镍-铁合金镀液中硼酸分析方法的改进

用传统方法分析镍-铁合金镀液中的硼酸,亚铁离子严重影响测定结果。用亚铁氰化钾沉淀分离镀液中的亚铁离子和镍离子,用甘露醇与硼酸反应生成酸性较强的络合酸,以酚酞作指示剂,用氢氧化钠标准滴定溶液滴定。实验表明,测定结果的平均偏差为0.20%,回收率为98.2%～101.2%。本法准确、简单,优于其它方法。     

镍铁镀液硼酸含量分析中的几个问题

镍铁合金镀液是近年来发展较快的镀种之一,许多电镀厂家的镍铁镀液都是从原来的亮镍镀液转化过来.同样地,镍铁镀液中的硼酸含量分析也可以仿照亮镍镀液中的硼酸分析方法进行.笔者采用快速法之一,即用柠檬酸钠络合镍、用丙二醇和硼酸生成络合酸、以酚酞为指示剂、用碱滴定的方法,经对照验证,总结以下几点,供同行参考:一、关于滴定终点的颜色亮镍镀液中硼酸分析的滴定颜色变化是由淡绿色变灰蓝色为终点.而在镍铁镀液中,由于铁离子的影响,颜色的变化是淡绿—草黄—黄中略见红色为终点.     

酸性锌镍合金镀液中镍、锌和硼酸的分析方法

制定了酸性锌镍合金镀液中镍、锌和硼酸的分析方法。用EDTA光度法测定镍;用EDTA容量法测定锌和镍的总量,用差减法计算锌的质量浓度;用甘露醇与硼酸反应生成酸性较强的络合酸,用亚铁氰化钾掩蔽锌和镍离子,以酚酞作指示剂用氢氧化钠滴定硼酸。这三种方法的准确度都较高,能够满足镀液中锌、镍和硼酸的监控要求。     

镍-钴合金镀液中硼酸的快速分析

0 前言 镍-钴合金镀液中硼酸的分析,目前采用的是沉淀分离法[1].用强碱使镍离子和钴离子生成氢氧化物沉淀,过滤后用硫酸酸化试液,以甲基红为指示剂,用碱中和过量的硫酸;在甘露醇存在的条件下,以酚酞作指示剂,用碱滴定硼酸.     

镀镍溶液中硼酸的分析方法

制定了测定镀镍溶液中硼酸的新方法。用草酸钾掩蔽镀液中的镍离子和镀液中铁杂质及锌杂质离子,用氟化钠掩蔽铝杂质离子,用甘露醇与硼酸反应生成酸性较强的配合酸,用酚酞作指示剂,以氢氧化钠滴定法测定配合酸。实验表明,本法的相对平均偏差为0.2%,回收率为99.62%,精密度和回收率都较高。     

不含铵盐的三价铬镀液中硼酸的分析

研究了不含铵盐的三价铬镀液中硼酸的分析方法。用草酸钾掩蔽三价铬,在弱酸性条件下草酸钾与三价铬离子生成络合物。用甘露醇与硼酸反应生成较强的络合酸,以酚酞作指示剂,用氢氧化钠标准滴定溶液滴定。镀液中的其它组分对测定无影响,分析结果的相对平均偏差为0.17%。     

钢铁电抛光溶液中硫酸和磷酸的连续测定方法

研究了在测定钢铁电抛光溶液中硫酸和磷酸时所用的掩蔽剂,以甲基橙作指示剂,用氢氧化钠标准滴定溶液滴定硫酸和磷酸的总量,然后向试液中加亚铁氰化钾掩蔽亚铁离子,以酚酞作指示剂,继续用氢氧化钠标准滴定溶液滴定磷酸二氢根。该方法能有效消除亚铁离子对测定结果的影响,明显优于其它分析方法。     

钢铁电抛光溶液中硫酸和磷酸测定方法的改进

用氢氧化钠滴定法测定钢铁电抛光溶液中硫酸和磷酸的含量时,抛光溶液中的二价铁离子影响磷酸二氢根的测定。以甲基橙作指示剂,用氢氧化钠滴定硫酸和磷酸的总量,然后向试液中加入柠檬酸钠掩蔽铁离子,继续用氢氧化钠滴定至酚酞指示剂变为红色,从而测得磷酸二氢根的含量。该方法有效地消除了二价铁离子对测定的干扰。     

镀钴溶液中硼酸的快速分析

研究了镀钴溶液中硼酸的快速分析方法。用亚铁氰化钾沉淀钴离子,消除钴对测定硼酸的干扰,用甘露醇与硼酸反应生成较强的络合物,以酚酞作指示剂,用氢氧化钠标准溶液滴定。实验表明,本法测定结果的相对平均偏差为0.29%。方法简单、快速,能够满足监控镀钴溶液中硼酸的要求。     

含铵盐的硫酸盐三价铬镀铬液中硼酸的测定

制定了测定含铵盐的硫酸盐三价铬镀铬液中硼酸的方法。用柠檬酸钠掩蔽三价铬离子和镍杂质,用甘露醇与硼酸反应生成较强的配合酸。以变色pH范围为6.8～8.4的酚红作为指示剂,用氢氧化钠标准溶液滴定配合酸,避免了硫酸铵对测定硼酸的影响。测定结果的相对平均偏差为0.28%,回收率为99.34%～100.46%。     

电白槽液中磷酸氢二钠和碳酸纳的分析

介绍了电白槽液中磷酸氢二钠和碳酸钠的分析方法。用磷钼蓝光度法测定电白槽液中磷酸氢二纳的质量浓度,用过硫酸铵破坏氰化物,消除其对测定的干扰。在硫酸介质中,以抗坏血酸作还原剂,硝酸铋作催化剂,使磷酸与钼酸钠生成杂多酸蓝色络合物,以显色剂作参比液,在波长660nm处测定吸光度。试验表明,镀液中的铜离子和其它组份对测定无影响,本法相对平均偏差为1.3%,回收率为97.3%-103%。用硝酸银掩蔽氰化钠,以酚酞作指示剂,用盐酸滴定法直接测定电白槽液中碳酸钠的质量浓度。试验表明,镀液中的Na2[Sn(CN)4]、Na2[Cu(CN)2]和磷酸氢二钠对测定无干扰,本法相对平均偏差为0.54%,回收率为101%。而用传统的铜锡合金镀液分析方法,电白槽中的磷酸氢二钠严重影响碳酸钠的测定。     

Copper electrodeposition from an acidic plating bath containing accelerating and inhibiting organic additives

Copper electrodeposition on copper from still plating solutions of different compositions was investigated utilising electrochemical impedance spectroscopy (EIS), cyclic voltammetry, and scanning electron microscopy (SEM). An acid copper sulphate plating base solution was employed either with or without sodium chloride in the presence of a single additive, either polyethylene glycol (PEG) or 3-mercapto-2-propanesulphonic acid (MPSA), and their mixture. Thallium underpotential deposition/anodic stripping was employed to determine the adsorption capability of additives on copper. In the absence of chloride ions, MPSA shows a moderate adsorption on copper, whereas PEG is slightly adsorbed. At low cathodic overpotentials, the simultaneous presence of MPSA and chloride ions accelerates copper electrodeposition through the formation of an MPSA-chloride ion complex in the solution, particularly for about 220 μM sodium chloride. The reverse effect occurs in PEG-sodium chloride plating solutions. In this case, from EIS data the formation of a film that interferes with copper electrodeposition can be inferred. At higher cathodic overpotentials, when copper electrodeposition is under mass transport control, the cathode coverage by a PEG-copper chloride-mediated film becomes either partially or completely detached as the concentration of chloride ions at the negatively charged copper surface diminishes. The copper cathode grain topography at the μm scale depends on the cathodic overpotential, plating solution composition and average current density. Available data about the solution constituents and their adsorption on copper make it possible to propose a likely complex mechanism to understand copper electrodeposition from these media, including the accelerating effect of MPSA and the dynamics of PEG-copper chloride complex adsorbate interfering with the surface mobility of depositing copper ad-ions/ad-atoms.     

分析酸性镀锌溶液中硼酸含量掩蔽剂的选择

目前,测定酸性镀锌溶液中硼酸的方法有几种,不同方法测定结果的差异较大,有些方法的误差是不能允许的。实验表明,不能用柠檬酸钠和EDTA-Na_2掩蔽锌离子。但是,用草酸钠或亚铁氰化钾掩蔽锌离子,能够消除锌离子对测定硼酸的干扰。用甘露醇与硼酸反应生成较强的络合酸,以酚酞作指示剂,用氢氧化钠标准溶液滴定。本法准确度较高,能够满足监控酸性镀锌溶液中硼酸的要求。     

Interaction of gossypol with the ferrous ion

Summary The preparation of a solution of sodium gossypolate in aqueous acetone has been described. Indications of a 1∶1 mole ratio combination of the gossypolate and ferrous ions were established through conductometric and potentiometric studies in the presence of either chloride or perchlorate anion. Application of the method of continuous variations to differences in the absorption spectra of the two species confirmed the 1∶1 mole ratio of ferrous ion to gossypol. This finding is supported by analytical data. Values of pK for the dissociation constant of ferrous gossypolate, calculated from spectrophotometric measurement, averaged 7.3. Since the peri-hydroxyls are the most plausible location of the sodium ions in sodium gossypolate, its reaction with ferrous ion results in displacement of the two sodium ions by the ferrous ion. Findings reported in this paper were included in a thesis submitted to Tulane University by Robert J. Demint in partial fulfillment of the requirements for the M.S. degree. One of the laboratories of the Southern Utilization Research Branch, Agricultural Research Service, U. S. Department of Agriculture.     

铝材表面化学镀镍技术

在常规铝材化学镀镍工艺基础上，提出一种在酸性化学镀镍前增加一道碱性化学预镀镍工艺的铝材表面化学镀镍新技术。介绍了其预镀镍的工艺流程与操作要点。研制了一种中等浓度的含镍、铁的多元合金浸锌液，并通过正交实验得出了浸锌最佳方案，确定了碱性化学预镀镍的最佳配方：25g／L硫酸镍，25g/L次磷酸钠，30g／L柠檬酸三钠，10g／L焦磷酸钠，10-15mL／L三乙醇胺，30g/L氯化铵。弯曲试验表明，镀镍层与铝基体结合强度很高；镀镍层SEM照片显示，镀镍层晶粒尺寸大小均匀，各晶粒间结合紧密，孔隙率低，耐腐蚀能力强。     

工业次氯酸钠溶液中氯酸钠含量的测定

利用次氯酸钠和氯酸钠的氧化能力不同,以双氧水消解次氯酸钠的影响,以硫酸中和次氯酸钠溶液中的氢氧化钠,以硫酸亚铁作还原剂,将试样中的氯酸钠还原,再用重铬酸钾标准溶液氧化过量的硫酸亚铁,从而测定工业次氯酸钠溶液中氯酸钠的准确浓度.方法简单可靠,测得的回收率高,检测极限（质量浓度）可达0.05g/L以下.     

光亮镀镍液中硼酸和氯化镍的连续滴定

介绍一种光亮镀镍液中硼酸和氯化镍的测定方法。采用732型阳离子交换树脂分离镍及其它阳离子后，分别用氢氧化钠和硼酸银滴定硼酸和氯离子，分析结果表明，本方法简便快速、准确度高。     

三价铬钝化废水处理工艺的开发

研究开发了不同三价铬钝化废水的处理工艺。处理含有羧酸类配位剂(不包括氨基乙酸)的三价铬钝化废水时,在碱性条件下用亚铁离子和钙离子共同沉淀羧酸配位剂,重金属离子生成氢氧化物沉淀。处理只含氢氟酸一种配位剂的三价铬钝化废水时,用氢氧化钙沉淀氟离子和重金属离子。处理含有羧酸和氢氟酸配位剂的三价铬钝化废水,或含有氨基乙酸配位剂的三价铬钝化废水时,在碱性条件下用二甲基二硫代氨基甲酸钠螯合剂、亚铁离子和钙离子共同沉淀重金属离子和配位剂(包括羧酸和氢氟酸)。处理结果满足《电镀污染物排放标准》(GB 21900–2008)中"表3"的要求。     

Kinetics of Iron-Sodium Disilicate Reactions and Wetting

Thermogravimetric and sessile drop measurements were used to study kinetics of redox reactions between sodium disilicate glass and iron. Two redox reaction sequences were identified; both introduced ferrous oxide into the glass at the interface. One consists of formation of ferrous oxide at the interface by reduction of sodium ions in the glass; this is primarily dependent on the a (FeO) in the metal being less than one. The second consists of oxidation of ferrous ions in the glass by the reduction of sodium ions to form ferric ions which subsequently react with the iron to form ferrous oxide. The reaction rates were shown to be sensitive to temperature, time, total ambient pressure, partial pressure of sodium and oxygen in the atmosphere, and the a (FeO) in the iron. Decrease of contact angles and spreading occur with the redox reaction in which the metal plays an active role, i.e. whose a (FeO) is less than one and whose composition undergoes a change.