流动注射化学发光法测定安痛定注射液中的氨基比林

在甲醛存在下,高锰酸钾与氨基比林能够发生化学发光反应,产生很强的化学发光,由此建立一种测定氨基比林的流动注射化学发光分析法。方法的检出限为３．０×１０－８ｇ／ｍＬ,相对标准偏差为１．３％（４．０×１０－５ｇ／ｍＬ氨基比林,ｎ＝１１）,线性范围为１．０×１０－７～８．０×１０－５ｇ／ｍＬ氨基比林。该法已用于安痛定注射液中氨基比林含量的测定。     

次氯酸钠-芦丁-盐酸氨基脲体系的化学发光反应研究

提出了以次氯酸钠－芦丁－盐酸氨基脲化学发光新体系,结合流动注射技术建立了测定芦丁的的化学发光新方法。芦本质量浓度在４．０×１０＾－１１－－１．０×１０＾－８ｇ／Ｌ范围内与发光信号叶线性关系。检出限为１．３×１０＾－１１ｇ／Ｌ。相对标准偏差为２．６％。     

高锰酸钾-亚硫酸钠-核黄素化学发光体系的研究

研究了核黄素在酸性条件下与高锰酸钾和亚硫酸钠发生化学发光反应的行为,建立了流动注射化学发光测定核黄素的新方法。核黄素浓度在１．０×１０＾－７－１．０×１０＾－５ｇ／ｍＬ范围内与化学发光强度呈良好的线性关系,检出限为３×１０＾－８ｇ／ｍＬ。对４．。０×１０＾－７ｇ／ｍＬ的核黄素进行１１次平行测定,得方法的相对标准偏差为１．６％。     

流动注射化学发光法测定甲氨蝶呤

研究了甲醛增强高锰酸钾与甲氨蝶呤的化学发光反应，由此建立了一种测定甲氨蝶呤的流动性注射化学发光分析法，方法的检出限为３．４×１０＾－９ｇ／ｍＬ，相对标准偏差为１．１％（２．０×１０＾－６ｇ／ｍＬ甲氨蝶呤，ｎ＝１１）线性范围为１．０×１０＾－８～１．０×１０＾－５ｇ／ｍＬ。该法已用于甲氨蝶呤针剂及片剂中甲氨蝶呤含量的测定。     

鲁米诺-高碘酸钾-抗坏血酸体系化学发光反应的研究与应用

基于抗坏血酸在碱性条件下与高磺酸钾和鲁米诺反应产有强的化学发光,建立了流动注射化学发光测定抗坏血酸的新方法。在碱性条件下的氧化过程易产生过氧化物和超氧自由基,是产生化学发光的关键。该法校准曲线线性范围为６．０×１０＾－６－４．０×１０＾－２ｇ／Ｌ,检出限达８×１０＾－７ｇ／Ｌ,相对标准偏差小于４％,采样频率为１２０次／ｈ。     

高锰酸钾—抗坏血酸化学发光体系测定抗坏血酸

本文研究了高锰酸钾－抗坏血酸化学发光体系，建立了测定抗坏血酸的化学发光分析新方法，线性响应的浓度范围为５．０×１０＾－７ｍｏｌ／Ｌ～４．０×１０＾－５ｍｏｌ／Ｌ，检出限为３．０×１０＾－７ｍｏｌ／Ｌ，对２．５×１０＾－６ｍｏｌ／Ｌ抗坏血酸进行１０次平行测定，相对标准偏差为１．６％，考察了２２种物质的干扰情况。用于维生素Ｃ片剂及注射液中抗坏血酸含量测定，结果令人满意。     

流动注射—吐温40化学发光新体系测定贵金属冶金物料中微量铱

本文研究了吐温４０－ＫＯＨ－Ｈ２Ｏ２－Ｉｒ化学发光新体系，采用流动注射进样技术，建立了测定铱的新的化学发光分析法，检测限为１．１×１０＾－１３ｇ／Ｌ；线性范围为每ｍＬ１．０×１０＾－９－１．０×１０＾－５ｇ。经离子交换分离Ａｕ和Ｏｓ离子后，测定贵金属冶金物料中微量铱，结果满意。     

空气中肼的流动注射化学发光分析

研究了肼在碱性条件下与鲁米诺和高磺酸钾产生化学发光行为，建立了流动注射化学发光测定痕量肼的新方法。肼的浓度在１．０×１０＾－８－１．０×１０＾－６ｇ／ｍＬ范围内与化学光强度成线性关系；检出限为４×１０＾－９ｇ／ｍＬ；相对标准偏差小于３％。     

流动注射化学发光法测定利血平

研究了利血平在酸性条件下与高锰酸钾和过氧化氢产生化学发光的行为，建立了流动注射化学发光测定利血平的新方法。利血平的浓度在１．０×１０＾－６￣８．０×１０＾－５ｈ／ｍＬ范围内与化学发光强度呈良好的线性关系；检出限为３×１０＾－７ｇ／ｍＬ。对６×１０＾－６ｇ／ｍＬ利血平进行１１次平行测定，得方法的相对标准偏差为１．３％。方法用于药剂中利血平含量测定，结果与药典标准方法测得值一致。     

测定钴的化学发光新体系

研究了新吖啶衍生物９，１０－二甲基吖啶氟磺酸盐的化学发光特性。建立了测定Ｃｏ６２＋的化学发光新体系。方法线性范围为１．０×１０＾－１０－１．０×１０＾－７ｇ／ｍＬ；检测限为５．０×１０＾－１１ｇ／ｍＬＣｏ＾２＋。测定５．０×１０＾－９ｇ／ｍＬＣｏ６２＋的相对标准偏差为６．０％。方法选择性好，用于自来水，江水，池塘水中痕量钴的测定，结果令人满意。     

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.     

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。     

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.     

Acid hydrolysis of carboxymethylcellulose of low degree of substitution

Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position.     

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.     

Estimation of Kinetic Parameters of Thermal Oxidation of Ilmenite

The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of hematite Fe₂O₃. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the best fitting experimental data. This revised version was published online in August 2006 with corrections to the Cover Date.     

Mechanism of action of base-catalyzed oxygenation of phenol derivatives

Cyclopropyl derivative of 2,6-di-tert-butylphenol is synthesized as a probe to investigate the mechanism of base-catalyzed autooxidation of phenol derivatives. Our study indicates that one electron reduction of molecular oxygen from phenolate gives phenoxyl radical 3, a key intermediate of autooxidation. The coupling of phenoxyl radical and superoxide radical gives peroxylate anion 4 and produces the final epoxy alcohol adduct 6.     

氯氧化镁生成热的研究

用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。     

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.