催化动力学光度法测定井水中痕量锰

研究了在 NH3· H2 O- NH4 Cl介质中锰催化过氧化氢氧化苋菜红的褪色反应及其动力学条件 ,测定了反应级数和表观活化能 ,建立了测定痕量锰的新方法。该方法的检出限为 2 .7× 1 0 -4 μg/m L Mn,线性范围为 0～ 2 .4μg/2 5m LMn。用于测定井水中痕量 Mn,与原子吸收法的测定结果一致。     

二甲酚橙催化光度法测定亚硝酸根的研究

基于硫酸介质中亚硝酸根催化溴酸钾氧化二甲酚橙的褪色反应 ,建立了测定痕量亚硝酸根的新方法 ,并探讨了动力学条件 ,测定了反应的表观速率常数( k=1 .32× 1 0 -3 S-1)和表观活化能 ( Ea=35 .0 2 k J/mol)。方法的测定范围为 0～ 0 .1 8μg/m L,检出限为 1 .1 ng/m L。方法已用于水中及水基产品中亚硝酸根的测定     

高灵敏催化光度法测定痕量锰

研究了痕量Mn2 + 催化KIO4 氧化棉红的反应动力学 ,测定了反应级数、表观速率常数和表观活化能 ,确立了速率方程 ,探讨了反应机理 ,建立了测定痕量锰的方法 ,方法灵敏度为 7.5×10 - 9g·L- 1,线性范围为 0 .0～ 6.0× 10 - 6g·L- 1。方法选择性好 ,直接用于化学试剂、井水及蒸馏水中痕量锰的测定 ,结果满意     

测定痕量锰的锰(Ⅱ)-锌试剂-重铬酸钾体系催化分光光度法

在Na2B4O7-NaOH缓冲介质及加热条件下 ,锰 (Ⅱ )对重铬酸钾氧化锌试剂引起褪色 ,有明显的催化作用 ,据此建立了测定痕量锰的新方法 ;该法的线性范围为0.69～40μg/L,检出限为0.22μg/L ,反应表观活化能为87.1kJ/mol,反应表观速率常量1.10×10-3/s,用该法测定蒙药样品中锰含量 ,结果令人满意     

二溴羧基偶氮胂催化动力学光度法测定痕量锰(Ⅱ)的研究

在 HAc- Na Ac介质中 ,在氨三乙酸存在下 ,表面活性剂溴化十六烷基三甲胺对锰 ( )催化高碘酸钾氧化二溴羧基偶氮胂的褪色反应有强烈的增敏作用。研究了反应的最佳条件 ,建立了动力学光度法测定痕量锰的新方法。该方法的检出限为4.1 0× 1 0 - 11g/m L,线性范围 0～ 1 4 μg/L,用于食品及铝合金中痕量锰 ( )的测定 ,结果令人满意。     

番红花红褪色光度法测定痕量铜

利用铜 ( )对过氧化氢氧化番红花红使其褪色的催化作用 ,建立了分光光度法测定痕量铜的新方法。研究了反应条件 ,测定了反应的级数和表观活化能。该方法的线性范围为 0～ 2 4 0 ng/m L Cu2 + ,检出限为 2 .5× 1 0 -9g/m L。用该法对人发中的铜含量进行了测定 ,结果与原子吸收法一致     

钒(Ⅴ)催化氧化甲基紫的反应动力学及其应用

在 H2 SO4 介质中 ,以抗坏血酸为活化剂 ,痕量的钒 ( )可强烈地催化溴酸钾氧化甲基紫的反应 ,研究了反应的最佳条件及动力学参数 ,探讨了反应机理 ,建立了测定超痕量钒的高灵敏方法 ,方法的线性范围 0 .0～ 2 50 pg/m L ,检出限为 6.5×1 0 - 13g/m L。方法用于井水、蔬菜及血清中痕量钒的测定 ,获得令人满意的结果     

测定超痕量铁的高灵敏指示反应

在稀 H2 SO4 介质中 ,1 ,1 0 -邻菲 口罗啉存在下基于 Fe( )催化过氧化氢氧化棉红的新指示反应建立了测定超痕量铁的一个新方法。方法检出限 1 .0× 1 0 - 11g/m L ,线性范围 0 .0 0～ 1 .2 ng/m L。用于井水、一次蒸馏水、黄豆、芹菜中痕量及超痕量铁的测定获得满意结果     

偶氮胂I-高碘酸钾催化光度法测定痕量Mn(Ⅱ)

研究了在HAc—NH4Ac介质中，以1，10-菲啰啉为活化剂，锰(Ⅱ)催化高碘酸钾氧化偶氮胂I褪色反应的条件及影响因素，建立了动力学光度法测定痕量Mn(Ⅱ)的新方法。方法线性范围为0-80μg/L，检出限为6．3ng/mL，对60μg/L,Mn(Ⅱ)测定的相对标准偏差为2．6％。导出了动力学方程，该催化反应的表观活化能为130．4kJ／mol。已用于野菜、水果样品中锰(Ⅱ)的测定。     

考马斯亮蓝G动力学光度法测定痕量铁的研究

研究了在稀盐酸介质中 ,α,α-联吡啶存在下 ,铁催化溴酸钾氧化考马斯亮蓝G,使其褪色这一新的指示反应及其动力学条件 ,建立了测定痕量铁的新方法。方法的检出限为 2 .2 6× 1 0 - 10 g/ m L,线性范围 0～ 0 .2 4μg/ 2 5 m L,用于食品及水中痕量铁的测定 ,结果满意     

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。     

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.     

探究“铁的锈蚀条件”实验创新设计

设计了铁的锈蚀实验,说明了铁钉的处理方法,增加了温度、酸、碱的影响条件,实现了铁跟蒸馏水及空气中氧气快速反应而生锈,使实验在5 min左右就能够得到准确的结果。