溴酚红-过氧化氢催化光度法测定痕量锌

在稀氢氧化钠介质中,Zn2+催化过氧化氢氧化溴酚红的褪色反应,通过试验确定了测定条件,建立了一个催化动力学光度法测定痕量锌的方法。Zn2+的检出限为1.5×10-7g.L-1,线性范围为0~4.8×10-2mg.L-1,方法用于测定头发中痕量锌。     

催化过氧化氢氧化杨梅红色素褪色光度法测定痕量锌

报道了杨梅红色素的提取与性质。基于加热条件下 ,Zn2 + 催化过氧化氢氧化杨梅红色素灵敏的褪色反应 ,提出了测定痕量锌的新方法。所建立的方法对Zn2 + 的线性范围为 0 .2～ 1 .0 μg L,并成功地用于发样和奶粉中锌的测定     

浊点萃取分光光度法测定水样中的痕量锌(Ⅱ)

为建立浊点萃取预富集测定水样中痕量锌的新方法,在表面活性剂TritonX-114存在下,利用5-Br-PADAP与锌(Ⅱ)产生显色反应的性能,采用分光光度法测定了水样中的痕量锌。结果表明,在pH8.5的NH3-NH4Cl缓冲体系中,锌(Ⅱ)与5-Br-PADAP形成紫红配合物,其最大吸收波长为λ=555 nm,摩尔吸光系数为ε=1.284×105L.mol-1.cm-1,检测限为0.003 7μg.mL-1.锌含量在0~1.2μg.mL-1范围内服从比尔定律。该法有较好的选择性,具有低毒、高效、安全、简便等特点,直接用于水样中痕量锌的测定,结果满意,重复6次测定相对标准偏差为2.18%。     

双波长双指示剂-催化动力学光度法测定奶粉中的锌

研究发现在HCl介质中,痕量锌对H2O2氧化甲基紫和亚甲基蓝褪色具有强烈的催化作用,通过测量580 nm和668 nm处催化反应体系和非催化反应体系吸光度的变化,建立了双波长双指示剂催化动力学光度法测定痕量锌的新方法。在最佳实验条件下,线性范围为1.5~60μg/L,线性方程为ΔA=0.0169ρZn2+(μg/mL)+0.0019,r=0.9982,方法检出限为0.84μg/L。该方法可用于奶粉痕量锌的测定。     

催化过氧化氢氧化镍-依来铬红B络合物褪色光度法测定痕量汞

基于在PVA存在下 ,痕量汞催化过氧化氢氧化镍 依来铬红B络合物的褪色反应 ,建立了催化褪色光度法测定痕量汞的新方法。汞浓度在 0 .0 1～ 0 .0 6 μg/L范围内符合比尔定律 ;检出限为 1 .2× 1 0 -9g/L。用于人发和废水等样品中痕量汞的测定 ,获得满意的结果。     

溴酸钾氧化偶氮胂动力学光度法测定钯

根据在稀 H2 SO4 介质中 ,痕量钯 ( )对溴酸钾氧化偶氮胂 褪色反应的显著的催化作用 ,建立了测定痕量钯的催化动力学光度法。方法检出限为 0 .1 3μg/L,测定范围为 0～ 8.0 μg/L。可用于矿石中痕量钯的测定。     

催化过氧化氢氧化杨梅红色素裉色光度法测定痕量锌

报道了杨梅红色素的提取与性质。基于加热条件下，Zn^2 催化过氧化氢氧化杨梅红色素灵敏的褪色反应，提出了测定痕量锌的新方法。所建立的方法对Zn^2 的线性范围为0．2－1．0μg/L，并成功地用于发样和奶粉中锌的测定。     

铬兰黑R-H_2O_2催化光度法测定痕量锌

研究了在稀硫酸介质中,Zn催化过氧化氢氧化铬兰黑R褪色反应,建立了测量痕量锌的新方法,Zn2+ 的检测限为1.5×10-10g/mL,线性范围为 0 ~ 3.1×10-2 mg / mL,该法用于测定头发中的痕量锌,结果满意。     

硫化镍试金富集-催化光度法测定痕量铑

在铑的硫酸配合物催化高碘酸钾氧化甲基红退色反应的基础上 ,提出了催化光度测定痕量铑的新方法。铑质量浓度在 0～ 0 .1 μg/mL范围内符合比尔定律 ,测定下限为 4× 1 0 - 3μg/mL。对于试样中质量分数为 1 6× 1 0 - 5%Rh的测定 ,RSD为 9 2 %,平均回收率为 89%。测定之前 ,痕量铑用小硫化镍试金富集分离。方法已用于原矿和尾矿中痕量铑的分析。     

动力学光度法测定痕量锌的研究

在微酸性介质中 ,痕量锌对过氧化氢氧化络黑T褪色反应有催化作用 ,提出了催化动力学光度法测定痕量锌的新方法 ,研究了该方法的适宜反应条件及动力学性质。方法的检出限为 6.9μg·L-1,测量线性范围为 2～ 64μg·L-1,用于人发及食品中锌的测定 ,获得了满意的结果     

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。