金矿石化学物相分析选择性溶剂实验探索

运用碘-碘化钾氨性溶液作为裸露及半裸露包裹金的选择性溶剂,硫代硫酸钠-亚硫酸钠溶液作碳酸盐包裹金的选择性溶剂,以及溴素-氯化钠溶液作硫化矿包裹金的选择性溶剂进行实验探索.使用国家标准物质GBW07190对方法进行评价,并对该标准物质中其他矿物中金(AAu)的这一相态做了更详细的分离,测定了其中的碳酸盐包裹金、褐铁矿包裹金、黄铁矿包裹金,石英和硅酸盐包裹金的含量.火焰原子吸收法测定金的检出限是0.05×10-6;石墨炉原子吸收法测定金的检出限是0.30×10-9.RSD为0.29%~11.6%,RE为0.11%~8.40%.方法适用于各种金矿物的相态分离,进一步细化了金的各种赋存状态,所得结果令人满意.完全满足矿床划带、选矿试验和成矿规律研究的实际需要.     

金化学物相分析的准确测定与进展

介绍了用I2–KI(NH4I)法测定金物相时应注意的事项,同时综述了近几年来金化学物相分析的研究进展,包括不同价态金的测定、"不可见金"在矿物中尤其是在硫化矿中的存在形式以及难处理金矿的化学物相分析技术的研究等。     

从碳到氮——以"金课"标准在碳基材料转化设计中提升学生创新思维培养

碳材料一直以来是无机化学教学中必不可少的内容,本文基于教育部提出的"两性一度"的金课标准,通过对碳基材料转化设计,由石墨和石墨烯逐渐切入新型光催化剂石墨相氮化碳,并对其进行结构、性质及改性分析,提高学生理论–实践–创新能力,培养学生创新思维。     

竹浆纤维素转化制低碳多元醇反应中有机氮对金属催化剂稳定性影响的研究

采用等体积浸渍法制备了一系列多孔竹炭负载的有机氮掺杂的镍钨催化剂,并将其应用于催化竹浆纤维氢解制C_2,3多元醇反应。有机氮源与催化剂前驱体中Ni²⁺络合,高温煅烧时载体表面碳、氮和金属离子相互作用后生成一定量的C₃N₄、氮化物和合金物相。通过XRD、XPS和TEM等表征手段分析了催化剂Ni-W/MBC表面物理化学性质与催化活性间的关系。结果表明,除了金属镍、氧化钨物相外,表面还含有Ni-W合金（NiWO₄为主）;金属粒子表面包围了一层石墨化C₃N₄物相。XPS分析表明,有机氮源高温分解反应后形成了C₃N₄物相。在反应条件下,15% Ni-20% W/MBC@M-0.25催化剂得到乙二醇收率为55.8%,而未添加有机氮源的催化剂15% Ni-20% W/MBC获得的乙二醇收率仅为36.9%。催化剂稳定性实验结果表明,Ni-W合金和C₃N₄物相的形成显著增强了Ni-W/MB催化剂的稳定性,延长了催化剂寿命。     

竹浆纤维素转化制低碳多元醇反应中有机氮对金属催化剂稳定性影响的研究（英文）

采用等体积浸渍法制备了一系列多孔竹炭负载的有机氮掺杂的镍钨催化剂,并将其应用于催化竹浆纤维氢解制C_(2,3)多元醇反应。有机氮源与催化剂前驱体中Ni~(2+)络合,高温煅烧时载体表面碳、氮和金属离子相互作用后生成一定量的C_3N_4、氮化物和合金物相。通过XRD、XPS和TEM等表征手段分析了催化剂Ni-W/MBC表面物理化学性质与催化活性间的关系。结果表明,除了金属镍、氧化钨物相外,表面还含有Ni-W合金(NiWO_4为主);金属粒子表面包围了一层石墨化C_3N_4物相。XPS分析表明,有机氮源高温分解反应后形成了C_3N_4物相。在反应条件下,15%Ni-20%W/MBC@M-0.25催化剂得到乙二醇收率为55.8%,而未添加有机氮源的催化剂15%Ni-20%W/MBC获得的乙二醇收率仅为36.9%。催化剂稳定性实验结果表明,Ni-W合金和C_3N_4物相的形成显著增强了Ni-W/MB催化剂的稳定性,延长了催化剂寿命。     

空心碳半球锂离子电池负极的高倍率性能研究

以聚苯乙烯球为模板,通过水热法包裹硬碳层,又用微波法迅速引发聚苯乙烯核裂解的两步反应,制备了高比表面的空心碳半球.采用扫描电镜和透射电镜观察材料形貌,并测试该负极的电化学性能.在高倍率充放电条件下,与石墨、中间相碳微球电极相比,空心碳半球显现出了更高的容量和优异的寿命.     

电感耦合等离子体质谱（ICP-MS）法测定碳质板岩样品中铂族元素

碳质板岩属黑色岩系,与多种金属(包括贵金属)成矿有密切的联系。按照常规的分析方法,硫镍试金溶剂配方都不能对贵金属元素有较好的富集,影响贵金属元素的测定。根据石墨岩中样品的成份特征,对测定铂族元素的常规硫镍试金配方进行了改进,增加了硝酸钾和氧化镁,且无需加入锇稀释剂。通过实验选择了合适比例配料,熔融后粉碎镍扣,加入盐酸分解,碲共沉淀剂富集。过滤沉淀用王水溶解。用电感耦合等离子体质谱(ICP-MS)法测定,Lu作内标,对碳质板样品中的铂族元素进行了测定。结果表明,加标回收率为85%～105%,能够满足碳质板岩中铂族元素的分析测定要求。     

基于g-C3N4/P25复合光电敏感体系的中草药抗氧化容量测定

采用粒径为25 nm的锐钛矿和金红石型混合相二氧化钛(TiO₂)材料(P25)替代常规锐钛矿型TiO₂, 制备了基于石墨氮化碳(g-C₃N₄)/混合相TiO₂(g-C₃N₄/P25)的可见光激发光电敏感体系. 研究结果表明, 石墨氮化碳(g-C₃N₄)大的平面结构不仅能够成为TiO₂纳米材料合适的高分散载体, 其高效载流子传输能力还赋予了复合体系优异的光电性能. 当g-C₃N₄掺杂质量分数仅为0.5%时, 复合体系的光电流响应信号可提高至原来的4.5倍, 增敏效果最好. 该光敏体系的研制显著简化了制备工艺并降低了成本, 同时有效提高了体系的可见光利用效率. 基于该g-C₃N₄/P25光电敏感复合体系, 首次采用光电化学方法实现了中草药抗氧化容量的测定, 为量化中药体系抗氧化性能评估提供了新的思路.     

多金属硫铁矿铜锌物相分析

有关岩石试样中铜锌物相分析,国内外已有许多研究,确定了不少常规分析流程。其中氧化铜与硫化铜的分离方法有H_2SO_(4~-)Na_2SO_3法、乙二胺法、(NH_4)_2CO_(3~-)NH_4OH法、HAc-Na_2SO_3法等。经作者试验,上述方法应用于含铜、铅、锌等元素的多金属黄铁矿试样,特别是含有较多活性硫化物(辉铜矿、斑铜矿、磁黄铁矿等)的试样时存在一定的问题。当用含有铵盐的试剂浸取氧化铜时,由于辉铜矿及斑铜矿的部分被浸取,使氧化铜的结果严重偏高;若采用H_2SO_4—Na_2SO_3酸法浸取时,则因各种共存活性硫化物的电化作用,使氧化铜的结果也徧高,在强酸介质中,由于会发生Cu~(2+)+ZnS(PbS)(?)CuS↓+Zn~(2+)的反应,使结果偏低。为克服上述问题,本文提出用50毫升15％乙酸-1毫升饱和氯化汞-1.2克无水     

不同包碳方式对LiFePO4/C微观结构及电化学性能的影响

综合利用碳-硫测试、XRD、SEM、BET、拉曼光谱、EIS及扣式电池测试等分析技术手段,对LiFePO4/C制备过程中原位包碳与非原位包碳(分别记为LFP-1、LFP-2)的研究结果表明,在碳含量、相结构一致的前提下,LFP-1为10μm左右带孔的大颗粒,LFP-2为由100nm左右小颗粒组成的类球状颗粒,前者的电荷转移电阻(Rct)、倍率性能、循环性能优于后者,这归结于不同的包碳方式导致的LiFePO4/C微观结构的不同,从而使拉曼光谱结果中LFP-1的ID/IG和Asp3/Asp2低于LFP-2,即前者石墨化程度高于后者。从而表明,碳的包裹情况对改善LiFePO4/C的电化学性能有重要的影响。该结果对提高橄榄石类锂离子电池正极材料的综合性能有重要意义。     

Application of Inductively Coupled Plasma-Atomic Emission Spectrometry/Mass Spectrometry to Phase Analysis of Gold in Gold Ores

Inductively coupled plasma-atomic emission spectrometry/mass spectrometry (ICP-AES/MS) is a potentially powerful tool in chemical phase analysis of gold in batch mode, especially applicable to the low-grade gold ores with gold content of far below detection limit of the other methods, but it has not been used in gold phase analysis of gold ores. In this work, three types of typical gold deposits (altered rock type, quartz vein type, and microscopic disseminated type) and national standard reference materials of gold ores were used to establish and validate a method for gold phase analysis of gold ores using ICP-AES/MS. The optimum conditions of phase analysis were determined, including the sample granularity and preparation procedures, separation absorbent, pretreatment procedures of various phases of gold and optimized instrument parameters. Evaluation of the optimized method showed that this method had acceptable precision (RSD: 1.1%–10.6%) and accuracy (relative error, RE: 0.5%–6.3%), and the detection results of gold in ores were comparable with those obtained using the hydroquinone volumetric method-extraction flame atomic absorption spectrometry (VOL-AAS) and graphite furnace atomic absorption spectrometry (GFAAS) methods. The sum content of gold of the 4 phases (free gold, F_Au; linked gold, L_Au; sulphide-bearing gold, S_Au; and other mineral-bearing gold, A_Au) conformed to the total gold content and was consistent with the results of rock-mineral identification. The proposed method had a low detection limit (0.30 ng g^–1) and wide linear range (5.0 ng mL^–1–20.00 μg mL^–1). It is a simple, rapid, and efficient method for gold phase analysis in batch form.     

氮杂环卡宾双核金络合物催化的胺芳基化反应

联萘胺出发合成了氮杂环卡宾双核和单核金络合物, 通过X射线的单晶衍射确定了它们的结构, 并将其应用于催化胺芳基化反应中, 以高达95%的收率得到吡咯烷类化合物. 综合上述实验结果, 发现氮杂环卡宾双核金络合物4b中存在着Au(I)-Au(I)间相互弱作用力, 而且这种弱相互作用可能对该催化反应起重要的作用, 以高收率得到吡咯烷类化合物.     

分子印迹聚合物负载纳米金催化剂的制备及其底物识别性能

以4-硝基苯甲醇与氯金酸的络合物为模板,利用聚合物空腔内胺基捕获NaBH4还原的纳米粒子,设计和制备了一种具有底物识别性能的分子印迹聚合物负载纳米Au催化剂(Au/MIP).运用红外光谱、紫外-可见光谱和扫描电镜等方法对催化剂进行了表征.同时以水为溶剂,过氧化氢为氧化剂,考察了催化剂在取代苯甲醇氧化反应中的催化性能.结...     

Environmentally Benign,Rapid, and Selective Extraction of Gold from Ores and Waste Electronic Materials

The extraction of gold from ores and electronic waste is an important topic worldwide, as this precious metal has immense value in a variety of fields. However, serious environmental pollution and high energy consumption due to the use of toxic oxidation reagents and harsh reaction conditions is a well‐known problem in the gold industry. Herein, we report a new chemical method based on the combined use of N ‐bromosuccinimide (NBS) and pyridine (Py), which has a greatly decreased environmental impact and reagent cost, as well as mild reaction requirements. This method can directly leach Au⁰ from gold ore and electronic waste to form Au^III in water. The process is achieved in a yield of approximately 90 % at room temperature and a nearly neutral pH. The minimum dose of NBS/Py is as low as 10 mm , which exhibits low toxicity towards mammalian cells and animals as well as aquatic creatures. The high leaching selectivity of Au over other metals during gold leaching is demonstrated, showing that this method has great potential for practical industrial application towards the sustainable refining of gold from ores and electronic waste.     

基于金纳米聚集体的核壳型SERS探针及其细胞内应用

利用金纳米粒子的聚集体作为表面增强拉曼散射（Surface enhanced Raman scattering,SERS）的增强基底,合成了一种二氧化硅包裹的核壳型SERS探针,并成功将该探针应用于活细胞的SERS光谱探测.实验中利用4-巯基苯甲酸（4-mercaptobenzoicacid,4MBA）作为拉曼标记物,...     

Deactivation studies of nano-structured iron catalyst in Fischer-Tropsch synthesis

A nano-structured iron catalyst for syngas conversion to hydrocarbons in Fischer-Tropsch synthesis (FTS) was prepared by micro-emulsion method. Compositions of bulk iron phase and phase transformations of carbonaceous species during catalyst deactivation in FTS reaction were characterized by temperature-programmed surface reaction with hydrogen (TPSR-H2), and XRD techniques. Many carbonaceous species on surface and bulk of the nano-structured iron catalysts were completely identified by combined TPSR-H2 and XRD spectra and which were compared with those recorded on conventional co-precipitated iron catalyst. The results reveal that the catalyst deactivation results from the formation of inactive carbide phases and surface carbonaceous species like graphite, and it will be increased when the particle size of iron oxides was reduced in FTS iron catalyst.     

Catalytic Activity of Anisotropic Gold Nanoplates towards Oxygen Reduction

Glassy carbon electrode (GCE) coated with anisotropic gold nanoplates (aAuNPs) was used for the study of oxygen reduction reaction (ORR) in 0.5 M sulfuric acid instead of bulk gold electrodes. The electrode cleaning/activation procedure lead to the removal of any charged and uncharged residues on the gold nanoplates, leaving the nanostructured surface highly active towards oxygen reduction. The advantages: much lower overpotential and larger current densities of oxygen reduction are ascribed to the unique nanostructures present on the carbon electrode surface‐the gold nanoplates. They are rich in edges providing a large population of Au (100) sites with unsaturated coordination exposed to the solution, and catalytically active. Measurements performed using a rotating disc electrode, modified with the gold nanoplates, confirmed that ORR proceeds via two separate steps: oxygen is reduced to hydrogen peroxide, and the peroxide is further reduced in a two‐electron reduction to water.     

双孔石墨管原子吸收法测定化探样品中的痕量金

建立了双孔石墨管原子吸收法测定化探样品中痕量金的方法。以王水溶解样品,泡沫塑料吸附,10 g/L的硫脲溶液解脱,2%抗坏血酸作为基体改进剂,用双孔石墨管原子吸收法测定化探样品中的痕量金。该方法仪器分析时间由65 s缩短到32 s,提高了工作效率,方法标准曲线线性相关系数为0.999 8,检出限为0.045 ng/g,测定结果的相对标准偏差为4.1%~6.9%(n=7),标准样品测定值与推荐值的相对偏差小于3.24%。该法适合批量化探样品中金的测定。     

The Electrochemical Oxidation of Sulphite on Gold Electrodes

The electro‐oxidation of sulphite is studied in acid media on gold macroelectrodes and Au particle array modified boron doped diamond electrodes. The sulphite oxidation proceeds through a one‐electron transfer process followed by a chemical step of second order (EC₂ mechanism), as evidenced by experimental voltammetry and digital simulation for both gold macroelectrodes and gold particle modified substrates. The diffusion coefficient of sulphite is calculated consistently for both cases at about 4×10^?9 m² s^?1, with the reverse peak behaviour concentration dependent. The arrays are made by electrodeposition and show a morphological transition from a quasi‐spherical to a star shape as the growth time of the particles increases. Kinetic parameters inferred from the electro‐oxidation at the macroelectrode can be successfully applied to model the gold particle modified electrode data to confirm the EC₂ mechanism, whilst recognising the overlapping diffusion layers of adjacent gold particles.