火焰原子吸收光谱法测定硅粉中的铜

介绍了用火焰原子吸收法测定工业硅粉中微量铜的具体方法和过程，同时也给出了最佳实验条件。实验中采用新的样品处理方法，得到了令人满意的结果。其中样品回收率为99．8％—104．0%，相对标准偏差为0．31％—0.38％。本方法在实际应用过程中，简单、快速、     

Preparation of heat‐resistant gradient‐index polymer optical fiber rods based on poly(N‐isopropylmaleimide‐co‐methyl methacrylate)

Using the interfacial gel polymerization method, a heat‐resistant gradient‐index polymer optical fiber (GI POF) was developed based on the copolymer of methyl methacrylate (MMA) and N‐isopropylmaleimide (IPMI) as the matrix material and bromobenzene (BB) as dopant. The gradient distribution of IPMI in the GI POF rod was determined by element analysis. IPMI had great advantage in improving glass transition temperature (T_g) and forming a gradient‐index profile. There was a significant enhancement in the heat‐resistant property in comparison with a conventional GI POF rod. The combination of high thermal stability and easy fabrication makes the novel BB–IPMI–MMA system very suitable for heat‐resistant GI POF. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 87: 280–283, 2003     

VC二步发酵高糖流加工艺的研究

利用从生产中选育得到的耐高糖菌株,通过在线的检测数据,应用改进的高浓度山梨糖流加控制工艺,考察了初始山梨糖浓度、底物浓度、流加阶段pH等对维生素C二步发酵的影响,确定了适宜的控制工艺,提高了发酵水平及设备利用率.     

N-甲基吗啉绿色合成研究

N-甲基吗啉生产的传统工艺条件苛刻,对设备腐蚀严重、对人体造成巨大危害、对环境造成严重污染.利用碳酸二甲酯和吗啉为原料合成了N-甲基吗啉,采用正交试验方法讨论了原料配比、反应时间、反应温度对收率的影响,并得出了优选反应工艺条件为:物料配比为n(C4H8NO):n(C3H6O3)=1:1.2,反应时间为3 h,反应温度为100 ℃.在此条件下的产品经色质联用仪检测,产品收率可以达到95%以上.结果表明:此法具有原料价廉易得、操作容易控制、不污染环境,是一条简单易行的典型的绿色合成途径.     

使用氯化铵生产硝酸铵系复合（混）肥的爆炸性分析

硝酸铵是硝基复合(混)肥生产的主要原料。近年,由于氯化铵价格低廉,也逐步成为硝基复合(混)肥生产的主要原料之一,而氯化铵会促进硝酸铵的分解,因此,讨论用氯化铵和其他无机原料生产硝酸铵系复合(混)肥的爆炸性。通过控制物料配比,避免物料超温,可确保生产安全。     

Photocatalytic decoloration of water-soluble azo dyes by reduction based on bisulfite-mediated borohydride

Investigation of the photocatalytic decoloration of nine water-soluble anionic azo dyes widely used for the coloration of textiles was conducted in a photoreactor by a selected reduction based on bisulfite-mediated borohydride. The influence of the irradiation power on their decoloration was discussed in this work. The decoloration processes of two typical azo dyes, Reactive Red MS and C.I. Direct Blue 15 were examined with UV–vis measurement and their decoloration kinetics was also investigated. Moreover, identification of benzidine compounds released from the photoreduction of four direct dyestuffs was undertaken. The results indicated that the reduction of the dyes was significantly enhanced under the increasing irradiation. It was found that the overall degradation followed pseudo-first-order kinetics and two distinct stages were observed in the decoloration processes of Reactive Red MS and C.I. Direct Blue 15. The decay rates at first stage were slightly changed, but the decay rates at second stage were significantly affected by the light intensity. In addition, UV–vis spectra showed that the azo linkages in molecule structure of the dyes were destroyed during the decoloration. Finally, dimethoxyl benzidine or benzidine produced from the photoreduction of four direct dyes was identified as the decoloration products through a rapid spectrophotometric method.     

洗车废水回用技术的研究应用进展

洗车废水含有油污，泥沙，表面活性剂及其他可溶性有机物。洗车废水处理回用技术因洗车规模大小不同存在很大差别。该文介绍了目前国内外大型洗车场废水处理回用的主要工艺，概括和比较了洗车点洗车废水回用装置的主要技术，分析了目前小型回用装置存在的问题，并对发展方向作了展望。     

无标样RP-HPLC测定α-吡咯烷酮乙酸甲酯

α-吡咯烷酮乙酸甲酯是一种医药中间体,建立了一种RP-HPLC方法,可以在没有α-吡咯烷酮乙酸甲酯标准对照品的情况下,测定合成样品中α-吡咯烷酮乙酸甲酯的含量,当α-吡咯烷酮乙酸甲酯含量为91%~96%时,SD为0.63%~0.82%,RSD为0.66%~0.89%,与化学分析法对比,结果令人满意。     

3-(5,5-二甲基-1,3-二(口恶)烷-2-基)-2-丁烯醛合成研究

以4-乙酰氧基-2-甲基-2-丁烯醛为原料,经醛基保护、酯交换、氧化合成3-(5,5-二甲基-1,3-二(口恶)烷-2-基)-2-丁烯醛.首次采用氯化亚铜协同TEMPO催化氧化2-(3-羟基-1-甲基-1-丙烯基)-5,5-二(口恶)甲基-1,3-二(口恶)烷,合成3-(5,5-二甲基-1,3-二(口恶)烷-2-基)-2-丁烯醛.初步研究了催化氧化反应机理,指明了催化氧化反应研究的方向.氯化亚铜协同TEMPO催化氧化α-烯醇合成α-烯醛,对于现代类胡萝卜素类药物和其他新药开发研究具有重要意义.     

Low temperature solid-state synthesis routine and mechanism for Li3V2(PO4)3 using LiF as lithium precursor

Monoclinic lithium vanadium phosphate, Li₃V₂(PO₄)₃, has been successfully synthesized using LiF as lithium source. The one-step reaction with stoichiometric composition and relative lower sintering temperature (700 °C) has been used in our experimental processes. The solid-state reaction mechanism using LiF as lithium precursor has been studied by X-ray diffraction and Fourier transform infrared spectra. The Rietveld refinement results show that in our product sintered at 700 °C no impurity phases of VPO₄, Li₅V(PO₄)₂F₂, or LiVPO₄F can be detected. The solid-state reaction using Li₂CO₃ as Li-precursor has also been carried out for comparison. X-ray diffraction patterns indicate that impurities as Li₃PO₄ can be found in the product using Li₂CO₃ as Li-precursor unless the sintering temperatures are higher than 850 °C. An abrupt particle growth (about 2 μm) has also been observed by scanning electron microscope for the samples sintered at higher temperatures, which can result in a poor cycle performance. The product obtained using LiF as Li-precursor with the uniform flake-like particles and smaller particle size (about 300 nm) exhibits the better performance. At the 50th cycle, the reversible specific capacities for Li₃V₂(PO₄)₃ measured between 3 and 4.8 V at 1C rate are found to approach 147.1 mAh/g (93.8% of initial capacity). The specific capacity of 123.6 mAh/g can even be hold between 3 and 4.8 V at 5C rate.