指示剂置换法识别阴离子的研究进展

指示剂置换法(IDA)是一种简单且逐渐被广泛使用的阴离子识别方法。本文简介了指示剂置换法,综述了近年来采用主要包括比色指示剂置换法(C-IDA)、荧光指示剂置换法(F-IDA)、金属络合物指示剂置换法(M-IDA)、对映选择性指示剂置换法(E-IDA)和新型指示剂置换法(N-IDA)等5种基于指示剂置换法的阴离子识别研究进展。     

气相色谱中多种死时间测定方法的比较

由烷烃同系物的保留时间计算死时间的方法有多种,常用的并得到认可的有Grobler-Balizs法(G-B法)、Guaradino法(G法)、Peterson-Hirsch法(P．H法)和Ambms法(A法)等。文献[5]已证明A法和G-B法是同一的。本文是文献[5]的继续,将证明A法、P-H法和G法也是同一的。     

GC和HPLC分析北豆根多糖的单糖组成的方法比较

采用GC法和HPLC法对北豆根多糖的单糖组成进行分析比较。采用糖腈乙酸酯衍生化—GC法和1-苯基-3-甲基-5-吡唑啉酮(PMP)柱前衍生—HPLC法分别对北豆根多糖的单糖组成进行测定,并评价两种方法的适用性。GC法检测出D-鼠李糖(D-Rha)、D-阿拉伯糖(D-Ara)、D-木糖(D-Xyl)、D-甘露糖(D-Man)、D-葡萄糖(D-Glc)和D-半乳糖(D-Gal);HPLC法检测出D-甘露糖(D-Man)、D-鼠李糖(D-Rha)、D-葡萄糖(D-Glc)、D-阿拉伯糖(D-Ara)、D-半乳糖(D-Gal)、D-木糖(D-Xyl),其中D-阿拉伯糖(D-Ara)和D-半乳糖(D-Gal)的色谱峰重叠。两种方法均检测出6种中性糖组分,对比北豆根多糖的单糖组成分析GC法和HPLC法联用较为适合。     

卡马西平在nano-TiO2/[BnMIM] PF6修饰碳糊电极上的电催化氧化及电分析方法

运用循环伏安法(CV)、计时电流法(CA)、计时库仑法(CC)、方波伏安法(SWV)研究了卡马西平(CBZ)在纳米二氧化钛(nano-TiO2)与离子液体1-苄基-3-甲基咪唑六氟磷酸盐([BnMIM]PF6)复合修饰碳糊电极(nano-TiO2-[BnMIM] PF6/CPE )上的电化学行为、电化学动力学性质及电分...     

食品中硒检测技术研究进展

对测定食品中微量元素硒的前处理方法(干法、湿法、微波消解法等)和检测方法(原子光谱法、分子光谱法、色谱法、电化学法等)的现状(主要在1990～2010年间发表的文献)及相关的原理和方法的特点之处作了综述(引用文献20篇)。     

水中氯化物检测及样品前处理技术研究进展

综述了近年来我国水中氯化物检测及样品前处理技术的研究进展。样品前处理技术包括试剂法和离子交换树脂法;检测方法包括常规化学分析法(容量法和分光光度法)、电分析方法(电位滴定法和电化学法)、离子色谱法、光谱法(原子吸收光谱法和共振光散射光谱法)、连续流动注射法等(引用文献37篇)。     

矿石及一些希有元素的光谱定量分析方法

目次Ⅰ、绪言Ⅱ、矿石的光谱定量分析法(一)固体分析法(1)粉末法i)冲淡法;ii)增量法;iii)结合化学处理法;iV)可利用的几种技术(空气冷却电极,转动或移动电极)。(2)压片法(二)液体分析法(1)液面打弧法;(2)干燥后打弧激发;(3)喷入光源法;(4)在液体中放电;(5)溶液流入法;(6)熔化后打弧。(三)气体分析法(1)利用带光谱;(2)用低压火花光源。(四)几种有用的技术(1)减除氰带光谱的方法;(2)阴极层效应的利用;(3)特殊形状电极的利用(双电弧、双室电极、物理     

Schiff碱金属配合物的合成及其抗菌活性研究进展

介绍了Schiff碱金属配合物的直接合成法、分步合成法、模板合成法、逐滴反应法、高度稀释法以及水热合成法等,综述了Ni(II)、 Cu(II)、 Co(II)、 Zr(II)等过渡金属以及Nd(III)、 Sm(III)等稀土金属等形成的Schiff碱金属配合物结构及其对大肠杆菌、金黄色葡萄球菌、枯草杆菌等多种细菌的抑制作用。讨论了Schiff碱金属配合物分子设计和应用中尚存的问题,对于新型抗菌药物的研发有一定的借鉴意义。     

空气中重金属元素的分析方法研究进展

综述了空气中重金属检测中样品的前处理方法(包括超声消解法、电热板消解法、微波消解法、全自动石墨消解法以及固体直接进样法等)和测定方法(包括原子吸收光谱法、原子荧光光谱法、原子发射光谱法、电感耦合等离子体质谱法、电化学法、生物传感器法等)的研究进展(引用文献54篇)。     

流动注射分析法与多种仪器分析联用的进展

对流动注射分析法(FIA)与多种仪器分析方法,包括分光光度法、电感耦合等离子体原子发射光谱法(ICP-AES)、原子吸收光谱法(AAS)、化学发光法(CL)、荧光光度法、电化学分析法、生物传感器、毛细管电泳、免疫分析法等联用在最近两年中的新进展作了评述,引述文献42篇.     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

Synthesis of phenolic components of Grains of Paradise

Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。     

Study of hydration of two cements of different strengths

Main hydration products of two cement pastes, i.e. CSH-gel, portlandite (P) (and specific surface S) were studied by static heating, and by SEM, TEM and XRD, as a function of cement strength (C-33 and C-43) hydration time (th) and subsequent hydration in water vapour.Total change in mass on hydration and air drying, M_o, increased with strength of cement paste and with hydration time. Content of water escaping at 110 to 220°C, defined as water bound with low energy, mainly interlayer and hydrate water, was independent on cement strength but its content increased with (th). Content of chemically bound (zeolitic) water in CSH-gel, escaping at 220-400°C, was slightly dependent on strength and increased with (th). It was possibly derived from the dehydroxylation of CSH-gel and AFm phase. Portlandite water, escaping at 400-500°C, was independent on cement strength and was higher on longer hydration. Large P crystals were formed in the weaker cement paste C-33. Smaller crystals were formed in C-43 but they increased with (th). Carbonate formated on contact with air (calcite, vaterite and aragonite), decomposed in cement at 600-700^oC. It was high in pastes C-33(1 month) and C-43(1 month), i.e. 5.7 and 3.3%, respectively; it was less than 1% after 6 hydration months (low sensitivity to carbonation) in agreement with the XRD study showing carbonates in the air dry paste (1month), and its absence on prolonged hydration (6 months) and on acetone treatment. Water vapour treatment of (6 months) pastes or wetting-drying increased this sensitivity.Nanosized P-crystals, detected by TEM, could contribute to the cement strength; carbonate was observed on the rims of gel clusters.This revised version was published online in November 2005 with corrections to the Cover Date.     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

Investigation of Kinetics of Solid-Phase Synthesis of Lithium Orthosilicate

The kinetics of the interaction between lithium carbonate and silica with various degrees of dispersion was investigated by TG and DTA methods. It was found that the utilization of pyrogenic silica with a specific surface area of about 300 m²g^-1 instead of aerosil with one of 175 m²g^-1 leads to an increase of the reaction rate between lithium carbonate and silica, which depends on the formation and growth of lithium orthosilicate crystals in the first stage, and is conditioned by the diffusion of lithium and oxygen ions through the lithium orthosilicate layer formed at temperatures above 800 K. This supposition is supported by the kinetic analysis results obtained with the use of the different models. The optimal regime of heating is recommended. This revised version was published online in July 2006 with corrections to the Cover Date.     

小环化合物中饱和碳质子化学位移的计算

小环化合物由于其张力、构型、构象和各向异性效应等原因,环碳上质子化学位移缺乏规律性,难以预测,对此作者曾提出一种近似算法。本文根据303种小环化合物中饱和碳质子的化学位移实验数据,将适于计算这类质子化学位移的公式表述为:     

恶臭嗅辨实验室建设探讨

针对恶臭测试的环境影响问题,提出了解决的实例方案,并对方案的要点及优缺点进行讨论,此方案在实际操作中具有较好的效果。     

Summary of development of the theory of stability of colloids and thin films

In this review, the research of the author in the field of colloidal systems is summarized. The factors influencing colloidal stability are systematized and analyzed. Examples are presented to illustrate the practical utilization of the theory of stability of colloids and thin films.This review was prepared on the basis of the works of the author, which were awarded the State Premium for 1991 in the field of science and technology, chemistry section.Institute of Physical Chemistry, Russian Academy of Sciences, 117915 Moscow. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 8, pp. 1708–1717, August, 1992.