库仑-称重法测量金属镀层厚度的研究

用库仑法溶解镀层,阳极溶解曲线判断溶解终点,天平确定镀层厚度,建立了库仑-称重法。在电镀锡板上的试验,取得了满意的结果,SD小于0．04g／m^2,RSD不超过0．36%。     

聚苯胺纳米点的氧化还原态与其库仑台阶效应

应用电化学恒电位法结合模板法制备聚苯胺纳米点阵列,导电原子力显微镜研究处于不同氧化还原态的聚苯胺纳米点的I～V特性,发现只有处于部分氧化态(导电态)的聚苯胺纳米点才出现库仑台阶效应,还原和全氧化态聚苯胺纳米点不显示库仑台阶.初步探讨了上述现象.     

吸附方波伏库仑法研究 Ⅰ简单吸附体系

对简单吸附体系方波伏库仑法进行了理论推导和实验验证，讨论了各种因素对伏库仑曲线的影响。研究表明，对于简单吸附体系，方波伏库仑法的灵敏度和检测限均优于方波伏安法。     

吸附方波伏库仑法研究：I.简单吸附体系

对简单吸附体系方法伏库仑法进行了理论推导和实验验证，讨论了各种因素对伏库仑曲线的影响，研究表明，对于简单吸附体系，方法伏库仑法的灵敏度和检测限均优于方波伏安法。     

贵金属元素的库仑分析法

本文展望了库仑法在贵金属分析中的应用前景,介绍了1958—1986年以来国内外库仑分析法的新体系、新方法。详细评述了各种库仑法在贵金属元素分析中的应用。附有参考文献81篇。     

库仑滴定法测定烟叶提取物中茄尼醇

本文提出用库仑滴定法测定茄尼醇。以含有1mol·L－1KBr的78％（V／V）醋酸溶液为介质，以5mA恒电流为电解电流，对布尼醇进行库仑滴定，用双铂电极电流法指示滴定终点，得到满意结果．方法简便、准确，不需要标准溶液，不需要昂贵仪器。     

吸附方波伏库仑法研究 Ⅱ络合吸附体系

对络合吸附体系分别推导了前行化学反应平衡常数Ｋ１和Ｋ１两种情况的方波伏库仑法的电量方程及作了实验验证，获得判别这两种络合吸附体系的理论依据。讨论了各种因素对伏库仑曲线的影响，并由实验比较了方波伏库仑法和方波伏安法的检测限。     

计时库仑法研究——报导1用计时库仑法测定钌

钌的价态、存在形式较复杂,给电分析测定带来许多困难,库仑分析虽有一些报导,但不够理想,计时库仑法具有恒电势库仑法的优点,又省时间。本文研究了在1NH_2SO_4底液中,将不同价态的钌用硼氢化钠还原为三价,于+0.85V(对饱和甘汞电极),在铂网电极上计时氧化为四价,10~(-3)～10～(-6)M的钌,固定时间20.0秒,所得电量与浓度间线性关系良好。对10~(-6)M的钌的测定结果误差在10％以下,多数贵金属和某些贱金属不干扰测定。样品     

极譜微庫仑法测定电极还原电子数

在无机或有机极谱研究中,往往都需要知道参与电极反应的电子数n。n值有助于研究复杂的氧化还原体系的电极反应的机理,有助于确定电极反应产物的结构。关于n值的测定,前人已积累了很多工作,如极谱法、库仑法和极谱库仑法等,各种方法各有其适用特点,本文将就极谱库仑法综述于后。     

电量法测定轻质石油产品中氯含量

轻质石油产品中痕量氯的测定有灯法、联苯钠法、氨钠法以及微库仑法等。但这些方法有的操作繁琐费时,有的消耗大量试剂造成空白偏高,有的条件过于苛刻,操作困难。本文用自制的WK-1型微库仑滴定仪,探讨了微库仑滴定法测定氯的影响因素,并对测定轻质石油产品中0.2～500ppm氯含量的操作条件进行了讨论。     

The study of the curing of lacquer films on tinplate by alpha-particle backscattering

The backscattering of⁴He⁺ ions of a few MeV has been used to measure the state of cure of oleo-resinous lacquer films on timplate. The elemental ratio of carbon to oxygen was studied as a function of curing temperature and duration of curing. This parameter could be determined rapidly enough to be used for process control and the precision of the method allowed stoving temperatures to be measured within manufacturing tolerance.     

电解氢化物发生原子荧光法测定镉

通过电解氢化物发生技术结合原子荧光光谱仪,采用自行设计的管式电解池,研究了管状阴极材料以及电解质种类、电解条件等因素对Cd的电解还原氢化物发生情况的影响。方法检出限为0.26μg/L,相对标准偏差为3.3%(n=11)。对标准物质海带及几种海产品中的Cd进行了测定,回收率在93%～110%之间。     

X射线荧光光谱法测定电解锰中锰、硅、磷和铁含量

熔融制样X射线荧光光谱法测定电解锰中锰、硅、磷和铁含量。用熔融后的四硼酸锂制作铂金坩埚保护层,以BaO2做氧化剂,在马弗炉内通过逐渐升温来氧化电解锰,然后熔融制取玻璃熔片,用X射线荧光(XRF)光谱法分析电解锰中锰、硅、磷和铁含量。锰、硅、磷和铁的相对标准偏差RSD分别为0.23%、2.82%、0.31%和0.53%。与其它分析方法比较,其结果更稳定。有效消除了电解锰熔融制样过程中的坩埚腐蚀问题,分析误差可完全控制在国家相关标准允许的范围内,实现了电解锰中各元素的快速准确测定。     

Determination of tritium in water using electrolytic enrichment: methodology improvements

The quality control of the method for tritium (³H) determination in water after electrolytic concentration by liquid scintillation counting measurements was improved considering more parameters in the uncertainty budget, besides the control charts to evaluate the electrolytic enrichment factor, the enrichment parameter and blank samples. The quality control upgrade of the method and the participation in proficiency tests allow its optimization. This methodology was applied to the determination of ³H activity concentrations in waters from different origins: surface, rain and drinking waters.     

废水中铜银的分离和银的回收研究

废水中铜银的分离和银的回收研究黄秀山（四川三峡学院化学系万县６３４０００）关键词分解电压，还原电势，回收一、引言本实验采用电解还原的方法回收贵金属银。目前此法主要用于回收废水中的铬、汞等，对银的研究很少。曾有人进行过自然渗析还原法回收银的研究。用自然...     

Continuous flow electrolytic cold vapor generation atomic fluorescence spectrometric determination of Hg in water samples

The determination of trace concentrations of Hg in water samples by the use of electrolytic cold vapor generation (ECVG) system and AFS was studied. Several buffer solutions were used and the detection limits with these systems were found to be by a factor of 1–2 lower than in the conventional electrolytic cold vapor generation system. Comparing with the traditional inorganic acid, phosphate buffer solution (PBS) increased the signal intensity of Hg vapor from electrolytic generation on Pt cathode and reduced the impact of cathode erosion on the stability of signal intensity. Moreover, buffer solution has better interference tolerance. The effects of the electrolytic conditions and interference ions on the ECVG have been studied. Under optimized conditions and with PBS as catholyte the detection limit for Hg was found to be 0.27 ng L⁻¹. The relative standard deviation was 2.8% for 11 consecutive measurements of 1 μg L⁻¹ Hg. This method has been applied in the determination of inorganic Hg in Yangtze River water.     

火焰原子吸收光谱法测定电解铝用冰晶石中锂

含锂冰晶石取代锂盐添加到电解质中被广泛应用于电解铝工业,其质量直接影响到电解铝工业的电解效率、吨铝能耗高低和电解铝产品质量优劣。控制冰晶石中锂含量是保证产品质量和应对废旧电解质再生对氟化盐市场冲击的一个重要举措。通过在铂坩埚中加入一定量高氯酸在高温条件下加热冒烟赶氟后再加入盐酸酸化至盐类完全溶解,建立了波长670.80 nm处采用火焰原子吸收光谱法测定铝用冰晶石中锂含量的方法,避免了大量氟基体的干扰,选择一定量的铝钠基体匹配来保证测试灵敏度和准确性;通过加标回收实验得知锂的回收率为102%;锂元素校准曲线线性相关系数≥0.9994;锂的检出限为0.0065μg/mL;不同含量含锂冰晶石的锂标准偏差均小于0.01%,与电感耦合等离子体原子发射光谱(ICP-AES)法测定结果相一致。方法准确可靠、简单易操作,满足铝电解工业生产分析的需要。     

Development and validation of Ni–Ni electrolytic enrichment method for tritium determination in samples of underground waters of Jeju Island

A method of tritium electrolytic enrichment was developed, optimized and validated. The enrichment parameters were compared with different current and total current charge variation and tritium separation factor was from 8 to 36 with a current density variation. The detection limit of tritium measurement is about 0.5 TU using 1,000 mL sample and 600 min counting time. Several samples of groundwaters were processed in our and another laboratory with good agreement of results within 15% deviation. Developed and validated method of tritium determination was applied groundwaters in Jeju Island with a liquid scintillation counter (LSC) and electrolytic enrichment method using Ni–Ni electrodes. The tritium concentrations in fifty eight groundwaters in Jeju Island were ranged <0.5 TU-3.9 TU and averaged value was 2.12 TU.     

高速离子交换色谱法分离重金属离子及铜和锌的测定

本文使用国产SY-202高速离子交换色谱仪(库仑检测器)以及国产YSG-SO₃Na型阳离子交换树脂研究了铜、锌、镍、钴、镉、铅和锰等七种二价离子在酒石酸盐、乳酸盐及柠檬酸盐体系洗脱液中的分离情况,考察了洗脱液及其流速对保留时间和柱效的影响以及不同离子和不同进样量对电解效率的影响。测定了黄铜和废水样品中的铜和锌。     

Product analysis of caffeic acid oxidation by on-line electrochemistry/electrospray ionization mass spectrometry

On-line electrochemistry/electrospray ionization mass spectrometry (EC/ESI-MS) was developed using a microflow electrolytic cell. This technique was applied to electrochemical oxidation of caffeic acid (CAF) which is known to be a highly antioxidative agent. Effects of electrolytic potentials on ion intensities of product ions and on electrolytic currents were examined at different pHs. Dimer products were detected at electrolytic potentials of E = 0.7 V (vs. Ag/AgCl) and trimer products at 1.0 V at pH 9. Dimer products were distinguished from hydrogen-bonded complexes by MS/MS experiments. Hydrogen/deuterium exchange experiments determined the number of hydroxyl and carboxyl groups in the Dimers formed by electrolysis. The mechanism of oxidative polymerization of CAF is discussed with speculation as to the structure of the dimer product.