金属盐在某些底物中的快原子轰击质谱

本文通过研究一系列盐类化合物在底物三乙醇胺和甘油醚中的快原子轰击质谱,总结出它们的加合阳离子系列,并从快原子轰击质谱的离化机理和亚稳跃迁结果探讨了这些离子的来源。     

Synthesis and crystal structure of 4-acetoxy-5,6-dihydro-5,5-dinitro-2H-1,3-oxazineN-oxide

A novel heterocyclic compound, 4-acetoxy-5,6-dihydro-5,5-dinitro-2H-1,3-oxazineN-oxide, has been synthesized by the reaction of the dipotassium salt of 1,1,5,5-tetranitro-3-oxapentane with aqueous acetic acid. The synthesized compound has been studied by X-ray diffraction analysis.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 12, pp. 2207–2210, December, 1994.We would like to thank G. V. Lagodzinskaya (Institute of Chemical Physics in Chernogolovka, Russian Academy of Sciences) for recording and interpreting¹H NMR spectra, A. M. Korolev (Institute of Chemical Physics in Chernogolovka, Russian Academy of Sciences) for helpful discussion, and V. I. Fetisov (Institute of Physiologically Active Compounds, Russian Academy of Sciences) for performing quantum-chemical calculations by the AM1 SCF MO LCAO method.     

Synthesis, Characterization and Thermal Decomposition Mechanism of Cetyltrimethyl Ammonium Tetrathiotungstate

The synthesis, characterization and thermal decomposition mechanism of cetyltrimethyl ammonium tetrathiotungstate （CTriMATT） were studied herein. The as-synthesized CTriMATT was characterized by Elemental analysis, X-ray diffraction （XRD）, Fourier transform infrared （FT-IR）, Ultraviolet visible （UV-Vis） spectra. The results showed that the as-synthesized CTriMATT had high purity and good crystallinity. The introduction of alkyl groups induced a shift of the stretching vibration band of W-S bond to lower wavenumber, while it had no influence on the position of WS4^2-. Thermogravimetric analysis （TG）, differential thermal analysis （DTA） and in situ XRD characterizations revealed that CTriMATT began to decompose at 423 K in nitrogen and was converted to WS2 eventually. In addition, the decomposition product of CTriMATT at 673 K in nitrogen was characterized by N2 adsorption （BET） and scanning electron microscopy （SEM）. The results demonstrated that WS2 with higher specific surface area, and pore volume could be obtained from the thermal decomposition of CTriMATT in nitrogen.     

毛细管电泳中高盐样品在线富集的研究进展

在毛细管电泳分析过程中，简便高效的高盐样品处理技术对血清、尿液、海水和工业废水等样品的富集分析具有重要的意义。综述了在CE中高盐样品在线富集的若干种方法，包括乙腈法、瞬间等速电泳法、pH修饰法、动态pH联接法、胶束反应法和瞬间移动化学反应界面法，并简要地介绍它们的应用和研究进展。     

四元交互体系Li~＋，Mg~（2＋）／Cl~－，SO_4~（2－）－H_2O

本文采用等温溶解平衡法研究了四元交互体系Ｌｉ＋，Ｍｇ２＋／ＣＩ－，ＳＯ－Ｈ２Ｏ２５℃的机关系和平衡液相的物化性质（密度、粘度、电导率、折光率和ｐＨ）．该体系２５℃有七个相区Ｌｉ２ＳＯ４·Ｈ２Ｏ，ＭｇＳＯ４·７Ｈ２Ｏ．ＭｇＳＯ４·６Ｈ２Ｏ．ＭｇＳＯ４·５Ｈ２Ｏ，ＭｇＣ１２，６Ｈ２Ｏ，ＬｉＣＩ．ＭｇＣｌ２．７Ｈ２Ｏ，ＬｉＣＩ·Ｈ２Ｏ，十一条单变量线，五个共饱点．其中ＬｉＣＩ·Ｈ２Ｏ＋ＬｉＣＩ·ＭｇＣｌ２·７Ｈ２Ｏ＋Ｌｉ２ＳＯ４·Ｈ２Ｏ为一致零变量点．与文献中的研究结果比较，我们得到两个新相区ＭｇＳＯ４·６Ｈ２Ｏ和ＭｇＳＯ４·５Ｈ２Ｏ．用经验和半经验公式计算了平衡液相的密度、折光率．由实验测定的溶解度数据求得了高锂浓度下的Ｐｉｔｚｅｒ参数．对该体系２５℃溶解度进行了理论计算复证．     

碳酸氢铵沉淀法制备氧化钇粉体时反应条件对产物粒度的影响

研究了碳酸氢铵沉淀法的反应条件对氧化钇粒度的影响,探讨了粒度变化规律。发现在沉淀反应中,晶型碳酸钇铵的形成与否是影响氧化钇粒度的关键因素。在较低的反应温度下,当碳酸氢铵和氯化钇的浓度大于0.25mol·L-1,摩尔比大于5,陈化时间大于60min时得到碳酸钇铵沉淀,经煅烧可获得粒度(D50)大于1μm的氧化钇。当反应物浓度较低、摩尔比小,陈化时间较短时得到无定型碳酸钇沉淀,煅烧沉淀可获得粒度(D50)小于0.5μm的氧化钇。实验证明选择适当的沉淀反应条件,可制备D50在0.3～10μm范围内的不同粒度级别的氧化钇粉体。     

Facile cyclic ammonium salt with the smallest size for high performance electric double layer capacitors

A novel cyclic ammonium salt, N,N-dimethylpyrrolidinium tetrafluoroborate (P₁₁-BF₄), was successfully synthesized for the first time. The smallest cyclic structure of P₁₁-BF₄ induced high solubility and conductivity in PC, which can easier enter the micropores of activated carbon and occupy more surface area during charge/discharge process.     

沐浴海绵Spongia zimocca aubspecles irregularia(Lendenfeld)中的含氮化合物

从沐浴海绵Spongia zimocca aubspecles irregularia(Lendenfeld)分离和处理得到3种含氮化合物,通过波谱法鉴定化学结构,化合物1为新的神经酰胺N-2-(1,3-二羟基-十五烷基)-2′,20′-二十一酰胺,2为神经酰胺(E)-N-2-(1,3-二羟基-4-十八烯基)-十六酰胺,3为醋酸胍.     

熔盐电解合成希土六硼化物的研究——REBO3、LiBO2和LiF体系熔盐电解合成RER6

本文在800℃和空气中电解REBO₃-LiBO₂-LiF熔盐体系合成了单相的REB₆.石墨川埚兼作容器和阳极.耐火金属棒如Cu和Mo等被悬吊在电解质中作为阴极.根据似二元体系LiBO₂-LiF和LiBO₂-LaBO₃的低熔点组成以La₂O₃、B₂O₃、Li₂CO₃和LiF为原料找到了具有较低熔点的熔盐体系.根据X射线粉末衍射,该熔体是由REBO₃、LiBO₂和LiF三个物相组成.     

Deshydratation de l'alun d'ammonium

Dehydration of hydrated ammonium alum is a function of physical gaseous pressure. During dehydration, two kinds of partially dehydrated amorphous alum appears. These solids differ in texture and residual water composition.