线和非CuKa特征谱线。用石英分析晶体（101）衍射面网将混入CuKa射线中的各种波长的谱线分离开，并测定其波长的范围，确定在CuKa射线中含有铁、镍、钴、铬四种元素的K系列谱线和钨的L系列谱线。发现在X射线粉末图谱中用CuKa（或Kβ）无法解释的弱衍射线却是由铁、镍等元素的特征谱线混入引起的。     

广西平果太平矿区外围铝土矿石工艺矿物学研究

以广西平果县太平铝土矿区外围的矿石为研究对象,采用化学分析、X射线粉晶衍射、光学显微鉴定、X射线能谱分析等方法对矿石的化学组成、矿物组成、矿物嵌布特征等进行了系统研究。结果表明,太平矿区外围铝土矿属于高铁的一水硬铝石型铝土矿,其中Al_2O_3含量为53. 06%,A/S值为10. 74,适用于拜耳法回收;共伴生组分中Fe_2O_3、Ti O_2、Ga、Nb达到综合回收利用指标。矿石选冶回收的目标元素Al主要以一水硬铝石、三水铝石的形式存在,平衡配分占比分别为85. 9%、6. 73%。矿石复杂的结构构造、矿物嵌布粒度、矿石中Fe、Si等元素不均匀分布等因素对Al的选冶回收有一定的影响。     

云南某含铜镍铁矿石回收铜镍的探讨

云南某铁矿含铜0.33%,镍0.14%,金0.11g/t,银0.13 g/t,铁14.60%,硅32.80%,氧化镁23.50%。利用了X射线衍射分析、扫描电镜等现代分析手段,进行了工艺矿物学研究,研究发现原矿中主要金属矿物为黄铜矿、磁铁矿、镍黄铁矿、赤铁矿,脉石矿物主要为蛇纹石、滑石、绿泥石。为了有效的回收矿石中的有价金属,进行了大量的试验研究。最终本文确定在磨矿细度60%-200目的条件下,以水玻璃+六偏磷酸钠+CMC做组合抑制剂,乙硫氮做捕收剂,采用一粗三精三扫的浮选流程,回收原矿中的铜、镍。所得混合精矿铜品位14.34%,回收率86.93%,镍品位4.30%,回收率64.17%。     

喷流沉积型多金属矿床中镍钼的赋存特征

喷流沉积型矿床是矿床地质学研究的前沿课题,查明矿石中重要组分(镍和钼)的赋存状态是该类矿床地质学研究的重要内容。湘黔地区天鹅山-黄家湾、大坪-大浒镍钼矿带是典型的海底喷流沉积矿床,本文采集该矿区的样品,应用化学和光谱定量分析、偏光显微镜和X射线衍射、扫描电镜、电子探针等大型现代仪器相结合的分析手段,研究了矿石中镍和钼的赋存状态。化学和光谱分析确定矿石中镍含量为3.76％,钼含量为4.99％;偏光显微镜下观察发现金属矿物零星分布,颗粒细小,结晶程度差,光学特征极不明显,晶体形貌特征难以观察,初步推断矿石矿物以胶状形式存在,但在光学显微镜下很难为这些矿物定名和描述;X射线衍射分析验证了偏光显微镜鉴定结果,印证了样品中存在很多非晶质矿物,仅有钨钼钙矿和镍黄铁矿两种矿物含有镍钼,且矿物含量很低(分别为0.4%和0.8%),对比化学分析结果,可推断样品还存在其他富含镍钼元素的矿物。进一步对富集镍钼元素的区域进行电子探针分析,最终确定了镍除了赋存于辉砷镍矿、方硫镍矿中,在胶状黄铁矿和磁黄铁矿边缘呈蠕虫状花边的镍黄铁矿中也有富集;钼主要赋存于碳硫钼矿中。矿石中的镍钼主要赋存于由胶态向结晶态过渡的金属矿物中,研究成果为该类矿床的矿石矿物学研究、选矿、冶炼及矿石综合利用提供重要的信息和依据。     

原位微区X射线荧光光谱分析装置与技术研究进展

原位微区X射线荧光(Micro-XRF)光谱分析技术是X射线光谱学领域一重要分支。近年来X射线毛细管光学透镜聚焦技术不断进步,以实验室X光源为基础的原位微区X射线光谱分析装置与应用技术快速发展,已成功应用于多领域样品的原位、多维、动态和非破坏性微区分析。文章介绍了近年来X射线毛细管光学透镜技术发展和原位微区X射线光谱分析装置研制进展,对近年来micro-XRF光谱分析技术在大气气溶胶颗粒物分析与来源识别、考古样品产地和真伪鉴别、古气候古环境重建研究中沉积纹层样品元素分析,以及刑侦科学中指纹样品的鉴定等应用领域进行了系统介绍,阐述了micro-XRF光谱分析技术性能的影响因素(空间分辨率和强度增益)。micro-XRF光谱分析技术不仅可以获取样品表面的信息,还能够获取样品内部的信息,成为目前国际上一门迅速发展的竞争技术。我国在毛细管透镜制造技术与性能研究,以及micro-XRF应用领域取得了重要进展。由于X射线焦斑尺寸对能量的依赖性以及样品基质对X射线的吸收效应,在微区定量分析中易引入较大误差,利用X射线毛细管透镜获取更小光斑尺寸与高稳定性的X射线光束,提高micro-XRF分析技术的空间高分辨率性能和对基体效应进行校正实验将是今后一个重要的研究目标和分析研究难点。     

熔融制样-波长色散和能量色散X射线荧光光谱仪应用于硅酸盐类矿物及疑难样品分析

目前硅酸盐类样品中主量元素一般采用熔融制样X射线荧光光谱法（XRF）测定，不仅单元素测定结果不能超差，而且百分数加和也要满足要求。但对于矿化样品，由于微量元素较高，往往造成不能满足加和质量要求。充分利用波长色散（WD）和能量色散（ED）复合式X射线荧光光谱仪同时波谱、能谱测定的优势，可使分析人员快速掌握样品组成信息，对评估矿化样品数据质量具有重要意义。本文利用波长-能量色散X射线荧光光谱仪，可在测定主量元素的同时加入更多的微量元素进行测定，而分析时间不延长。主量元素采用波长色散定量，次量元素主要采用能量色散测定，在保证主量元素准确度的情况下，合理设置测量条件，延长能谱测量时间，实现在波长色散12min左右测定主量元素的同时，能够提供14个微量元素如Rb、Sr、Y、Zr、Ba、Cu、Zn的测定结果和10个线性范围较窄或含量较低元素如Co、Ge、Pr、Ta的参考结果，24个微量元素最大检出限为16.76μg/g。通过准确度考核，主量元素测定结果与认定值基本一致，高含量微量元素测定结果亦满足定量分析要求。该方法可使分析人员快速掌握样品组成信息，为提供更加准确、可靠的数据奠定基础，有效地解决矿化疑难样品主量元素测定问题。     

利用工业废镍催化剂制结晶硫酸镍的研究

本文扼要介绍利用工业废镍催化剂制结晶硫酸镍的实验研究。实验结果表明，其产品质量达到国家标准，回收率达８８％。     

应用能谱-扫描电镜分析铜矿床伴生元素的赋存状态

铜矿床中的伴生元素通常具有较高经济价值,其矿物颗粒细小,往往从微米级到纳米级,因此难以被发现和获得利用,进而导致无法系统地对其赋存状态进行研究。本文以"里伍式"铜矿床中的矿石矿物为研究对象,通过背散射图像、二次电子像观察以及X射线光谱点、线与面分析技术的相互佐证,获得铜矿床伴生元素矿物物相、形貌特征、赋存状态、定性/定量及分布规律等信息。实验中选取扫描电镜的加速电压20kV、发射电流10μA、能谱脉冲处理活时间100s,同时对样品前处理、测试过程中的关键技术进行详细探讨,形成了一套有效的分析铜矿床中有关伴生元素的能谱-扫描电镜(EDX-SEM)微区分析方法。应用该方法分析查明四川里伍铜矿床中金、银、钴、铋、硒等元素的赋存状态,这些元素以独立矿物存在或类质同象的形式分布在其他矿物中。通过对这些伴生元素赋存状态的研究,为矿物工业价值的认定、矿床资源评价、伴生元素的回收利用提供了微观依据,为矿山的开采、选矿以及冶炼工艺过程的制定提供了技术支撑。     

地质样品中钴、镍的分析进展

早在20世纪初期,化学家就开展了比色法分析钴、镍的研究工作。由于比色法灵敏度不高且操作繁琐,人们开始追求更高效的固体样品消解方法、更简便的操作以及更高灵敏度和高精度的分析技术。在样品分解方面,逐渐发展出了酸溶和碱熔两套样品分解体系;在仪器分析方面,则发展出了原子吸收光谱法、等离子体光谱法、X射线荧光光谱法、等离子体质谱法等更加高效简洁的仪器分析技术。随着地质科学的发展,电子探针和激光剥蚀电感耦合等离子体质谱微区原位分析技术,以及多接收等离子体质谱镍同位素分析技术也逐渐发展起来。在元素分析方面,原子吸收光谱法、等离子体光/质谱法一般需要经过酸或者碱将样品分解为溶液状态,前处理流程较为繁琐;而X射线荧光光谱法采用熔片或者压片进行样品制备,前处理方法简单高效,更加受到青睐。在同位素分析方面,镍同位素逐渐应用到钴镍矿床研究中,近年有望通过典型矿床剖析明确多种成矿过程镍同位素的行为与分馏机制,如岩浆演化、热液蚀变、风化等。镍同位素的分离技术难度较高,因此,创新镍同位素的分离过程和测试方法,并建立更加简便的分析流程是未来发展的重点方向。在微区分析方面,激光剥蚀-电感耦合等离子体质谱比电子探针的样品...     

铜,镍高冰镍中主要硫化矿物的合成与研究

本文在合成高冰镍中主要矿物赫硫镍矿和辉铜矿的基础上,利用X射线衍射分析,光电能谱等手段研究赫硫镍矿晶体中镍、铜离子的存在状态。研究认为,镍以二价正离子和金属原子的形式存在于赫硫镍矿中。铜以一价化合态形式有限地取代镍离子进入赫硫镍矿的晶格,使其晶胞参数a增大0.0426,c增大0.0597。用电子探针分析,低温状态下赫硫镍矿含铜1.63wt%。     

Mineralogical and geochemical investigations of pyrite-rich mine waste from a kyanite mine in Central Virginia with comments on recycling

A pyrite-rich waste stream is one of three types generated from a kyanite mine in central Virginia near the town of Dillwyn, Buckingham County. Currently, ore consists of approximately 3% pyrite waste and an estimated 382,000 tons of this waste stream has been generated over the past 60 years. The mineralogy of the waste stream consists of variable amounts of pyrite (70–>99%), talc (1–20%), quartz (1–10%), kyanite (0.5–5%) with minor or trace amounts of magnetite, hematite, galena, anorthite and rare earth phosphate. Energy dispersive spectroscopy analysis indicates that talc has minor amounts of Al up to 1.57 wt% and Fe up to 4.29 wt% and pyrite grains have no impurities above detection limit of approximately 0.1 wt%. Bulk chemical analysis of selected elements using inductively coupled plasma-mass spectrometry analysis indicate that Zn (28.82–367.71 ppm), As (8.94–18.26 ppm), Se (44.62–64.50 ppm), Cd (0.19–1.03 ppm), Hg (0.87–35.91 ppm), and Pb (65.10–189.66 ppm) occur at levels of some environmental concern. Au and Ag concentrations are negligible. Currently the waste stream is well managed and sold, but for a low price. Talc is of sufficient quality to be of interest for recycling but the estimated 540 tons generated per year is not a suitable quantity to be economically viable. Currently, the waste stream is not viable for recycling for higher monetary value; however, the characteristics of the pyrite may enable such recycling in the future for solar energy technologies. This and other associated waste streams show long term promise for integrated recycling and may play important economic roles in an economically disadvantaged region.     

Recovery of valuable materials from aluminium salt cakes

Salt cakes, which are nominally waste products derived from aluminium dross melting furnaces, are complex mixtures of some 20 different compounds made up of many different elements. Normally they are regarded as waste products and they are disposed of in toxic waste dumps. However, it is shown here that some components are readily recoverable as high-grade products for recycling or sale and that the residues thus generated can be non-toxic. Recoverable components include metallic aluminium, salt (halite (NaCl) and sylvite (KCl)), alumina-containing compounds, and possibly hydrogen gas.     

一种香石(玉)的矿物种属及香味成分与成因分析

针对产自我国某地的一种具有天然奶油巧克力香味的香石(玉),利用常规化学分析、红外光谱分析及X射线衍射分析方法,确定了此种香石(玉)的矿物归属.并用固相微萃取-气相色谱-质谱联用分析技术分析香石(玉)的挥发性气体成份,结果表明:香石(玉)的化学成份w(B)/%为SiO2 49.02;MgO 43.51;Al2O3 0.48;CaO2.01;Fe2O3 1.41;H2O+11.00.红外光谱具有蛇纹石红外光谱特征,X射线粉末数据亦与蛇纹石吻合,其矿物种属确定为蛇纹石.香石(玉)的挥发成份中有67种有机组分,经鉴定含有18种具有香味的有机化合物,香味成分约占挥发性成分总量的55%左右.蛇纹石是一种层状硅酸盐矿物,呈卷曲的园柱管状结构,这种特殊结构决定了它具有吸附能力,在地质构造运动产生的特殊温度、压力环境下,被吸附的有机物熟化使蛇纹石产生如奶油巧克力的特殊香味.     

花石嘴元墓出土化妆品的初步研究

运用红外光谱、X射线衍射、拉曼光谱、X射线荧光光谱等分析手段对花石嘴元墓出土的化妆品进行了初步的定性分析和定量分析。结果表明,其主要成分为无机物,以碳酸铅最多,其次为磷氯铅矿,另含有少量石英;有机物含量则非常低,可能为油脂。根据古代文献的记载及相关的研究,推测该化妆品应作肤用增白之用。     

Rare earth elements:A review of applications,occurrence,exploration,analysis,recycling,and environmental impact

Rare earth elements(REE)include the lanthanide series elements(La,Ce,Pr,Nd,Pm,Sm,Eu,Gd,Tb,Dy.Ho,Er,Tm,Yb,and Lu)plus Sc and Y.Currently these metals have become very critical to several modern technologies ranging from cell phones and televisions to LED light bulbs and wind turbines.This article summarizes the occurrence of these metals in the Earth’s crust,their mineralogy,different types of deposits both on land and oceans from the standpoint of the new data with more examples from the Indian subcontinent.In addition to their utility to understand the formation of the major Earth reservoirs.multi-faceted updates on the applications of REE in agriculture and medicine including new emerging ones are presented.Environmental hazards including human health issues due to REE mining and large-scale dumping of e-waste containing significant concentrations of REE are summarized.New strategies for the future supply of REE including recent developments in the extraction of REE from coal fired ash and recycling from e-waste are presented.Recent developments in individual REE separation technologies in both metallurgical and recycling operations have been highlighted.An outline of the analytical methods for their precise and accurate determinations required in all these studies,such as,Xray fluorescence spectrometry(XRF),laser induced breakdown spectroscopy(LIBS),instrumental neutron activation analysis(INAA),inductively coupled plasma optical emission spectrometry(ICP-OES),glow discharge mass spectrometry(GD-MS),inductively coupled plasma mass spectrometry(including ICP-MS,ICP-TOF-MS,HR-ICP-MS with laser ablation as well as solution nebulization)and other instrumental techniques,in different types of materials are presented.     

熔融制样-X射线荧光光谱法测定重晶石中主次量元素

准确测定重晶石中硫酸钡及锶等组分的含量,对于评价矿石的质量品级十分重要。文章应用X射线荧光光谱法测定重晶石中BaO、Al2O3、Fe、CaO、MgO、SiO2、Na2O、K2O、Sr等9种主、次量组分。采用熔融片制样,消除了矿物结构效应,降低基体效应的影响,研究了熔样的条件,确定仪器测量的最佳参数。各元素相对标准偏差(RSD,n=10)≤10%,测定结果与化学法测定值相符,同时满足了ISO 9507对各元素分析结果准确度≤0.5%的要求。方法快速、准确,方便快捷,具有良好的精密度和准确度,可用于重晶石矿选矿样品尾矿、中矿、精矿中钡、锶、铁、钙、镁、铝、硅、钾、钠的同时测定,也可代替传统的化学法用于选冶实验分析。     

Kinetics of nickel leaching from spent catalyst in sulphuric acid solution

The kinetics of spent nickel oxide catalyst (NiO/Al₂O₃) leaching in sulphuric acid solutions was investigated. The effects of sulphuric acid concentration, temperature, stirring speed, and particle size on the rate of nickel leaching were studied. In addition, the reaction residues at various levels of nickel extraction were examined by SEM, X-ray diffraction, electron microprobe, and chemical analysis. The results of the kinetic analysis of the leaching data for various experimental conditions indicated that the reaction is controlled by diffusion through the catalyst network with the activation energy of 16.6 ± 0.9 kJ/mol. A linear relationship between the rate constant and the inverse square of the initial particle diameter is also characteristic for a diffusion-controlled process.     

高钙碳酸盐地质样品中铜镍的测定

用电感耦合等离子体质谱法和电感耦合等离子体发射光谱法测定高钙碳酸盐样品中的铜和镍。通过试验分析了高钙碳酸盐样品中钙对铜、镍测定的影响,并确定其影响因子,提出两套检测高钙碳酸盐样品中铜、镍的方案。方法经国家标准物质验证,测定值与标准值相符;相对标准偏差(RSD,n=10)两元素均小于2%。     

Biodiesel synthesis from non-edible oils by transesterification using the activated carbon as heterogeneous catalyst

The need for renewable environmentally friendly energy resources is growing every day. Biodiesel is one of the most promising alternatives to the conventional non-renewable energy resources. Heterogeneous catalysts proved a high efficiency in the transesterification of oils to produce biodiesel. In this research, activated carbon was tested as a heterogeneous catalyst in the transesterification of two non-edible oils (waste cooking oil and Jatropha oil) with methanol to produce biodiesel. Activated carbon was characterized using X-ray diffraction, scanning electron microscope and Fourier transformed infrared. The effect of different operating parameters, namely operation time (30, 60, 120 and 180 min), alcohol-to-oil molar ratio (4:1, 6:1, 8:1 and 10:1), catalyst loading [0.5, 1, 2, 3 and 5% (w/w)] and rotational speed (100, 200, 300 and 400 rpm), was investigated. Results showed that increasing the operational time, the alcohol-to-oil molar ratio and the catalyst loading increases the conversion to biodiesel but only to some extent; increasing the stirring rate was found to be beneficial to the process. The optimum conditions were found to be 2 h of heating, 6:1 alcohol-to-oil ratio, 1 wt% catalyst loading and 400 rpm stirring. Under optimum conditions, the conversion to biodiesel reached 93.95 and 93.27% for the waste cooking oil and the Jatropha oil, respectively. The properties of the obtained biodiesel (density, viscosity, flash point, pour point and cloud point) were measured giving promising results.     

Mineralogical and geochemical investigations of silicate-rich mine waste from a kyanite mine in central Virginia: implications for mine waste recycling

A kyanite mine in central Virginia produces a silicate-rich waste stream which accumulates at a rate of 450,000–600,000 tons per year. An estimated 27 million tons of this waste stream has accumulated over the past 60 years. Grain size distribution varies between 1.000 and 0.053 mm, and is commonly bimodal with modes typically being 0.425 and 0.250 mm and uniformity coefficients vary from 2.000 to 2.333. Hydraulic conductivity values vary from 0.017 to 0.047 cm/s. Mineralogy of the waste stream consists of quartz, muscovite, kyanite and hematite. Muscovite grains have distinct chemical compositions with significant Na₂O content (1.12–2.66 wt%), TiO₂ content (0.63–1.68 wt% TiO₂) and Fe content, expressed as Fe₂O₃ (up to 1.37 wt%). Major element compositions of samples were dominated by SiO₂ (87.894–90.997 wt%), Al₂O₃ (6.759–7.741 wt%), Fe₂O₃ (1.136–1.283 wt%), and K₂O (0.369–0.606 wt%) with other components being <1.000 wt%. Elements of environmental concern (V, Cr, Ni, Cu, Zn, As, Ag, Sn, Sb, Ba, Hg, Tl, and Pb) were detected; however, the concentrations of all elements except Ni were below that of the kyanite quartzites in the region from which the waste is derived. Both major and trace element compositions indicate minimal variation in composition. The waste stream has potential for recycling. Muscovite is suitable for recycling as a paint pigment or other industrial applications. Muscovite and hematite are commonly intergrown and are interpreted to be material where much of the elements of environmental concern are concentrated. Reprocessing of the waste stream to separate muscovite from other components may enable the waste stream to be used as constructed wetland media for Virginia and nearby states. Recycling of this mine waste may have a positive impact on the local economy of Buckingham County and aid in mitigation of wetland loss.