二甲氧基羟基苯基荧光酮光度法测定生物样品中锗

研究了二甲氧基羟基苯基荧光酮光度法测定锗。在H3PO4 介质中 ,TritonX 10 0存在时 ,锗与二甲氧基羟基苯基荧光酮形成 1∶2橙红色络合物 ,最大吸收在 5 0 5nm波长处 ,表观摩尔吸光系数为 1.8× 10 5L·mol- 1·cm- 1,并且具有灵敏度高、选择性好的特点。当锗含量在 0～ 7μg/2 5ml范围内符合比耳定律。已用于茶叶、党参和药物中锗的测定     

固相分光光度法测定枸杞中的痕量锗

建立了以苯基荧光酮为显色剂固相分光光度法测定痕量锗的新方法。在0 .1 5 mol/L HCl介质中 ,锗吸附于树脂上 ,再与苯基荧光酮显色 ,直接在最大吸收波长 5 35 nm处对树脂相进行测量。锗含量在 0～ 2 5 0 μg/L范围内符合比尔定律 ,表观摩尔吸光系数为 2 .6× 1 0 6L· mol-1· cm-1。该法已应用于枸杞中痕量锗的测定     

新显色剂三甲氧基苯基荧光酮光度法测定锗

研究了新试剂三甲氧基苯基荧光酮光度测定锗的方法。在 3mol/ m LH3PO4 介质中 ,当 Triton X- 1 0 0存在时 ,锗与三甲氧基苯基荧光酮形成 1∶ 2橘红色络合物 ,最大吸收在 5 0 5 nm波长处 ,摩尔吸光系数为 1 .7× 1 0 5L· mol-1·cm-1且具有高的选择性。当锗含量在 0～ 6μg/ 2 5 m L范围内符合比尔定律。已用于大蒜与枸杞子中锗的测定     

用罗丹明B-锗钼蓝分光光度法测定植物性中药和食品中微量锗的研究

在酸性介质中，非离子表面活性剂聚乙烯醇存在下，用罗丹明B－锗钼蓝离子缔合物水相分光光度法测定食品、中药中的微量锗。缔合物最大吸收波长为580nm，摩尔吸收系数为1．02×105mol·L－1·cm－1，0～0．40mg·L－1锗满足比尔定律。方法精密度为5．9％，回收率为95％～105％。     

氢化物发生-分光光度法测定中药中微量锗

研究了在L 半胱氨酸存在下 ,锗与硼氢化钠反应产生锗化氢挥发分离 ,再用显色剂 2 (5 NO2 2 吡啶偶氮 ) 5 二乙氨基酚 (5 NO2 PADAP) ,次氯酸钠 ,六次甲基四胺的混合液吸收显色 ,有色溶液在 5 6 4nm处有最大吸收 ;摩尔吸光系数为 1 84× 10 5L·mol-1·cm-1,锗在 0～ 5 0 0 μg/L范围内服从比尔定律 ;样品标准加入回收率为 89%～ 97% ;相对标准偏差小于 6 .3% ;用本法对中药材中微量锗的测定 ,结果令人满意     

巯基葡聚糖凝胶分离富集-光度法测定微量有机锗和无机锗

研究了巯基葡聚糖凝胶分离富集 光度法测定微量有机锗和无机锗。在HCl介质中,在抗坏血酸(Vc)、溴化十六烷基三甲基胺存在下锗与2,4 二甲氧基苯基荧光酮形成有色络合物,其ε=1.12×105L·mol-1·cm-1,锗浓度在0～12μg/25mL范围内符合比耳定律。方法可用于多种样品中痕量有机锗和无机锗的测定,结果令人满意。     

速效胃宁冲剂中锗含量分析

用分光光度法测定了五批速效胃宁冲剂中锗的含量,结果表明,用该法测定药物中的锗含量,摩尔吸光系数为1.0888*10^4L.mol^-1.cm^-1,线性范围0．050－0．250mg.L^-1,回收率在98．43％－103．19％,五批速效胃宁冲剂锗含量甚微,这为临床合理用药提供了有用数据。     

耐尔蓝-12-钼锗酸-聚乙烯醇体系测定锗

本文报告了在聚乙烯醇(PVA)存在下,在高氯酸水溶液中以耐尔蓝(NB)-12-钼锗酸体系灵敏光度法测定锗。讨论了定量形成12-钼锗酸(GeMo)及耐尔蓝-12-钼锗酸离子缔合物(NB-GeMo)的适宜条件。NB-GeMo的最大吸收位于605nm,表观摩尔吸光度ε值为9.08×10~5L·mol~(-1)·cm~(-1),服从比耳定律范围为0～4.0μgGe/25ml,至少稳定16h。用平衡移动法和摩尔比法测定了主要组分的摩尔比为NB:GeMo=9:1。红外光谱图表明,高氯酸根参与了缔合物组成。本法已用于实物中锗的测定,结果满意。     

克霉唑与氯冉酸的荷移反应及其测定

克霉唑与氯冉酸在丙酮介质中发生电荷转移反应 ,生成 1∶1型络合物 ,该络合物的λmax=5 2 5nm ,表观摩尔吸光系数是 1.2 2× 10 3 L·mol-1·cm-1,药物浓度在 0～ 30 0mg/L范围内符合比耳定律 ,6次测定的相对标准偏差为 1.4 % ,回收率在 97%以上。用拟定的方法测定药物片剂中有效成分的含量 ,结果与药典方法相符     

2-羟基-3-甲氧基苯基荧光酮分光光度法测定中药中痕量锗

研究了新试剂2羟基3甲氧基苯基荧光酮(HMPF)与锗的显色反应。建立了测定几种中药中锗的光度分析方法。在磷酸(2+1)介质和非离子型表面活性剂OP介质中,2羟基3甲氧基苯基荧光酮与锗发生灵敏的显色反应,其最大吸收峰为505.50nm,表观摩尔吸光系数为1.56×105L·mol-1·cm-1,锗量在0～12μg/25mL符合比耳定律。锗与试剂的显色反应有良好的选择性,绝大多数金属离子特别是钙、镁、铁、锌和钼有非常高的允许量,可直接应用于几种中药中锗的测定,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.     

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.

     

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。     

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:     

解决能源问题的新途径--光解水制氢的研究

面对日益枯竭的能源危机,氢能是一种洁净、最有前景的替代能源。目前在各种制氢的方法中光催化分解水制氢的研究最多,光解水过程中催化剂最关键,本文对利用太阳能光解水的途径、提高光催化反应效率以及光催化剂的开发研究进行了综述。