Development and applications of an on-line thermal neutron prompt-gamma element analysis system

This paper introduces the principles, instrumentation, implementation, and industrial applications of an on-line thermal neutron prompt-gamma element analysis system (using a²⁵²Cf neutron source, Am–Be neutron source, or neutron generator). The energy resolution of the system at the H prompt-gamma full-energy photopeak (2.22325 MeV) is 3.6 keV. The concentration measurement error of Al₂O₃, FeO₃, CaO, and SiO₂ is ±0.3%, ±0.1%, ±0.4%, and ±0.4%, respectively. The system has been tested on-site at both the Shandong and the Zhengzhou Aluminium Works. Our preliminary on-site measurements confirm that the stability, reliability, measurement range, and accuracy of the system can meet the requirements of the aluminium production process. Facilitation of this measurement at aluminium plants is expected to reduce plant costs by over 3 million dollars annually through reduced energy consumption, more rapid qualification of pulps being mixed during the production process, and in reduced labor costs.Other participants of Shandong and Zhenghou Aluminium Works are: Wang Aili, Zengshen, Dei Jianguo and Lu Jinnan, Wang Deyu, Jin Hequan.     

铅在铂电极上的还原电位溶出分析法

研究了以亚铁氰化钾为还原剂铅在铂电极上的还原电位溶出法；讨论了电极的预处理、阳极富集和随后的还原电位溶出及铅测定的干扰。     

液相色谱中一个新的表征参数Z：Ⅱ.反相液相色谱中小分子极性溶质体系

反相高效液相色谱（ＲＰＬＣ）中小分子极性溶质的极性是可以用液相色谱中溶质计量置换保留模型中的Ｚ值（１ｍｏｌ溶质被固定相吸附时，在固定相与溶质子间释放出置换剂的ｍｏｌ数）来表征的，其大小可用带有该极性端基的同系物的Ｚ值对碳原子数线性作图的截距求得。这些检性基的Ｚ测量定值与疏水性片段指数１ｇｆ间有极好的线性关系。依此关系还可测出一些用其他实验方法无法测得的某些基团的１ｇｆ值。     

新显色剂6,8-二磺酸萘偶氮氯磺酚与铌(Ⅴ)显色反应的研究及应用

本文研究了新显色剂6,8-二磺酸萘偶氮氯磺酚与Nb(Ⅴ)的显色反应和测定条件。在酸度为0.6～3mol/L盐酸时。络合物的组成比为Nb(Ⅴ):R=1:3,摩尔吸光系数为4.42×10~4L·mol·L~(-1)·cm~(-1)。可不经分离直接测定钢铁试样中的铌。     

钌—钛金属氧化物涂层电极的电子能谱分析

用X-光电子能谱分析了Ru-Ti金属氧化物电极的组成、结构和元素价态。结果表明,电极表面不同于体内,讨论了表面和体内Ti的价态区别对Ru-Ti阳极活性和寿命的影响,指出掺杂Ir和Pd后会提高电极活性。     

低价钒化合物结构化学研究 Ⅰ. [VCL2·(THF)4]+[ZnCl3·THF]-的合成与晶体结构

The title compound has been synthesized under nitrogen atmosphere using V_2O_5 for the initiator by Schlenk techniques. It′s single crystal, which is very air and water-sensitive, was obtained and determined from three-dimensinal x-ray diffraction data collected by the four-circle diffractometer. The crystals are orth- orhombic with space group D_2~4-P_(212121) and unit cell constants a=0.909 nm, b=1.4909 nm, c=2.1635 nm and z=4. We derived first the positional parameters of V, Zn, Cland O atoms by direct method using SHELXTL program. The coordinates of other the non-hyleast-squares refinement for all atoms gave a final discrepency factor R=0.0945 and RW=0.0674.The result of structure analysis shows that the compound is composed of the octahedral cation [VCl_2·(THF)_4]~+ and the tetrahedral anion [ZnCl_3·THF]~-.The reaction mechanism was discussed. The title compound is reaction product of VCl_3 with ZnCl_2 in THF.     

A novel histidine assay using tetraphenylporphyrin manganese (III) chloride as a molecular recognition probe by resonance light scattering technique

A novel histidine-selective method has been developed for the determination of histidine in aqueous solutions by resonance light scattering (RLS) technique. At pH 8.0, the weak RLS intensity of tetraphenylporphyrin manganese (III) chloride [MnTPPCl] was greatly enhanced by the addition of histidine with the maximum peak located at 483 nm. Under the optimum conditions, it was found that the enhanced RLS intensity was in proportion to the concentration of histidine in the range 7.8 × 10⁻⁷-2.4 × 10⁻⁵ mol l⁻¹. Low detection limit of 9.2 × 10^-8 mol l⁻¹ has been achieved. The histidine concentrations in synthetic samples and real samples were determined with satisfactory results. The sensitivity and selectivity of this method are high enough to permit the determination of trace amounts of histidine without any significant interference from high levels of other components such as common anions and especially, other amino acids.     

Determination of several sugars in serum by high-performance anion-exchange chromatography with pulsed amperometric detection

In this paper, a sensitive, simple and direct method for simultaneous determination of glucose, ribose, isomaltose and maltose in serum sample by high-performance anion-exchange chromatography coupled with integrated pulsed amperometric detection was developed. The four target analytes were easily and completely separated on an anion-exchange column at a flow-rate of 0.25 mL/min by binary step gradient elution in about 16 min and the two eluents were deionized water and 500 mM sodium hydroxide, respectively. The separated four analytes were detected directly by using a gold electrode and quadruple-potential waveform integrated pulsed amperometry without derivatization. Under the optimized conditions, when the injection volume was 25 microL, the detection limits (signal-to-noise ratio equal to 3) for glucose, ribose, isomaltose and maltose were 0.92, 7.50, 12.9 and 10.3 ng/mL, respectively. The calibration graphs of peak area for the four analytes were linear over two to three orders of magnitude with correlation coefficients greater than 0.998. R.S.D. of peak areas of the four analytes for five determinations were no more than 5.6%. The analytical method had been applied to the determination of glucose, ribose, isomaltose and maltose in real serum samples and good results with low relative standard deviation not more than 5.3% were obtained. The accuracy of the proposed method was tested by recovery measurements on spiked samples and good recovery results (98.1-107.9%) were obtained.     

离子液体的酸性测定及其催化的二苯醚／十二烯烷基化反应

 采用乙腈探针红外光谱法测定了［bmim］Cl／AlCl3类离子液体的酸性．结果表明，乙腈可以区分离子液体的酸类型（Bronsted酸或Lewis酸），同时可以指示离子液体的Lewis酸强度．使用［bmim］Cl／AlCl3类离子液体催化二苯醚与十二烯的烷基化反应，研究了离子液体的酸强度、反应温度和醚烯比对反应的影响，并与AlCl3催化体系进行对比．结果发现，该离子液体对二苯醚与十二烯烷基化反应的催化活性明显高于AlCl3．使用离子液体作催化剂显著提高了烷基化反应的产率，简化了产物的分离与提纯，且对环境友好．当控制反应温度为80℃，原料醚烯摩尔比为7，并采用酸强度适中的离子液体时，目标产物单十二烷基二苯醚的产率接近90％．     

Li/LiClO4-碳酸丙烯酯体系的交流阻抗研究

结合扫描电子显微镜, 用交流阻抗法对Li/LiClO_4-碳酸丙烯酯锂电极体系的研究表明, 锂电极表面膜层的生长分三个阶段,相当于两个紧密层和一个疏松层。里紧密层由Li_2CO_3组成, 厚度约10 nm, 是Li~+导体和电子绝缘体, 电阻率为1.4×10~8 Ωcm, 对锂电极的充放电无不利影响。外紧密层由Li_2CO_3和有机物组成。疏松层是在外紧密层表面不断破裂和修复中形成的。它们都不利于锂电极的充放电。