FAAS法分析当归、黄芪及当归补血汤中金属元素的形态

采用正辛醇-水分配体系模拟中药水煎液在人体肠胃中的分配情况,应用火焰原子吸收光谱法测定了当归、黄芪及当归补血汤中锌、铁、锰、铜、镁、钙、镍7种金属元素在药材中的总含量,以及水煎液中各金属元素的水溶态、醇溶态含量,探讨了配伍和酸度对水煎液中金属元素含量的影响。实验结果表明,中药中金属元素的形态与中药成分、配伍情况及作用靶位(肠胃)的酸度有关,配伍及酸度对中药中金属元素的溶出率及水煎液中金属元素的形态影响较大。     

氢化物发生-原子荧光光谱法(HG-AFS)测定特硬铅合金中硒和碲

建立了氢化物发生-原子荧光光谱法(HG-AFS)测定特硬铅合金中硒和碲的分析方法。试样经硝酸和酒石酸溶解,硫酸沉淀分离基体铅元素。移取部分试液,在40%盐酸介质中直接用氢化物发生-原子荧光光谱法(HG-AFS)测定样品中的硒;另移取部分试液,加入氢溴酸挥发除去砷、锑、锡、硒等元素,在40%盐酸介质中用氢化物发生-原子荧光光谱法(HG-AFS)测定样品中的碲。考察了测定的最佳条件、铅及共存元素对测定的影响。测定硒和碲的相对标准偏差分别为7.5%～9.3%和3.6%～13.0%,加标回收率分别为88%～92%和98%～102%。准确度和精密度均能满足分析需要,具有较强的实用性。     

植物样品中痕量砷的形态分析研究进展

介绍了近十年来国内外植物样品中包括药用植物中砷的形态分析研究进展。由于植物中的砷含量甚低,其主要的检测手段是:氢化物电感耦合等离子体原子吸收光谱法(HG-ICP-AAS)、高效液相色谱-等离子体质谱法(HPLC-ICP-MS)、氢化物原子荧光光谱法(HG-AFS)。     

一次消解土壤样品测定汞、砷和硒

建立了测定土壤中3种挥发性元素(汞、砷、硒)的一次消解方法,确定以程序控温石墨自动消解仪+王水-氢氟酸-硼酸络合敞开体系为最佳消解体系,采用氢化物发生-原子荧光光谱法(HG-AFS)分别测定同一消解液中汞、砷、硒的含量.采用国家标物中心有证标准物质土壤环境样品GSS-1~GSS-8进行了方法验证,结果均符合标准偏差的允许范围.此消解方法相比于现行标准方法,避免了针对各元素的分次处理,简化了消解步骤,节省了前处理时间,减少了试剂消耗,提高了实验效率,适用性广、灵敏度高、检出限低,尤其适合批量样品的微量/痕量元素分析,可作为一种大规模土壤样品中重金属污染监测和治理的快捷方法.     

流动注射-氢化物发生原子发射光谱法测定板蓝根中的有害元素

使用流动注射-氢化物发生-电感耦合等离子体原子发射光谱联用技术同时测定中药板蓝根中微量有害元素砷、铅、镉和汞的含量。对影响分析信号的主要工作条件进行了选择和优化。砷、铅、镉和汞的检出限分别为0．51、1．5、0．33和0．25μg／L;其回收率分别为98%、101%、103％和108％。本法用于中药板蓝根中微量有害元素的分析,结果满意。     

西红花中金属元素的分析

西红花为鸢尾科植物番红花(Crocus sativus L)的干燥柱头.具活血化瘀,凉血解毒,解郁安神等功效.采用原子吸收分光光度法(AAS)测定西红花中部分金属元素的含量,通过对其宏量元素及微量元素含量的测定结果,分析了西红花中金属元素及其生理作用与药用功效之间的关系.随着元素医学的不断发展,金属元素与中药药效关系及对生物体系的作用有待研究.     

催化裂化催化剂中微量金属元素的测定

原料油中的微量金属元素会污染催化裂化催化剂而使其中毒,对于使用中的再生、平衡催化裂化催化剂进行微量金属元素含量分析,可以有效地指导炼油厂的生产．通过对检出限、重复性以及准确性的考察．表明等离子发射光谱法测定催化剂中微量金属元素含量检出限低、重复性好、准确度高、且具有多元素同时测定以及线性范围宽的特性,是催化裂化催化剂中金属元素含量快速测定的最有效方法之一．     

黄芪中铅的初级形态分析

黄芪是我国盛名的大宗传统中药材,也是常用的中药及食疗药膳品.关于黄芪的研究较多,但主要集中于有机成分与药理作用的研究.中草药药效不仅同药材中的有机成分有关,与微量元素之间关系已被越来越多的研究所证实[1,2].因此对中药微量元素的研究仅仅提供元素总量的信息是不够的,更需要对金属元素的存在化学形态进行分析[3].中药中微量元素的形态分析属一新研究领域,文献报道较少[4-7].本实验选取不同产地的黄芪药材,采用微波消解样品,氢化物发生-电感耦合等离子体原子发射光谱法(HG-ICP-AES)[8],对不同产地黄芪中重金属铅进行了形态分析,这对药材道地性研究,质量控制具有积极的意义.     

氢化物发生原子荧光光度法测定水中微量砷

砷是一种对人体有害的元素,在饮用水质量标准中对砷的含量有着严格的要求,建立水中微量砷的快速检测方法有重要意义.氢化物发生原子荧光光度法测定水中微量砷是在酸性条件下,以硼氢化钾为还原剂,使砷与硼氢化钾和酸生成氢化物气体,由载气(氩气)载入石英原子化器,用砷空心阴极灯作激发光源,产生原子荧光,其荧光强度在一定范围内与砷含量成正比.该方法克服了其他分析方法操作繁琐、灵敏度低的缺陷,具有灵敏度高、干扰少、分析速度快的特点.本文探讨应用原子荧光光度计测定水中微量砷的方法.     

液体硅肥中砷形态的氢化物发生原子荧光光谱分析

本文应用氢化物发生-原子荧光光谱法(HG-AFS)测定了液体硅肥中不同形态的砷含量。研究了酸介质、还原剂和增感剂对砷的荧光信号的影响。实验确定酸介质为2.5 mol.L-1HCl,还原剂和增感剂为5%硫脲 5%抗坏血酸混合溶液。在选定的实验条件下测得硅肥中三价砷、五价砷及总砷的含量分别为5.08 ng.L-1、0.72 ng.L-1、5.80 ng.L-1。三价砷和五价砷的检出限分别为72.0 ng.L-1和153 ng.L-1;方法的精密度为2.2%~4.1%,回收率为96.5%~104%。     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

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.     

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.

     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

Calculation of enthalpies of hydrogenation of hydrocarbons

Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.     

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。