微波消解/等离子体发射光谱法测定蒙药哈日阿-布日-16中的多种元素

采用高压密封微波消解,以V(HNO3) V(HClO4)=5 1为溶样试剂,电感耦合等离子体原子发射光谱法(ICP-AES)测定了蒙古药—哈日阿-布日-16中的镁、钙、铬、锰、铁、钴、镍、铜、锌、锶、银、镉、铅等金属元素的含量。结果表明,回收率为99.5%~104.7%,RSD为0.4%~2.3%。哈日阿-布日-16中的多种金属元素,尤其镁、钙、锌、锶的含量较高,未测到有铅、银等元素。     

电感耦合等离子体原子发射光谱法测定枸杞中11种元素含量

采用电感耦合等离子体原子发射光谱法测定了枸杞中锌、铅、锰、铁、铬、镁、钙、铜、钠、钾和镉11种元素含量。选择硝酸(2+98)溶液作为介质,选择波长为213.86,220.35,257.61,259.94,267.72,279.08,324.75,317.93,589.59,766.49,226.50 nm 11条谱线依次作为测定锌、铅、锰、铁、铬、镁、钙、铜、钠、钾和镉的分析线,测得11种元素的检出限(3δ)均低于0.07 mg·L~(-1),相对标准偏差(n=11)在0.72%～2.40%之间。比较了常规湿法消化法、高压消化罐法和微波消解法处理样品对测定结果的影响。研究表明,高压消化罐法和微波消解处理样品精密度好。     

金花茶花朵中微量元素的研究

对金花茶花朵不同部位微量元素的含量进行了分析研究.采用微波消解样品,电感耦合等离子体原子发射光谱法同时测定钾、钠、钙、镁、磷、铜、铁、锌、锰、钼、镍、铅、镉、铬的含量.结果表明,花朵中富含微量元素,且而各元素含量在花瓣、花蕊、花粉之中差异较大,为进一步开发金花茶的花朵提供依据.     

微波消解样品-电感耦合等离子体原子发射光谱法测定镍精矿中10种金属元素

采用微波消解样品-电感耦合等离子体原子发射光谱法同时测定镍精矿样品中铝、钙、钴、铬、铜、锰、镁、镍、铅、锌等10种金属元素的含量。0.200 0g试样置于消解罐中,先后加入盐酸2mL、硝酸6mL及氢氟酸1mL,密闭罐盖按设定的微波消解程序进行消解。试验选择铝、钙、钴、铬、铜、镁、锰、铅、锌和镍的分析线分别为308.215,317.933,228.616,267.716,324.745,279.079,257.610,220.353,206.200,231.604nm,配制工作曲线时采用基体匹配的方法消除基体干扰。方法用于镍钴矿标准样品(GBW 07283)和镍精矿实际样品的分析,此方法的测定值与认定值及国标方法的测定值相一致。方法的回收率在95.8%～103.1%之间,相对标准偏差(n=6)均小于4.5%。     

微波消解-电感耦合等离子体发射光谱(ICP-OES)法测定固体中兽药制剂中金属元素

为了实现对固体中兽药制剂中金属元素的准确测定,采用硝酸-双氧水及微波消解进行样品前处理,消解后置消解管于赶酸仪中170℃赶酸,采用微波消解和电感耦合等离子体发射光谱（ICP-OES）法相结合对固体中兽药制剂中铬、砷、镉、铅、钠、镁、钾、锰、铁、铜、锌、硒、钙、磷等14种元素同时测定,轴向观测方向,内标法定量。消解及赶酸效果理想,整个过程安全、高效、无损。对消解方式进行了考察,并对消解酸体系及消解温度进行了优化,选择了最优的赶酸温度及元素分析谱线,同时也通过试剂加标回收、样品加标回收、样品处理液加标回收相比较的方式验证了方法的可行性。结果表明,铅、镉、铬、砷在0.001～0.01 μg/mL,锰、铜、硒在0.002～0.02 μg/mL,铁、锌在0.1～1.0 μg/mL,镁、钙在1.0～10.0 μg/mL,钠、钾、磷在2.0～50.0 μg/mL之间线性关系良好,相关系数（r）均大于0.9990,各元素方法检出限在0.1～1.0 mg/kg之间,平均回收率在90.0%～110.0%,精密度RSD小于10%（n=5）。该方法前处理简便快捷,干扰小,重现性好,灵敏度高,可同时测定多种元素,满足批量测定固体中兽药制剂中铬、砷、镉、铅、钠、镁、钾、锰、铁、铜、锌、硒、钙、磷等14种元素定量分析的要求。     

微波消解-火焰原子吸收光谱法测定中药女贞子中9种金属元素

用微波消解法处理样品,用硝酸-过氧化氢(4+1)混合溶液作为消解剂进行微波消解,火焰原子吸收光谱法测定了中药女贞子中钙、镁、钾、钠、铁、锶、锰、铜和锌元素含量。9种元素检出限(3S/N)在0.000 6~0.024 8 mg.L-1之间,回收率在93.0%~107.3%之间,相对标准偏差(n=10)在0.86%~4.39%之间。试验结果表明:女贞子中钾、钙、镁、铁、钠、锌、锰、铜和锶质量分数分别为16 940,1 790,1 640,467.8,116.0,24.5,15.0,9.6,1.9μg.g-1,锌与铜含量的比值为2.55。由此可见,女贞子中钙、镁、钾元素含量丰富,铁含量也较高。为探讨中药金属元素种类及含量与治疗心血管疾病的关系等提供有用数据。     

超级微波消解-电感耦合等离子体发射光谱（ICP-OES）法测定土壤中18种元素

为提高土壤多元素同时检测的效率,采用超级微波消解-电感耦合等离子体发射光谱法测定土壤中钾、钠、钙、镁、铜、铁、锰、锌、磷、硫、硼、砷、镉、铬、铅、钴、镓、锂等18种元素含量。比较了超级微波消解、常规微波消解和电热板消解的处理效果,采用超级微波消解法对样品进行前处理,并优化了消解条件。在最优条件下,各元素的检出限在0.05~20 mg/kg,加标回收率在86.2%~107.5%,RSD在0.1%~3.0%,方法准确度及精密度可以满足多元素同时测定的需求,且该方法具有简单、快速、成本低、用酸量少、重现性好等特点。     

微波消解-电感耦合等离子体质谱法探讨青海不同产地枸杞中微量元素的差异

采集了生长于青海省6个不同地区的枸杞样品150个,并制取分析用样品。每个样品称取约0.5g置于石英管中,加入水1mL和硝酸4mL,按程序进行微波消解,所得溶液在电感耦合等离子体质谱工作条件下测定其中24种微量元素(钾、钠、钙、镁、铁、锌、铜、锰、钴、镍、铅、砷、镉、铬、硒、钼、锑、锶、锡、镨、钆、镝、汞、铽)。用各元素的标准溶液绘制标准曲线。测得各元素的检出限(3s)在0.008～10μg·L-1之间。选用都兰地区的样品进行精密度和回收试验,24种元素测定值的相对标准偏差(n=6)在0.95%～6.6%之间。在回收试验中,称取4份样品,其中1份样品的测定值为本底值,其余3份样品中分别加入3个浓度水平的15种元素的标准溶液,按方法测得各元素的含量,计算得回收率在85.0%～107%之间。运用仪器自带的MPP软件对所有样品所测得的24种元素的分析数据进行主成分分析和聚类分析。结果表明:钠、镁、钙、锰、铁、钴、镍、铜、锌、镉、铅、钼、镨等元素含量在不同个体样品中差异较明显;来自德令哈与格尔木的样品区分度较好;都兰、乌兰和诺木洪的样品散布比较广,样品间的差异不明显;在青海省各地产出的枸杞的24种元素中,钆与镝存在高度相关。     

微波消解ICP-OES法快速测定雪莲果中的微量元素

微波消解雪莲果样品后,等离子体发射光谱仪一次进样曝光快速测定了钾、钠、钙、镁、铜、铁、锌、锰、钼、镍10种微量元素。结果表明,雪莲果中富含钾、钙、镁等元素。该法一次消解样品、多元素同时测定,准确、快速、精密度高,符合分析要求。     

微波消解样品-火焰原子吸收光谱法测定淡竹叶中痕量元素

产自3个不同地区的淡竹叶样品用硝酸经微波辅助消解,采用火焰原子吸收光谱法测定所得样品溶液中锌、铁、铜、锰、钾、钙、钠、镁、镍、铅、铬、钴、铝和硒等14种痕量元素的含量。14种元素的质量浓度在一定的范围内均与其吸光度呈线性关系。以1#样品为基体,加入适量9种痕量元素的标准溶液做方法的回收试验,测得回收率在98.1%～108.0%之间,测定值的相对标准偏差(n=5)均小于8%。     

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.     

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。     

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^-。     

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.     

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。