红土镍矿样品前处理方法和分析测定技术研究进展

随着常规镍来源的硫化镍矿资源的日益枯竭,可直接生产氧化镍、镍锍和镍铁等产品的红土镍矿倍受关注。对于红土镍矿中主量、次量、痕量元素的检测,相同的检测项目存在多种测试方法,且部分相同原理的测试方法存在细节上的差异,使得检测者选择合适的检测方法变得困难。本文综述了近年来红土镍矿中24种元素测定的样品前处理方式及分析技术研究进展。样品前处理方式依据目标元素及后续的分析方法进行选择,其中酸溶法和碱熔法用途最广。酸溶法引入的盐分少,操作简单,但是分解过程中易导致挥发元素As、Sb、Bi、Hg的损失,Cr易随高氯酸冒烟损失。碱熔法分解能力强,适合分析Cr、Si、全铁等项目,但会引入大量的盐类和因坩埚材料损耗而带入其他杂质,给后续分析带来困难。红土镍矿的分析技术依据实验室条件及目标元素的性质和浓度进行选择。电感耦合等离子体发射光谱法(ICP-AES)是主量、次量元素的主要分析方法,适合于分析含量为10-5~30%级别的金属元素;X射线荧光光谱法主要用于分析含量为10-3~1级别的元素,尤其适合于测定Al、Si、Ti、V和P,由于该方法的准确性依赖于一套高质量的标准样品,故更适合炉前检测或检测大批红土镍矿样品。电感耦合等离子体质谱法(ICP-MS)最适合于分析10-4含量以下的重元素,特别是稀土和贵金属元素。原子吸收光谱法(AAS)适合于分析10-4~10-2级别的Ca、Mg、Ni、Co、Zn、Cr、Mn等低沸点、易原子化元素。分光光度法主要用于分析Ni和P。原子荧光光谱法(AFS)主要用于分析As、Bi、Sb等易形成气态氢化物的元素。容量法主要用于分析Al、Fe、Mg和Si O2等主含量元素。尽管AAS、分光光度法、AFS法和容量法检测周期长,但所用仪器为实验室常规配置,可满足缺乏相应大型仪器实验室的日常检测。本文认为,针对各种检测方法的适用性及存在问题,应从开发微波消解法、固体进样直接测汞法、ICP-MS法以及Cr与其他元素同时分析的快速分析方法等方面开展研究,建立灵敏、准确的检测方法,从而更好地服务于红土镍矿的贸易、检验和综合利用。     

CdTe量子点荧光猝灭法测定赤泥中痕量镍

Cd Te量子点具有荧光强度高和稳定性好的优点,应用Cd Te量子点荧光猝灭法分析基体复杂的样品,需要有效分离对测定干扰的金属元素和高效富集待测元素。本文以巯基乙酸(TGA)作稳定剂,采用水相合成法制备了巯基乙酸修饰的Cd Te量子点,基于镍离子在p H=10.0硼砂缓冲溶液中对Cd Te量子点的荧光具有较强猝灭作用,建立了一种测定赤泥中痕量镍的荧光光度方法。荧光猝灭反应的最佳实验条件为:Cd Te量子点的浓度3.0×10-4mol/L,反应温度为室温,反应时间10 min,在此条件下镍离子浓度在2.0×10-7~7.8×10-5mol/L范围内与Cd Te量子点的相对荧光强度呈良好的线性关系;方法检出限为1.5×10-7mol/L。本方法针对Fe3+、Co2+、Cu2+等主要基体金属元素允许量低的问题,采用25%的2-羟基-4-仲辛氧基二苯甲酮肟(N530)磺化煤油萃取回收滤液中的Ni2+,镍回收率达到99%以上;赤泥中痕量镍的测定结果与催化光度法相符,加标回收率为98.3%-104.2%。     

利用X射线衍射和岩矿鉴定等技术研究河南汤家坪钼矿区主要矿物标型特征

汤家坪钼矿床是2006年探明的一处大型斑岩型钼矿床,前人用常规地质方法对该矿区基础地质工作和成矿规律研究已比较系统和完整,认为汤家坪钼矿床属于深源浅成斑岩型钼矿床,汤家坪花岗斑岩体为矿区钼矿的成矿母岩;但是没有从矿物学角度来应证这些成矿规律。本文从矿物学角度,采用分离单矿物进行化学分析、X射线衍射(XRD)及岩矿鉴定等技术,对汤家坪钼矿区的辉钼矿、黄铁矿、石英、长石4种矿物标型特征(化学组成、微量元素、晶体结构、晶胞参数、结构状态等)进行研究。结果表明:1该矿区辉钼矿全部是2H型多型变体,且成分中Re含量很低;辉钼矿的δ34S值为3.0‰,硫同位素变化范围小,接近于陨石硫,具深源硫的特点,硫来源于花岗斑岩。2黄铁矿微量元素以富含Mo、Co、Cu,贫Ni、Pb、Zn为标型特征,另外Au、Ag含量低,S/Se大于250000,与前人"S/Se大于250000~500000的地区不可能找到金矿"的结论相符。3石英富含Mo;成矿期石英脉中δ18O降低,表明成矿晚期有少量大气降水参与热液蚀变成矿。4长石富含Mo;轻稀土(La~Nd)含量大于中稀土(Sm~Ho)和重稀土(Er~Y)含量;钾长石的有序度、三斜度以及结构参数的值均较高,结构温度较低,表明该矿区钾长石为低温状态下的三斜对称的微斜长石,是热液作用的产物,岩体钾长石化对钼矿化最为有利。本研究应证了汤家坪钼矿床属于深源浅成斑岩型钼矿床,对于总结斑岩型钼矿成矿规律、找矿标志有重要意义。     

人体乳腺癌矿化的同步辐射研究

同步辐射具有常规光源不可比拟的优良性能,可用于微量生物矿化样品的物相、结构、形貌和成分研究。本文利用基于同步辐射光源的X射线粉末衍射(SR-XRD)、傅立叶变换红外光谱(SR-FTIR)、X射线荧光分析(SR-XRF)和X射线三维成像,对人体乳腺癌矿化进行了表征。研究表明,乳腺癌矿化的主要矿物物相为碳羟磷灰石,含有Sr、Zn等微量元素,其中砂粒体矿化具有独特的分层结构。研究结果为乳腺癌的病理研究和诊断提供了矿物学参考信息。     

风化煤及提腐植酸后残渣热解行为与动力学分析

应用热重-质谱(TG-MS)联用技术对风化煤(WC)及其腐植酸提取后残渣(WCR)的热解行为进行了研究,分析了非烃类(H2、H2O、CO和CO2)、低碳烃类(CH4、C3H6和C3H7)和芳烃类(C6H6)的实验结果,并利用Coast-Redfern积分法对其热解和烃类生成动力学进行了探讨,获得了热解过程和烃类生成动力学参数。结果表明:热解过程中风化煤的质量损失率(38.9%)略大于其腐植酸提取后残渣(36.6%);除CO和CO2外,残渣中非烃类、低碳烃类和芳烃类产物的逸出量都稍微或显著多于风化煤中各类组分的逸出量。用Coast-Redfern积分法求得的动力学参数很好地解释了这一结果。     

Distribution and partitioning of major and trace elements in pyrite-bearing sediments of a Mediterranean coastal lagoon

The formation of iron sulphide minerals exerts significant control on the behaviour of trace elements in sediments. In this study, three short sediment cores, retrieved from the remote Antinioti lagoon (N. Kerkyra Island, NW Greece), are investigated concerning the solid phase composition, distribution, and partitioning of major (Al, Fe) and trace elements (Cd, Cu, Mn, Pb, and Zn). According to ²¹⁰Pb, the sediments sampled correspond to depositions of the last 120 years. The high amounts of organic carbon (4.1–27.5%) result in the formation of Fe sulphides, predominantly pyrite, already at the surface sediment layers. Pyrite morphologies include monocrystals, polyframboids, and complex FeS–FeS₂ aggregates. According to synchrotron-generated micro X-ray fluorescence and X-ray absorption near-edge structure spectra, authigenically formed, Mn-containing, Fe(III) oxyhydroxides (goethite type) co-exist with pyrite in the sediments studied. Microscopic techniques evidence the formation of galena, sphalerite and CuS, whereas sequential extractions show that carbonates are important hosts for Mn, Cd, and Zn. However, significant percentages of non-lattice held elements are bound to Fe/Mn oxyhydroxides that resist reductive dissolution (on average 60% of Pb, 46% of Cd, 43% of Zn and 9% of Cu). The partitioning pattern changes drastically in the deeper part of the core that is influenced by freshwater inputs. In these sediments, the post-depositional pyritization mechanism, illustrated by overgrowths of Fe monosulphides on pre-existing pyrite grains, results in relatively high degree of pyritization that reaches 49% for Cd, 66% for Cu, 32% for Zn and 7% for Pb.     

UTEVA树脂分离纯化珊瑚中铀、钍的改进研究

珊瑚是记录海洋环境变化信息的载体之一,测定其U/Ca比值可重建海水温度或测定Th/U同位素比值可计算年龄重建海平面高度等.准确测定珊瑚中U、Th含量及同位素比值是提取所记载的海洋环境变化信息的前提,其难点在于高Ca基体分离和痕量U、Th富集纯化.基于此,本研究拟采用UTEVA树脂改进了一步富集分离珊瑚中U、Th的前处理...     

A Fundamental Plane of Black Hole Activity: Pushing Forward the Unification Scheme

We examine the disc-jet connection in stellar mass and supermassive black holes by investigating the properties of their compact emission in the hard X-ray and radio bands. We compile a sample of ∼100 active galactic nuclei with measured mass, 5 GHz core emission, and 2–10 keV luminosity, together with eight galactic black holes with a total of ∼50 simultaneous observations in the radio and X-ray bands. Using this sample, we study the correlations between the radio (L_R) and the X-ray (L_X) luminosity and the black hole mass (M). We find that the radio luminosity is correlated with both M and L_X, at a highly significant level. We show how this result can be used to extend the standard unification by orientation scheme to encompass unification by mass and accretion rate.     

Dynamics and radiation of young type-Ia supernova remnants: Important physical processes

Astronomy Letters - We analyze the physical processes that should be taken into account when modeling young type-Ia supernova remnants (SNRs) with ages of several hundred years in which forward...