长链烷基(2-羟乙基)二甲基氯化铵用作分析增敏试剂

合成了3种含季氮原子及羟基的同系列分析增敏试剂十六烷基(2-羟乙基)二甲基氯化铵(HEMAC)、十四烷基(2-羟乙基)二甲基氯化铵(TEMAC)和十二烷基(2-羟乙基)二甲基氯化铵(DEMAC),测试其基本物性,并用作测定微量钪、铁(Ⅲ)、锗的增敏试剂,获得了与阳离子表面活性剂及醇类有机溶剂联用时相仿的增敏效果。     

表面活性剂在极谱分析中的应用 Ⅲ.铽在铜铁试剂-氯化十二烷基三甲铵(DTMAC)-氯化铵-氢氧化铵体系中的极谱性质及应用

本文研究了16种表面活性剂对铽-铜铁试剂-氯化铵极谱体系的增敏作用。实验结果表明,除阳离子表面活性剂、长链烷基吡啶以及在溶液中不能形成“胶束”的表面活性剂外,其它的阳离子表面活性剂、非离子表面活性剂和两性表面活性剂均能对上述体系产生增敏作用。氯化十二烷基三甲铵(DTMAC)的增敏作用最强。利用示波导数极谱测定铽的最佳条件为:0.03MNH_4Cl-0.08％铜铁试剂(Cup)-0.005％DTMAC-O.1％NH_4OH,pH～9.铽浓度在4.4×10~(-10)M～4.4×1O~(-9)M之间与波高成线性关系。干扰元素经萃取和色谱分离后,本方法可成功地用于矿石中痕量铽的测定。     

水杨基萤光酮-溴化十六烷基三甲基铵胶束增溶光度法测定微量铟

本文研究了阳离子、阴离子及非离子型表面活性剂对铟-水杨基萤光酮络合反应的胶束增敏作用的适宜pH范围和吸收光谱特性,并对其增敏机理进行探讨。试验表明溴化十六烷基三甲基铵(CTMAB)增敏作用最强,摩尔吸光系数可达1.8×10~5,pH范围宽。并考察了四十多种离子对反应的影响。拟定测定微量铟的方法,可不用有机溶剂萃取,对环境保护有利。     

Mo-苯芴酮-Triton X-100增溶光度法测定微量钼

应用有机染料测定微量钼的光度法,灵敏度虽高但操作较繁琐。随着保护胶和表面活性剂的应用,微量钼的测定又有一些灵敏度较高的方法。用阿拉伯树胶作为钼与苯芴酮络合物的保护胶比色测定钼,摩尔吸光系数为3.02×10~4。用氯化十六烷基吡啶作为钼与苯芴酮络合物的增溶剂,可在波长540nm处测定钼。用溴化十六烷基三甲基铵作钼与苯芴酮络合物的增溶剂,摩尔吸光系数为1.03×10~5。我们用非离子表面活性剂Trition X-100作钼     

硫氰酸钾-OP光度法测定有机相中微量铁

用二元或三元有机磷类萃取剂萃取铀时,铁也部分被萃取,工艺过程中需加以控制。有机相中微量铁可用邻菲咯啉比色法直接测定,此法以无水乙醇作稀释剂,三烷基氧膦(TRPO)作乙醇和煤油(试样)的混溶剂,但取样量不能超过1毫升,否则引起TRPO无法抑制的混浊。我用曾用萃取原子吸收分光光度法或用盐酸反萃后测定有机相中微量铁。随表面活性剂在胶束增溶分光光度法中的广泛应用,我们研究了Fe-SCN-OP的显色反应,并应用于二元或三元磷类萃取体系的有机相中微量铁的测定。本法操作简便,选择性良好,表观摩尔吸光系数为     

吸光光度法测定聚碳酸酯树脂中微量铁

采用光度法在水相中测定聚碳酸酯树脂中微量铁已有报道,本文研究了在非离子表面活性剂平平加存在下,用二溴苯基荧光酮测定聚碳酸酯树脂中微量铁的方法,该法灵敏度高,摩尔吸光系数达1.6×10~5,精密度好,干扰元素少,用于样品中铁的测定,结果满意。     

两性表面活性剂胶束增溶显色反应的应用及机理的研究 Ⅰ.DDMAA-CAS高灵敏度分光光度法测定微量铝

将阳离子表面活性剂、非离子表面活性剂和阴阳离子表面活性剂应用于铝(Al)-铬天青S(CAS)体系以测定微量铝,已有不少报导,对提高反应的灵敏度,改善反应条件取得了良好的效果,有的体系已用于钢铁中微量铝的测定。我们曾把两性表面活性剂用于稀士元素的分析,表现出灵敏度高,选择性强,水溶性、稳定性好等优点。本文试图把两性表面活性剂应用于Al-CAS体系,研究其分光光度性质和反应机理,并寻求一个高灵敏度测定微量铝的新方法。试验证明,两性表面活性剂:N-十二烷基二甲基铵基乙酸(DDMAA),N-十二烷基二聚氧乙烯铵基乙酸(DDPAA)均能与铝、铬天青S形成三元胶束络合物,并表现出突出     

水杨基萤光酮-溴化十六烷基三甲铵高灵敏分光光度法测定微量锰

近年,以非离子表面活性剂增溶,用吡啶偶氮类显色剂在水相测定微量锰的光度法获得了较好的结果。用水杨基萤光酮-表面活性剂体系光度法测定微量锰的研究尚未见报导。本文探讨了用水杨基萤光酮-溴化十六烷基三甲铵体系光度法测定锰的最佳条件。试验表明,在pH8.6～9.8范围内,锰与水杨基萤光酮和溴化十六烷基三甲铵生成可溶于水的蓝紫色络合物,最大吸收波长为562nm,摩尔吸光系数高达1.31×10~5,是目前水相介质中光度法测定锰灵敏度最高的体系。     

新试剂1-(2-羟基-3,5-二硝基苯基)-3-[4-(苯基偶氮)苯基]-三氮烯的合成及与季铵盐型阳离子表面活性剂的显色反应

合成了新试剂1-(2-羟基-3,5-二硝基苯基)-3-[4(苯基偶氮)苯基]-三氮烯(HDNPAPT),研究了该试剂在NaOH介质中与阳离子表面活性剂漠化十六烷基三甲铵(CTMAB)、溴化十六烷基吡啶(CPB)、溴化十二烷基二苄铰(DDMBAB)形成1:3的紫红色离子缔合物显色体系.测定了显色体系表面活性剂的临界胶束浓度、表观摩尔吸光系数ε_(max)、符合比尔定律的范围.探讨了微量阳离子表面活性剂CMTAB、CPB和DDMBAB的测定方法,结果满意.     

光度法测定微量铁实验中还原剂的优化选择

对分光光度法测定微量铁实验中还原剂的还原效果进行对比研究,结合可见吸收光谱、动力学研究、酸碱环境适应性等实验的分析说明不同还原剂所产生的结果：所选还原剂中盐酸氯丙嗪和维生素C效果最好,盐酸氯丙嗪集还原、增敏于一体,摩尔吸光系数ε=2.60×104 L·mol-1·cm-1,在含铁量为0.2~2.0 μg/mL范围内线性关系良好,符合朗伯比尔定律,适用于水中微量铁的测定。     

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。     

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.

     

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.     

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.     

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.     

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^-。     

Thermodynamics of the formation of oxosulfides of rare-earth elements

The enthalpies of solution of several oxosulfides of rare-earth elements and the high-temperature enthalpies of oxosulfides and oxosulfates of lanthanum and yttrium were measured using solution calorimetry and high-temperature microcalorimetry techniques. Standard enthalpies of formation and some thermodynamic properties of oxosulfides and oxosulfates were calculated. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2 pp. 294–297, February, 1997.     

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。