己基苯并咪唑硫醚树脂固相萃取钯

合成萃取剂己基苯并咪唑硫醚(HBMS),对其分子结构进行分析,并将其制备成HBMS树脂,研究该树脂萃取钯的性能;考察H+浓度对萃取钯的影响。结果表明:在低酸度条件下,利用HBMS树脂可实现铂、钯的分离。紫外-可见吸收光谱、红外吸收光谱研究结果表明:盐酸介质中HBMS树脂萃取Pd(Ⅱ)的机理为配位取代。萃合物的晶体结构表明:培养出的HBMS-Pd(Ⅱ)萃合物单晶中的HBMS通过苯并咪唑基上的氮原子与Pd(Ⅱ)直接配位,萃合物以钯原子为中心呈完全对称平面正方型构型,萃合物的组成为nPd(Ⅱ):nHBMS=1:2。     

钯(Ⅱ)碘络合物在丙醇-硫酸铵双水相萃取体系中的分配行为及在钯测定中的应用

研究了Pd(Ⅱ)碘络合物在丙醇-硫酸铵双水相萃取体系中的分配行为,在HCl介质中,碘化铵存在下,Pd(Ⅱ)能形成离子缔合物[PdI42-.(PrOH2 )2]从而被萃入丙醇相.获得了最佳萃取条件,结果表明本方法能定量萃取Pd(Ⅱ),在最佳萃取条件下,Pd(Ⅱ)的萃取率可达99.2%.合成样的分离结果表明,本方法可应用于从大量基体金属如Fe2 、Ca2 、Mg2 、Mn2 、Al3 、Pb2 和Zn2 中分离Pd(Ⅱ).对从废碳钯催化剂中Pd的回收也进行了试验,结果与火试金法相符.     

盐酸介质中异戊基苯并噻唑亚砜萃取Pd(Ⅱ)的机理

合成了异戊基苯并噻唑亚砜(ABSO),研究了盐酸介质中ABSO萃取Pd(Ⅱ)的机理。考察水相H 浓度和萃取剂浓度对钯萃取的影响,采用斜率法、红外光谱和核磁共振H谱法确定了萃合物的组成及萃取平衡的机理。结果表明:低酸度条件下,H 浓度对钯的分配比无影响,ABSO以中性配位萃取机理萃取Pd(Ⅱ),并通过苯并噻唑环上的氮原子与Pd(Ⅱ)配位形成萃合物PdCl2(ABSO)2。     

Pd（Ⅱ）—4‘—磺胺偶氮氯膦光度法及分离法的研究和应用

1.前言 4'-磺胺偶氮氯膦(简称4'-SMCP)是一种不对称偶氮氯膦类试剂,由于它与稀土元素有较好的络合能力,因此经常做为稀土元素的显色剂.有人曾利用4'-SMCP做为显色剂测定稀土元素.本文研究了4'-SMCP与Pd(Ⅱ)的分光光度行为,实验发现在酸性介质中(>0.1MHNO_3),4'-SMCP与Pd(Ⅱ)于624nm处有最大吸收,ε=5.1×10~4L·mol~(-1)·cm~(-1).钯含量在55μg/ml以下符合比尔定律,最低检测限1μg/25ml(0.04ppm).络合物的摩尔比为Pd∶4'-SMCP=1∶2,络合物表观稳定常数约7.2×10~(11). Pd(Ⅱ)与其它元素的分离和富集多采用萃取法,也有人曾用阳离子交换树脂分离Pd(Ⅱ),但高价阳离子与之分离有一定困难.本文研究了Pd(Ⅱ)于阴离子交换树脂     

不对称亚砜BSO萃取钯的性能及机理研究

研究了不对称亚砜BSO从盐酸介质中萃取钯的性能和机理,结果表明:待萃液Pd(Ⅱ)浓度为1.0g.L-1,HCl浓度为0.1mol.L-1,用0.3mol.L-1BSO-煤油按相比1:1混合萃取Pd(Ⅱ),经过5min的萃取振荡时间,萃取率可达99.8%。通过斜率法和红外光谱分析表明,在低酸度([H+]≤0.3mol.L-1)下,亚砜主要以中性溶剂络合萃取机理萃取钯,萃合物组成为[PdCl2.2BSO](0);在高酸度(1.0≤[H+]≤4.0mol.L-1)下,亚砜以离子缔合萃取机理萃取钯,萃合物组成可能为[H+.hH2O.(BSO)2]2.[PdCl42-](0)。     

石油亚砜Ⅱ（2）萃Pd（Ⅱ）机理的研究

研究在盐酸介质中石油亚砜Ⅱ(2)萃Pd(Ⅱ)的机理,并分析水相中影响(Ⅱ)萃取的主要因素及其原因,考察不同盐酸浓度下亚砜的萃合方式,盐酸浓度的萃钯(Ⅱ)实验曲线及其对贵金属萃取分离的意义,还测定了萃合物组成.     

吐温80—达旦黄分光光度法测定微量钯

1.前言在非离子表面活性剂吐温80存在下,达旦黄—Pd(Ⅱ)的络合物可用于测定微量 Pd(Ⅱ)。在 pH10.5～12.0的碱性溶液中,络合物最大吸收波长为475～480纳米,表观摩尔吸光系数为ε_(480)=1.05×10~5。络合物在15分钟内发色完全,4小时内吸光度稳定不变。Pd(Ⅱ)含量在0～20微克/50毫升范围内符合比尔定律。测定了 Pd(Ⅱ)和达旦黄的     

钯(II)碘络合物在丙醇-硫酸铵双水相萃取体系中的分配行为及在钯测定中的应用(英文)

研究了 Pd(II)碘络合物在丙醇-硫酸铵双水相萃取体系中的分配行为,在 HCl 介质中,碘化铵存在下,Pd(II)能形成离子缔合物[PdI42-·(PrOH2+)2]从而被萃入丙醇相。获得了最佳萃取条件,结果表明本方法能定量萃取 Pd(II),在最佳萃取条件下,Pd(II)的萃取率可达 99.2%. 合成样的分离结果表明,本方法可应用于从大量基体金属如 Fe2+、Ca2+、Mg2+、Mn2+、Al3+、Pb2+和 Zn2+中分离 Pd(II)。对从废碳钯催化剂中 Pd 的回收也进行了试验,结果与火试金法相符。     

合成亚砜BSO萃取分离钯铂的性能研究

对合成亚砜BSO萃取Pd(Ⅱ)、Pt(Ⅳ)性能的研究表明,在不同酸度下BSO对Pd(Ⅱ)均有优异的萃取性能,而只有在高酸度介质里BSO对Pt(Ⅳ)有较高的萃取能力.在低酸度下利用BSO对Pd(Ⅱ)、Pt(Ⅳ)萃取性能的差异,能很好地萃取分离Pd(Ⅱ)、Pt(Ⅳ);也可以在高酸度下共萃Pd(Ⅱ)、Pt(Ⅳ),再利用水反萃Pt(Ⅳ),达到分离Pd(Ⅱ)、Pt(Ⅳ)的目的.     

纤维状材料对模拟高放废液中钯的吸附行为

为从高放废液中分离富集钯Pd(Ⅱ),考察纤维状吸附材料Smopex~?-102 FG对Pd(Ⅱ)的静态吸附行为,研究HNO_3浓度、接触时间、初始金属离子浓度、温度对Pd(Ⅱ)吸附行为的影响,并考察吸附过程的动力学和热力学。结果表明:在研究条件下,Smopex~?-102 FG对Pd(Ⅱ)的吸附分配系数Kd随HNO_3浓度的减小而逐渐增加,在HNO_3浓度为0.001 mol/dm~3时,分配系数Kd为142.0 cm~3/g。Smopex~?-102 FG吸附Pd(Ⅱ)的动力学过程迅速,20 min即达到平衡状态,且平衡吸附率(R)皆在70%以上,吸附动力学符合拟一阶和拟二阶动力学模型,理论平衡吸附量与实验值(Q_e=19.82 mg/g)基本吻合。Weber-Morris粒内扩散模型表明,Pd(Ⅱ)在纤维状吸附材料Smopex~?-102 FG的表面和颗粒内的扩散共同控制吸附速率。与此同时,随着初始金属离子浓度的增大,Smopex~?-102 FG对Pd(Ⅱ)的平衡吸附量呈线性增加,而其对Pd(Ⅱ)的吸附率却随之减小,吸附过程遵循Freundlich等温吸附模型,为优惠吸附。从热力学实验结果可知,该吸附是自发吸热过程,温度升高有利于吸附过程的进行。静态吸附实验表明,纤维状吸附材料Smopex~?-102 FG对钯离子表现出良好的吸附性能,是一种适用于处理高放废液中Pd(Ⅱ)的吸附材料。     

Effects of Post-weld Heat Treatment on Microstructure,Mechanical Properties and the Role of Weld Reinforcement in 2219 Aluminum Alloy TIG-Welded Joints

In as-welded state, each region of 2219 aluminum alloy TIG-welded joint shows diff erent microstructure and microhardness due to the diff erent welding heat cycles and the resulting evolution of second phases. After the post-weld heat treatment, both the amount and the size of the eutectic structure or θ phases decreased. Correspondingly, both the Cu content in α-Al matrix and the microhardness increased to a similar level in each region of the joint, and the tensile strength of the entire joint was greatly improved. Post-weld heat treatment played the role of solid solution strengthening and aging strengthening. After the post-weld heat treatment, the weld performance became similar to other regions, but weld reinforcements lost their reinforcing eff ect on the weld and their existence was more of an adverse eff ect. The joint without weld reinforcements after the post-weld heat treatment had the optimal tensile properties, and the specimens randomly crack in the weld zone.     

The First Phase of the SRIF Industrialized Base in ＂West Area＂ Has Been Put into Operation

After nearly two years＇ tense construction, the first phase of industrialized base of Shenyang Research Institute of Foundry （SRIF）, located at the Tiexi Casting and Forging Industrial Park in the west of Tiexi District, has now been completed and formally put into operation.     

Thermodynamics Study on the Decomposition of Chromite with KOH

Institute of Process Engineering, Chinese Academy of Sciences, China, has proposed a method for oxidative leaching of chromite with potassium hydroxide. Understanding the mechanism of chromite decomposition, especially in the potassium hydroxide fusion, is important for the optimization of the operating parameters of the oxidative leaching process. A traditional thermodynamic method is proposed and the thermal decomposition and the reaction decomposition during the oxidative leaching of chromite with KOH and oxygen is discussed, which suggests that chromite is mainly destroyed by reactions with KOH and oxygen. Meanwhile, equilibrium of the main reactions of the above process was calculated at different temperatures and oxygen partial pressures. The stable zones of productions, namely, K2CrO4 and Fe2O3, increase with the decrease of temperature, which indicates that higher temperature is not beneficial to thermodynamic reactions. In addition, a comparison of the general alkali methods is carried out, and it is concluded that the KOH leaching process is thermodynamically superior to the conventional chromate production process.     

Influence of Heat Treatment on Damping Behaviour of the Magnesium Wrought Alloy AZ61

The effect of isochronal heat treatments for 1h on variation of damping, hardness and microstructural change of the magnesium wrought alloy AZ61 was investigated. Damping and hardness behaviour could be attributed to the evolution of precipitation process. The influence of precipitation on damping behaviour was explained in the framework of the dislocation string model of Granato and Lücke.     

Effect of Rare Earth Doping on Impedance,Modulus and Conductivity Properties of Multiferroic Composites:0.5(BiLa_xFe_(1-x)O_3)–0.5(PbTiO_3)

The Lanthanum-doped bismuth ferrite–lead titanate compositions of 0.5(Bi LaxFe1-xO3)–0.5(Pb Ti O3)(x = 0.05,0.10,0.15,0.20)(BLxF1-x-PT) were prepared by mixed oxide method.Structural characterization was performed by X-ray diffraction and shows a tetragonal structure at room temperature.The lattice parameter c/a ratio decreases with increasing of La(x = 0.05–0.20) concentration of the composites.The effect of charge carrier/ion hopping mechanism,conductivity,relaxation process and impedance parameters was studied using an impedance analyzer in a wide frequency range(102–106Hz) at different temperatures.The nature of Nyquist plot confirms the presence of bulk effects only,and non-Debye type of relaxation processes occurs in the composites.The electrical modulus exhibits an important role of the hopping mechanism in the electrical transport process of the materials.The ac conductivity and dc conductivity of the materials were studied,and the activation energy found to be 0.81,0.77,0.76 and 0.74 e V for all compositions of x = 0.05–0.20 at different temperatures(200–300 °C).     

Quantitative Analysis of the Crystallographic Orientation Relationship Between the Martensite and Austenite in Quenching–Partitioning–Tempering Steels

The orientation relationships(ORs)between the martensite and the retained austenite in low-and medium-carbon steels after quenching–partitioning–tempering process were studied in this work.The ORs in the studied steels are identified by selected-area electron diffraction(SAED)as either K–S or N–W ORs.Meanwhile,the ORs were also studied based on numerical fitting of electron backscatter diffraction data method suggested by Miyamoto.The simulated K–S and N–W ORs in the low-index directions generally do not well coincide with the experimental pole figure,which may be attributed to both the orientation spread from the ideal variant orientations and high symmetry of the low-index directions.However,the simulated results coincide well with experimental pole figures in the high-index directions{123}_(bcc).A modified method with simplicity based on Miyamoto’s work was proposed.The results indicate that the ORs determined by modified method are similar to those determined by Miyamoto’method,that is,the OR is near K–S OR for the low-carbon Q–P–T steel,and with the increase of carbon content,the OR is closer to N–W OR in medium-carbon Q–P–T steel.     

Using Finite Element and Contour Method to Evaluate Residual Stress in Thick Ti-6Al-4V Alloy Welded by Electron Beam Welding

This work was to reveal the residual stress profile in electron beam welded Ti-6Al-4V alloy plates(50 mm thick) by using finite element and contour measurement methods.A three-dimensional finite element model of 50-mmthick titanium component was proposed,in which a column–cone combined heat source model was used to simulate the temperature field and a thermo-elastic–plastic model to analyze residual stress in a weld joint based on ABAQUS software.Considering the uncertainty of welding simulation,the computation was calibrated by experimental data of contour measurement method.Both test and simulated results show that residual stresses on the surface and inside the weld zone are significantly different and present a narrow and large gradient feature in the weld joint.The peak tensile stress exceeds the yield strength of base materials inside weld,which are distinctly different from residual stress of the thin Ti-6Al-4V alloy plates presented in references before.     

Microstructures and Tensile Properties of Ultrafine-Grained Ni–(1–3.5) wt% SiC_(NP) Composites Prepared by a Powder Metallurgy Route

Silicon carbide nanoparticle-reinforced nickel-based composites(Ni–Si CNP),with a Si CNPcontent ranged from1 to 3.5 wt%,were prepared using mechanical alloying and spark plasma sintering.In addition,unreinforced pure nickel samples were also prepared for comparative purposes.To characterize the microstructural properties of both the unreinforced pure nickel and the Ni–Si CNPcomposites transmission electron microscopy(TEM) was used,while their mechanical behavior was investigated using the Vickers pyramid method for hardness measurements and a universal tensile testing machine for tensile tests.TEM results showed an array of dislocation lines decorated in the sintered pure nickel sample,whereas,for the Ni–Si CNPcomposites,the presence of nano-dispersed Si CNPand twinning crystals was observed.These homogeneously distributed Si CNPwere found located either within the matrix,between twins or on grain boundaries.For the Ni–Si CNPcomposites,coerced coarsening of the Si CNPassembly occurred with increasing Si CNPcontent.Furthermore,the grain sizes of the Ni–Si CNPcomposites were much finer than that of the unreinforced pure nickel,which was considered to be due to the composite ball milling process.In all cases,the Ni–Si CNPcomposites showed higher strengths and hardness values than the unreinforced pure nickel,likely due to a combination of dispersion strengthening(Orowan effects) and particle strengthening(Hall–Petch effects).For the Ni–Si CNPcomposites,the strength increased initially and then decreased as a function of Si CNPcontent,whereas their elongation percentages decreased linearly.Compared to all materials tested,the Ni–Si CNPcomposite containing 1.5% Si C was found more superior considering both their strength and plastic properties.     

Directional Growth of Tin Crystals Controlled by Combined Solute Concentration Gradient Field and Static Magnetic Field

A new method was introduced to achieve directional growth of Sn crystals. Microstructures in liquid(Pb)/liquid(Sn) diffusion couples were investigated under various static magnetic fields. Results show that the β-Sn crystals mainly reveal an irregular dendritic morphology without or with a relatively low static magnetic field(B0.3 T). When the magnetic field is increased to 0.5 T, the β-Sn dendrites close to the final stage of growth begin to show some directional character. With a further increase in the magnetic field to a higher level(0.8–5 T), the β-Sn dendrites have an enhanced directional growth character, but the dendrites show a certain deflection. As the magnetic field is increased to 12 T, the directional growth of the β-Sn dendrites in the center of the couple is severely destroyed. The mechanism of the directional growth of the β-Sn crystals and the deflection of the β-Sn crystals with the application of static magnetic field was tentatively discussed.     

电化学噪声数据处理方法概述

综述了常见的电化学噪声数据处理方法,介绍了直流趋势剔除、统计分析、快速傅立叶变换(FFT)法计算功率谱密度(PSD)以及小波变换处理电化学噪声信号的基本过程,并阐释了各种数学处理及所得参数的物理意义。