铁-4,7-二苯基-1,10-菲啰啉-TritonX-100体系析相法测定痕量铁的研究

本文把析相法应用于Fe(Ⅱ)-4,7-二苯基-1,10-菲啰啉-Triton X-100体系测定天然水中痕量铁。在pH3.8,90℃,水浴加热70分钟,析相完全。λ_(max)=532nm。在含铁量0—40μg/L范围内工作曲线为直线。水中常见离子除Cu~(2+)以外均无干扰。用于测天然水中痕量铁得到满意的结果。     

盐酸胍中微量铁的光度测定

本文考察了盐酸胍对邻菲口罗啉光度法测定微量铁的实验条件的影响，并建立了邻菲口罗啉分光光度法直接测定盐酸胍中微量铁含量的方法。当盐酸胍中铁含量为5μg／g时，相对标准偏差为2％。     

以4,7-二苯基1,10-邻菲罗啉为试剂萃取分光光度法测定高纯氧化锌中的微量铁

用4,7-二苯基1,10-邻菲罗啉(BPT)测定微量铁,灵敏度高,重现性好,广泛用于各种材料和钕玻璃中微量铁的测定,但少数金属离子如Zn~(2+)等干扰测定。虽曾有人介绍过EDTA为掩蔽剂,用1,10-邻菲罗啉比色测定金属锌和镉中的铁,但测定灵敏度低,难以满足要求。本文提出以EDTA为掩蔽剂,酒精为增溶剂,直接用BPT溶剂萃取分光光度法测定高纯氧化锌中的微量铁,取得了满意的结果。     

铁-4,7-二苯基-1,10-菲啰啉-Triton X-100体系的三元胶束络合物分光光度法的研究

用4,7-二苯基-1,10-菲啰啉(BPT)为试剂萃取分光光度法测定水、血清、高纯氧化锌中微量铁已有报导,但手续繁杂。用非离子表面活性剂Triton X-100胶束增溶BPT-Fe体系分光光度法未见报导。本文用Triton X-100增溶BPT-Fe体系,发现在pH为1.9-4.7乙酸介质中,Fe-BPT-Triton X-100可形成稳定的三元胶束络合物。在532.2nm处有最大吸收,摩尔吸光系数ε_(532.2)为2.2×10~4。除Cu~+离子外,其他常见离子均不干扰。用于测定天然水及海洋生物中微量铁,结果良好。     

4,7-二苯基-1,10-菲罗啉作显色剂水相吸光光度法测定铁价态

研究了Fe(Ⅱ)与4,7-二苯基-1,10-菲罗啉的水相显色反应。试验表明,在pH1.6的盐酸-氯化钾缓冲液中,当有吐温-80存在时,Fe(Ⅱ)与4,7-二苯基-1,10-菲罗啉形成一稳定的配合物。该配合物的λ_(max)为536nm,ε为2.2×10~4,Fe(Ⅱ)量在0～14/μg/10ml范围内符合比耳定律。柠檬酸三铵可消除Fe(Ⅲ)对Fe(Ⅱ)的影响,加入盐酸羟胺,可测定铁的总量。所拟方法用于水样中的Fe(Ⅱ)和Fe(Ⅲ)分析,结果满意。     

分子荧光法测定水中的微量铁

基于Fe（Ⅱ）与邻菲口罗啉生成络合物使其荧光猝灭的特性,讨论了在室温下,pH 5.5的乙酸-乙酸铵的缓冲介质中,以λex=270 nm为激发波长,于eλm=365 nm波长处测定该络合物荧光强度。结果表明Fe（Ⅱ）质量浓度在0.8-120.0 ng/mL范围内与络合物的荧光强度具有良好的线性关系,相关系数0.9994,检出限0.50 ng/mL。对60 ng/mL的Fe RSD（n=9）为2.8%。Fe的回收率为98.03%-102.9%。方法已用于水中微量铁的测定。     

铁(Ⅲ)-硫氰酸钾-乙基紫三元络合物光度法测定水中微量铁

建立铁(Ⅲ)-硫氰酸钾-乙基紫三元络合物光度法测定水中微量铁的新方法,该络合物的最大吸收波长为510nm,表观摩尔吸光系数ε=9.26×10~4L/(mol·cm),铁(Ⅲ)在0-20μg/(25mL)范围内符合比耳定律,线性回归方程为A=0.01 0.386X,相关系数r=0.9999,回收率为96.5％～98.0％,检出限为0.0082μg/mL,测量结果的相对标准偏差为1.64％～1.79％。     

链霉素、1,10-邻菲啰啉体系测定铁强化食品中铁(Ⅲ)的分光光度法研究

在pH=5.0时,采用链霉素、1,10-邻菲啰啉作为显色剂,与Fe(Ⅱ)形成三元络合物测定Fe(Ⅱ)。此方法灵敏度较高(ε=4.35×10~4L·mol~(-1)cm~(-1))。线性范围较宽(0.14μg/ml～28μg/ml)。常见离子无干扰。显色相当稳定。对铁强化醋,铁强化固体饮料中Fe(Ⅱ)进行了测定,回收率分别为93～105％和92～112％。相对标准偏差分别小于5.98％和3.88％。     

1-（4-硝基苯基）-3-（2-苯并咪唑）-三氮烯的合成及与铜（Ⅱ）的显色反应

报道了1-（4-硝基苯基）-3-（2-苯并咪唑）-三氮烯（NPBMT）的合成及其与铜（Ⅱ）的显色反应。在非离子表面活性剂OP存在下,于pH11．5的Na2B4O7-NaOH缓冲介质中,NPBMT与铜（Ⅱ）形成2：1的桔红色络合物,络合物的最大吸收峰为417nm,表观摩尔吸光系数为2．62×10^4 L·mol^-1·cm^-1,10mL溶液中,铜（Ⅱ）量在0—15μg／mL范围内符合比尔定律。该法用于人发和食品中微量铜的测定,测定结果与AAS法相符。     

Fe（Ⅱ）—DPPT—OP光度法测定非金属矿物中微量铁

4,7-二苯基—1,10-二氮杂菲(DPPT)与Fe~(2 )显色有良好的选择性.且灵敏度为1,10-二氮杂菲的2倍.但DPPT为非水溶性物质,故文献[1]采用Triton X-100增溶后,用于测定天然水和海洋生物体内微量铁.本工作采用容易获得的国产品乳化剂OP(主要成分为聚乙二醇辛基苯基醚)代替Triton X-100,并将方法用于非金属矿物中微量铁的测定,获得满意结果.     

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.     

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。