7-（4-安替吡啉偶氮）-8-羟基喹啉-5-磺酸的合成及其与铜的显色反应

7-（4-安替吡啉偶氮）-8-羟基喹啉为安替吡啉单偶氮类试剂中的一种，该试剂可与镓（Ⅲ）、铟（Ⅲ）、铋（Ⅲ）、钯（Ⅱ）、镍（Ⅱ）、钴（Ⅱ）、铜（Ⅱ）、铁（Ⅱ）等离子发生显色反应。本文在其5位引入磺酸基，合成了7-（4-安替吡啉偶氮）-8-羟基喹啉-5-磺酸（分子式为C20H17N5O5S）试剂。     

7-(4-安替吡啉偶氮)-8-羟基喹-5-磺酸的合成及其与铜的显色反应

7-(4-安替吡啉偶氮)-8-羟基喹啉为安替吡啉单偶氮类试剂中的一种,该试剂可与镓(Ⅲ)、铟(Ⅲ)、铋(Ⅲ)、钯(Ⅱ)、镍(Ⅱ)、钴(Ⅱ)、铜(Ⅱ)、铁(Ⅱ)等离子发生显色反应[1,2].本文在其5位引入磺酸基,合成了7-(4-安替吡啉偶氮)-8-羟基喹啉-5-磺酸(分子式为C20H17N5O5S)试剂.该试剂分子的共轭体系增大,分析功能基及成键原子的电荷密度大大提高,可提高显色反应的灵敏度.文献[3～5]研究表明,8-羟基喹啉-5-磺酸-7-偶氮化合物可能是一类较有价值的光度分析试剂.本文以4-氨基安替吡啉的重氮盐为重氮组分与8-羟基喹啉-5-磺酸进行偶合反应,合成了7-(4-安替吡啉偶氮)-8-羟基喹啉-5-磺酸,产物的结构用红外光谱进行了表征,并研究了该试剂与铜的显色反应.     

以钛-二安替吡啉甲烷-变色酸三元络合物的形式分光光度法测定钛

变色酸(XK)、二安替吡啉甲烷(дAM)是测定钛的两种重要试剂。近年来ганаго等研究了钛-二安替吡啉甲烷-溴代邻苯三酚红及钛-二安替吡啉甲烷-变色酸的形式分光光度法测定钛。我们对后者进行了研究,经试验发现显色液中有白色针状结晶析出。我们加入了乙醇防止了沉淀析出并对多种离子进行了干扰试验。实验证明本法是一个高选择性、精密度较好的快速分析法。     

偶氮氯膦Ⅲ-铌(Ⅴ)配合物光谱探针测定血清蛋白质

研究了偶氮氯膦Ⅲ-铌（Ⅴ）配合物与牛血清白蛋白（BSA）的反应体系。实验表明,在pH 4.4的HAc-NaAc缓冲溶液中,随着BSA量的增加,偶氮氯膦Ⅲ-铌（Ⅴ）配合物在572 nm波长处吸收峰也随着减小。据此建立了以偶氮氯膦Ⅲ-铌（Ⅴ）配合物为光谱探针,分光光度测定蛋白质的新方法。牛血清白蛋白在0-38 mg/L范围内与体系的褪色程度呈良好的线性关系,其相关系数为r=0.9992,摩尔吸光系数为5ε72=3.40×10^5L.mol^-1.cm^-1。方法已用于人血清蛋白中蛋白质的测定。     

以硫醚为主链的螯合树脂研究Ⅰ.4-氨基安替吡啉树脂和乙基原磺酸基树脂的合成及吸附性能

聚环硫氯丙烷或环硫氯丙烷与环氧氯丙烷共聚物，在少量二乙烯三胺存在下制得交联预聚物，将交联预聚物与4－氨基安替吡啉（4AAP）或乙基原磺酸钾（PEA）反应，制得四种侧链带氨基安替吡啉，乙基原碘酸基的新型螯合树脂。它们对贵金属具有优良的吸附性能和高的吸附选择性。并通过X－射线光电子能谱初步探讨了树脂对金属离子的螯合作用。     

稀土与二苯甲酰甲烷及与安替吡啉三元配合物的合成和性质

稀土与二苯甲酰甲烷及与安替吡啉三元配合物的合成和性质李夏王娓胡秋菊（首都师范大学化学系北京１０００３７）关键词稀土配合物二苯甲酰甲烷安替吡啉安替吡啉具有很好的协同萃取效果［１］。金林培等对二苯甲酰甲烷及与安替吡啉所形成的二元配合物进行了ＩＲ、低温荧光...     

钒(Ⅴ)-2-(2-噻唑偶氮)-5-二甲氨基苯甲酸显色反应的研究

钒是具有重要用途的元素,其测定受到重视.二安替比林甲烷类[1]及杂环偶氮苯酚类显色剂[2,3]测定钒灵敏度和选择性较高,变色酸偶氮类显色剂[4-5]的应用也曾有报道,而杂环偶氮苯甲酸类显色剂研究较少[7,8].本文研究了钒(Ⅴ)与2-(2-噻唑偶氮)-5-二甲氨基苯甲酸(TAMB)的显色反应,结果表明,在pH 3.5～3.8甲酸-NaOH缓冲介质中,钒(Ⅴ)与TAMB反应生成一种稳定的可溶于水的蓝色配合物.     

2—（4—安替比啉偶氮）—5—二甲氨基苯胺合成及其与钴（Ⅱ）显色反应的研究

合成了新的安替比啉偶氮试剂2-(4-安替比啉偶氮)-5-二甲氨基笨胺(AADMAA)。在pH4时,AADMAA与Co(Ⅱ)形成红色络合物,λ_(max)为520nm,ε为6.48×10~4。钴量在0—20μg/25mL符合比尔定律,选择性较好,加入适当的掩蔽剂可以不经分离直接测定某些物料中微量钴。     

石煤渣中痕量铌的高灵敏光度法测定

1引言利用Nb（Ⅴ）-SCN-RhB-PVA高灵敏显色体系。在聚乙烯酸（PVA）存在下,铌（Ⅴ）与疏氰酸盐形成配阴离子再和罗丹明B（RhB）形成较稳定的离子缔合物,可用光度祛在水相中直接测定铌（Ⅴ）。通过试验,确立了体系反应的最佳条件,在PVA介质中,离子缔合物的λmax=565nm,ε＝7．9×105·mol－1·cm－1,铌（Ⅴ）量在0－0．2mg／L范围内服从比耳定律。本法用于测定石煤渣中痕量铌,获得了满意结果。2实验部分2．1仪器和试剂721型分光光度计（上海第三分析仪器厂）;pffe3型酸度计（上海第二分析仪器厂）;501型超级恒温器（上海实…     

在表面活性剂存在下2-(3,5-二溴-2-吡啶偶氮)-5-二甲氨基苯酚与铋的显色反应的研究

曾有人研究了数种吡啶偶氮类化合物与铋的显色反应,用于络合滴定时的金属离子指示剂和萃取光度法的显色剂。本文研究了另一种吡啶偶氮化合物2-(3,5-二溴-2-吡啶偶氮)-5-二甲氨基苯酚(简称3,5-Br_2-DMPAP)与铋的显色反应。在Tween-80存在下,水相显色,具有较高的灵敏度且显色速度快、稳定时间长。用邻菲啰啉作掩蔽剂使该反应具有较好的选择性,采用巯基棉进行分离可用于铜、锌等有色金属中微量铋(0.00X％)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。