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| 昆明贵金属研究所->《贵金属》杂志-> 2007年第3期摘要 |
《贵金属》2007年第3期（总109期）摘要 郑雅杰，郭 伟，白 猛 摘 要：采用双氧水盐酸混合溶金制得氯金酸溶液，在氯金酸溶液中加入氯化钾蒸发结晶得到桔黄色氯金酸钾晶体。研究表明，5g金粉中加入5倍理论量的双氧水和盐酸，100℃下搅拌反应20min，得到氯金酸溶液，溶液中加入理论量氯化钾，搅拌蒸发结晶得到KAuCl4.2H2O晶体。热重差热(TG-DTA)实验结果表明，样品在25～431.68℃有2个明显吸热过程和1个连续失重过程。根据Ｘ射线衍射(XRD)实验，329℃时KAuCl4.2H2O热分解固体产物为KAuCl4，376℃时KAuCl4热分解固体产物为Au和KCl。 Preparation of Potassium Chloroaurate and Its Thermal Decomposition ZHENG Yajie, GUO Wei, BAI Meng Abstract：Potassium chloroaurate was prepared by evaporating and crystallizating
the chloroaurate acid solution after the addition of potassium chloride,
and the chloroaurate acid solution was produced through dissolution
of gold powders with hydrogen peroxide and hydrochloric acid. 5g gold
powders were dissolved completely at 100℃ and for 20min when HCl and
H2O2 were 5 times theoretical dosage, respectively. The optimum dosage
of KCl to HAuCl4 is a theoretical dosage. TG-DTA tests indicate that
the sample has two distinct heat absorption processes and one continuous
weight loss process from 25℃ to 431.68℃. XRD tests indicate that the
KAuCl4.2H2O decomposes to KAuCl4 at 329℃ and KAuCl4 decomposes to
KCl and Au at 376℃.
徐志广1,2，余日牛3，古国榜2，陈柱慧2 摘 要: 研究了合成亚砜BSO萃取Pd、Pt、Cu、Fe和Ni的性能。结果表明低酸度时，Pd2+几乎完全被萃取，其它金属的萃取率极低。钯易于从Pt、Cu、Fe和Ni金属中分离出来，且反萃容易。利用红外光谱研究了BSO萃取Pd和Pt的机理。低酸度时，在钯萃合物的红外光谱中，出现2个新的吸收峰(1122和931cm-1)，表明BSO通过硫和氧原子以中性配位机理萃取钯；高酸度时，没有新的红外吸收峰出现，表明BSO以离子缔合机理萃取钯。BSO以离子缔合方式萃取铂。 Study on Extraction Mechanism of Palladium and Platinum with Sulfoxide BSO XU Zhiguang1,2, YU Riniu3, GU Guobang2, CHEN Zhuhui2 Abstract: The extraction properties of palladium, platinum, copper,
iron and nickel with sulfoxide BSO were studied. The results show
that Pd2+ can be well extracted in 0.1mol/L [HCl] and is easily separated
from Pt4+, Cu2+, Fe3+ and Ni2+ by solvent extraction with synthetic
sulfoxide BSO. Furthermore, Pd2+ in organic phase is stripped by ammonium
chloride-ammonia solution in high effect. Mixed S and O coordination
is confirmed with two new peaks near 1122 and 931cm-1 at low acidity,
and ion-pair is formed at high acidity by IR spectrum of BSO Pd (II)
extraction complexes. Ion-pair extraction mode is also found in Pt4+
extraction with BSO at high acidity.
张杜超，杜新玲，杨天足，杜作娟，窦爱春 摘 要: 利用配位化学理论，研究了pH值、亚硫酸钠浓度、氯离子浓度对亚硫酸钠浸出氯化银的影响。结果表明：pH值的增大和亚硫酸钠浓度的提高，使与银配位的亚硫酸根离子增多，从而氯化银的溶解度明显提高；在亚硫酸钠循环浸出氯化银的过程中，溶液中不断积累的氯离子导致浸银效果逐渐变差。结合工业生产，确定了亚硫酸钠浓度为2mol/L，控制每次浸出液中银的浓度为30g/L时，亚硫酸钠溶液可以循环浸出氯化银11次。 Study on Leaching of Silver Chloride in Sodium Sulfite Solution Containing Chloride Ions ZHANG Duchao, DU Xinling, YANG Tianzu, DU Zuojuan,
Dou Aichun Abstract: The influences of pH value, concentrations of sodium sulfite
and chloride ion on leaching of silver chloride by sodium sulfite
were studied based on coordination equilibrium. The results show that
sulfite ion increases with pH value and concentration of sodium sulfite,
which results in the increase of solubility of silver chloride. In
the circular leaching solution, the solubility of silver chloride
becomes lower with the increase of concentration of chloride ion.
In industrial production, the solution can circularly leach silver
chloride 11 times when the concentration of sodium sulfite is 2mol/L
and the concentration of silver ion is 30g/L after every leaching
process.
徐 云1，郭迎春1，刘方方2，耿永红1，张昆华1 摘 要：研究了Ag-La2NiO4触点材料在直流阻性负载条件下的材料转移，以及接触电阻等电接触性能。实验结果表明：不同电压(DC
8V、DC 18V)、电流条件下，材料的转移方向、转移量及损耗均不同；DC 18V下接触电阻和熔焊力很不稳定，且随电流值增加有不同程度的波动。 Study on Arc Erosion of Ag-La2NiO4 Contact Materials XU Yun1, GUO Yingchun1, LIU Fangfang2, GENG Yonghong1, ZHANG Kunhua1 Abstract: The contact resistance and the material transfer of Ag-La2NiO4
contact materials was studied under the condition of different DC
and resistance load. The results indicate that the amount and the
direction of the material transfer are different with the change of
the voltage and the current: the transfer is from anode to cathode
as voltage DC 8V or DC 18V with current＞20A, and the transfer direction
is opposite as voltage DC 18V with current＜20A. The contact resistance
and the welding resistance force are unstable and change with the
current value.
董颖男, 董守安*, 唐 春 摘 要：研究了在可溶性聚合物体系中Pd纳米粒子的光化学合成。Pd(II)-PEG-丙酮溶液以紫外波长300nm光辐照，获得了胶体Pd纳米粒子并对其进行TEM表征。结果表明，Pd粒子的平均粒径为1.8～5.7nm，具有好的分散性。研究了各种组分的影响，探讨了体系中Pd(II)的快速光化学还原和纳米Pd粒子的稳定性机理。 Preparation of Pd Nanoparticles by Photochemical Method in Dissoluble Polymer System DONG Yingnan, DONG Shouan*, TANG Chun Abstract: The photochemical synthesis of Pd nanoparticles was studied
in dissoluble polymer system. Pd(II)-PEG-acetone solution was irradiated
by UV-300nm light and the colloidal Pd nanoparticles obtained were
characterized by TEM. The results show that Pd nanoparticles with
fine dispersion are 1.8nm to5.7 nm in average diameter. The influence
of PEG and acetone on the photochemical synthesis of Pd nanoparticles
was investigated, respectively. Rapid photochemical reduction of Pd(II)
ion and the mechanisms of stabilizing nanoparticles were discussed.
刘方方1,2，陈敬超2*，郭迎春3，耿永红3，管伟明3 摘 要：抗电弧侵蚀性能是衡量电接触材料好坏的一个重要指标。本文对采用反应合成技术制备的AgSnO2电接触材料进行电接触试验，并通过扫描电镜观察材料在电弧侵蚀后的形貌，对AgSnO2(10)材料在直流、阻性负载条件下的电弧侵蚀特征进行研究。结果表明，反应合成法制备的AgSnO2(10)电接触材料在电流≤20A条件下，材料由阴极向阳极转移；电流＞20A条件下，材料的转移方向反转。归纳出电弧侵蚀后的AgSnO2(10)的表面形貌特征。 Investigation on Arc Erosion Performances of AgSnO2 Electrical Contact Materials Fabricated by Reactive Synthesis LIU Fangfang1,2, CHEN Jingchao2*, GUO Yingchun3, GENG
Yonghong3, GUAN Weiming3 Abstract: The electrical contact tests were carried out for silver
tin oxide electrical contact materials which were fabricated by reactive
synthesis. The electrical erosion performances of AgSnO2(10) under
DC and resistance loads conditions were studied. The morphology of
AgSnO2(10) after arc erosion were investigated by means of scanning
electronic microscopy(SEM). The results indicated that the anode gains
mass when current value is less than 20A; and the anode losses mass
when current value is more than 20A. The surface morphologies of AgSnO2(10)
contacts were classified.
赵 宏1，尹福军1，许兴友1，王大雷1，徐正萍1，张 雯1，郑军伟2 摘 要：通过对玻璃基底的硅烷基化，金纳米粒子被组装到玻璃基底上，SEM表明金纳米粒子在玻璃基底上形成二维的亚单层组装结构。同时又利用聚苯乙烯模板对金纳米粒子进行图案化组装，在玻璃基底上形成“面包圈”结构。 Study on Assembly and Spectroscopy of Gold Nanoparticles ZHAO Hong1, YIN Fujun1, XU Xingyou1, WANG Dalei1,
XU Zhengping1, ZHANG Wen1, ZHENG Junwei2 Abstract: Gold nanoparticles were immobilized onto glass slide surfaces
by 3-mercaptoprophltrime-thoxy (MPTMS) silanization of the glass and
templating of polystyrene nanoparticles，forming long- range ordered
assembly structures. SEM characterization demonstrated that a two-dimensional
submonolayer of gold nanoparticles is formed on the MPTMS-silanized
substrate surface. In the case of polystyrene microsphere templating
assembly, gold nanoparticles are deposited in a patterned manner,
a doughnut-type assembled structure of the gold nanoparticles is formed
at the bottom of the ordered polystyrene nanoparticles.
陈 松，管伟明, 孔建稳，张昆华，邓德国 摘 要：为了克服传统Ir坩埚铸造研究中需占用大量Ir和资金的缺点，作者采用有限元方法计算了3种不同尺寸的Ir坩埚在铸造过程中的温度场变化特点。通过对计算结果的分析，有效地预测了缩孔在Ir坩埚壁出现的位置、浇口处缩孔的位置和形状等特点，同时给出了Ir坩埚底部中心处在凝固过程中的温度与时间关系的曲线。对于Ir坩埚实际铸造过程的工艺制定和优化具有指导作用。 Simulating Temperature Field during Iridium Crucible
Casting CHEN Song, GUAN Weiming, KONG Jianwen, ZHANG Kunhua,
DENG Deguo Abstract: In the present paper, the finite element method was used
to calculate casting iridium crucible temperature field of three samples.
The calculation results indicated that the method not only predicts
perfectly the location of shrinkage hole in the wall, but also predicts
the location and shape of shrinkage hole in the sprue of iridium crucible.
The time dependence of temperature in the center of the iridium crucible
bottom is given also. Those results are important for establishing
and optimizating the casting technology of iridium crucible.
摘 要：采用电化学和荧光方法研究了Pt(II) 水合物与甲胎蛋白(AFP)相互作用的机理，发现它们具有较强的相互结合能力。文中对Pt(II)-
AFP体系的适宜反应条件、影响因素及信号强度与AFP浓度的关系进行了研究。结果表明，在一定Pt(II)浓度范围内，AFP浓度与其荧光峰电流强度成正比。本方法有较高的灵敏度，对AFP的检出限为10.2ng/mL。考察了共存物质的干扰影响，并对实际血清样品中的AFP进行分析，结果满意。 Study on Interaction between Platinum and Alpha Fetoprotein
and GAN Ning, HOU Linxi, WANG Luyan, LI Tianhua, XU Weimin
Abstract: The reaction of aqueous platinum(II) hydrate with alpha
fetoprotein proteins(AFP) was studied by electrochemical and fluoremetry
method. The results show that Pt(II) can react with AFP strongly.
Therefore, a novel method for the determination of trace amounts of
AFP by fluoremetry method has been established. In the certain range
of Pt(II), the concentration of AFP is directly proportional to the
enhanced intensity of FL. The suitable reaction conditions, affecting
factors as well as the influence of some coexisting substances were
investigated. The method has high sensitivity, with the detection
limit of 10.2ng/mL for AFP protein and good selectivity. It was applied
to the determination of AFP in practical samples with satisfactory
results.
王娴婷，郭忠诚*，朱晓云
摘 要：本文论述了以银包玻璃微珠为导电相的低温聚合物导体浆料中树脂的选择实验，通过对所得浆料各种性能的比较，得到比较适合银包玻璃微珠的2种树脂A和F。适合的浆料配方是：35%～40%A树脂(TYI油墨类)配合使用60%～65%的导电相，30%～35%
F树脂(改性聚脂4#)配合使用65%～70%的导电相。把浆料样品放置72天，阻值变化率基本在10%以内。 Choice of Adhesives Used for Low Temperature Polymer Conductive Pastes WANG Xianting, GUO Zhongcheng*, ZHU Xiaoyun Abstract: The suitable resins for the low temperature polymer conductive
paste that uses the silver-plated glass beads as the electric conductive
phase were selected based on experimental results. It was found that
two kinds of A and F are suit for the silver-plated glass bead conductive
paste. The best composition of the conductive paste is: 60%~65% silver-plated
glass bead fixed with 35%~ 40% A resin or 65%~70% fixed with 30%~35%
F resin. For the pastes put in the air for 72 days, the resistance
changed less than 10%.
高传柱1,2，刘伟平1*，普绍平2 ,3，高文桂1 摘 要：根据目前临床使用的铂类抗癌药物的缺点和不足，作者报道了一种结构新颖的铂类配合物的合成方法，通过元素分析、质谱、红外、核磁共振氢谱等对合成物进行了结构表征，确认合成物为目标化合物。采用SRB比色法，测定的化合物对A549癌细胞及KB癌细胞的半数抑制浓度(IC50)分别为13.4mg/L和20.0mg/L。 Synthesis and Anticancer Activity of 3-benzyloxy-1,1-dicarboxycyclobutane GAO Chuanzhu1,2, LIU Weiping1*, PU Shaoping2,3, GAO
Wengui1 Abstract: Platinum-based drugs are one of the most important anticancer
drugs in clinical use. In this paper, a new platinum complex, 3- benzyloxy
-1,1-dicarboxycyclobutane diammine platinum(Ⅱ) was synthesized. Its
structure is confirmed by modern analytical techniques. IC50 of the
compound is 4.8mg/L for A549 tumor cells and 18.0mg/L for KB tumor
cells, respectively.
王 芳 摘 要：采用密度泛函理论中的广义梯度近似(DFT/GGA)方法，对Run团簇(n = 9~26)的几何结构与稳定性、团簇表面的Ru与内部Ru间相互作用进行了研究。结果表明：将金属团簇体系放大后，基态稳定结构的原子平均束缚能Eb随着团簇尺寸的增大而增大，当原子数n
= 26时，Eb = -6.69eV，与大块金属的Eb(-6.74eV)接近，表明其已接近大块金属的性质；Ru26的平均间距 = 2.65
?，与理论值2.70 ?和实验值2.704?相近；平均配位数CN随着n值的增大而增大，呈现收敛于块体值的趋势。另外，由于大块金属表面的原子不能与足够的原子配位形成饱和的配位结构，所以其上的电子向内层原子转移，使得内层Ru原子呈负电荷，而外层原子呈正电荷，最终导致内层原子之间的相互作用增强而导致键的收缩，外层原子之间键的减弱，从而出现所谓的“驰豫效应”。 Density Functional Study on Run (n = 9～26) Metal Clusters WANG Fang( Chemistry Department, Shaanxi Institute of Education, Xi’an, Shaanxi 710061, China ) Abstract: In this paper, the geometry, stability, interaction between
surface and inner Ru atom of Run clusters are investigated by Density
Functional Theory (DFT). The average atom binding energy increases
with the increase of the atom number for magnified metal clusters.
When n = 26, the binding energy which is comparable to that of bulk
metals(-6.74eV) is -6.69eV, which indicates that the binding energy
approaches to the property of bulk metals; The average bond distance
is 2.65?, which is close to theoretic(2.70?) and experimental values(2.70?);
The average coordination number(CN) presents the trend of convergence
to bulk metals. The lack of coordinative saturation for the exterior
atoms of the cluster implies that some electrons, which in the bulk
metal would be involved in bonding interactions with atoms that are
absent in the cluster, are free to migrate to the central atom, which
make the central Ru atoms have negative effective charges and surface
Ru atoms have positive charge in all clusters, results in the appearance
of relaxation effect.
朱利亚1，陈云江1，赵 辉1，赵忆宁2，黄章杰3，杨光宇3，朱武勋1 摘 要：提出了微波密闭快速消解Pt(NH3)2(NO2)2、Pt(NH3)2Cl2、Pt(NH3)4Cl2、 (NH4)2PtCl6、K2PtCl4难分解化合物的新方法；优化了KMnO4电流滴定法测定Pt(Ⅳ)的条件；比较了本法与氯铂酸铵重量法、水合肼还原重量法、烘箱罐消解电流滴定法；同时，将精密电流滴定法应用于PtCl4、Na2PtCl6、K2PtCl6、H2PtCl4化合物中Pt(Ⅳ)含量的测定。结果表明：测定37%~65%的Pt(Ⅳ)含量，本法、氯铂酸氨重量法、水合肼还原重量法的相对平均误差分别为-0.14%~+0.13%、-0.21%~+0.21%、-0.13%~+0.14%，相对标准偏差分别为0.05%~0.08%、0.11%~0.14%、0.08%~0.09%，故本法的准确度和精密度与水合肼还原重量法的基本一致，较氯铂酸氨重量法的略好；但本法消解快速、节能、安全，操作简便，对环境污染程度小，适宜推广运用。 Determination of Platinum Content in Platinum Compounds
Using Microwave ZHU Liya1, CHEN Yunjiang1, ZHAO Hui1, ZHAO Yining2,
HUANG Zhangjie3, Abstract: A microwave-assisted sealing digestion method for determination
of platinum in difficultly decomposed compounds of Pt(NH3)2(NO2)2,
Pt(NH3)2Cl2, Pt(NH3)4Cl2, (NH4)2PtCl6 and K2PtCl4 is proposed. The
condition for determination of platinum (Ⅳ) with KMnO4 micro electricity
titration was optimized. The proposed method was compared with traditional
gravimetric analysis and oven-heating analysis. At the same time,
the platinum (Ⅳ) in compounds of PtCl4, Na2PtCl6, K2PtCl6 and H2PtCl4
was also determined under optimal conditions. Experimental results
showed that the relative average error of the proposed method, the
hydrazine hydrate gravimetry and the ammonium chloroplatinate gravimetry
is -0.14%~+0.13%, -0.21%~+0.21% and -0.13%~+0.14%, respectively, and
the relative standard deviation of three methods is 0.05%~0.08%, 0.11%~0.14%
and 0.08%~0.09%, respectively, for Pt content from 37% to 65%. Therefore,
the accuracy and precision of the proposed method are almost the same
with hydrazine hydrate gravimetry, and are a little better than ammonium
chloroplatinate gravimetry. But it is rapid, economic, secure, easy
to operate and environmental friendly.
赵宇侠，许兴友，马卫兴，张秋容，陈文宾 摘 要：研究了在CTMAB存在下，Au(Ⅲ)与氯磺酚偶氮硫代若丹宁的显色反应，实验表明，在pH = 3.0的盐酸溶液中，Au(Ⅲ)与试剂形成1∶2的橘黄色络合物，其λmax
= 460 nm，? = 1.52×105 L?mol-1?cm-1。Au(Ⅲ)含量在0～14 ?g/10mL符合比尔定律。本法用于金矿石中微量金的测定，结果满意。 Determination of Trace Gold by Spectrophotometric Method with HSCT ZHAO Yuxia，XU Xingyou，MA Weixing，ZHANG Qiurong，CHEN
Wenbin Abstract: The colour reaction of the reagent O-hydroxybenzenediazoaminoazobenzene
with Au(Ⅲ) in the presence of CTMAB was studied. Results show that
the new colour reagent reacts with Au(Ⅲ) to form a stable red complex(1﹕2)
in the presence of HCl buffer at pH 3.0. The maxium absorption wavelength
and apparent molar absorptivity are 460nm and 1.52×105 L?mol-1?cm-1,
respectively. Beer?s law is obeyed in the range of 0～14?g/10mL Au(Ⅲ).
The method has been applied to the determination of trace gold with
satisfactory results.
李光俐，王应进，朱武勋 摘 要：试样用HNO3与HCl溶解，ICP-AES法直接测定富银渣中0.01%～5%的Ag、Au、Cu、Ni、Sb、Bi、Zn、Al、As、Sn等元素。研究了溶剂、试样中铅及其它共存元素的干扰，选择了合适的分析线。加标回收率在99.6%～107.1%，相对标准偏差为0.59%～3.08%，方法准确、简便、快速。 Analysis of Rich Ag Residue by ICP-AES Technology LI Guangli, WANG Yingjin, ZHU Wuxun Abstract: The samples were dissolved in HNO3-HCl. The ICP-AES method
was used to determine directly Ag, Au, Cu, Ni, Sb, Bi, Zn, Al, As,
Sn in the rich Ag residue. The interference from Pb and other coexisting
elements was investigated, and the optimum analyzing bands were selected.
The standard recovery rates are from 99.6% to 107.1%, The relative
standard derivation of 0.59% to 3.08% is reached. The method is accurate,
simple and rapid.
Stephen Cooke, Algis Naujokas, James Lynn Abstract: The industry procedures for analysis of spent noble metals
bearing catalysts, including the fire assay collection and acid leaching,
and their advantages and disadvantages were introduced. The quality
control procedures were discussed in detail. They consist of three
levels of quality control for the analysis of spent noble metals bearing
catalysts: the method quality control, the sample specific quality
control and the instrumental quality control. A flow chart detailing
both fire assay and leach was given. 含贵金属废催化剂的分析 Stephen Cooke, Algis Naujokas, James Lynn 摘 要: 介绍了含贵金属废催化剂的工业分析方法，包括试金和湿法浸出分析法及其优缺点，详细地讨论了分析过程中的三级质量控制，包括方法质量控制、样品质量控制及仪器质量控制。给出了试金分析及湿法浸出分析原则流程图。
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