聚芳醚酮膜的溶剂吸附与诱导结晶行为

研究了聚芳醚酮系列在１，２－二氯乙烷中的吸附，及溶剂与温度诱导结晶行为。得到６０℃时的最大吸附量Ｃ∞及假扩散系数Ｄ为：ＰＥＥＫ，Ｃ∞＝４６％，Ｄ＝３．１０×１０＾－１２ｍ＾２·ｓ＾－１；ＰＥＥＫＫ，Ｃ∞＝５０％，Ｄ＝６．５７×１０＾－１２ｍ＾２·ｓ＾－１；ＰＥＫＫ，Ｃ∞＝５５％，Ｄ＝９．４１×１０＾－１２ｍ＾２·ｓ＾－１。实验表明，吸附及脱附行为均与分子链刚性或羰基含量有关，膜的分子链受溶剂作用而     

修饰微带金电极上细胞色素C电极过程的热力学研究

研究了细胞色素Ｃ（Ｃｙｔ．Ｃ）在一种新的电子转移促进剂４，６－二甲基－２－巯基嘧啶修饰微带金电极（ＤＭＭＰ／Ａｕ）上的氧化还原热力学；求得Ｃｙｔ．Ｃ在ＤＭＭＰ／Ａｕ电极上反应的标准电极电位Ｅ＾ｏ，熵变△Ｓ＾ｏ，焓变△ＩＩ＾ｏ及Ｇｉｂｂｓ自由能的改变△Ｇ１０值分别为：０．２７２Ｖ（ｕｓ．ＮＨＥ），－１２３．７Ｊ．ｍｏｌ＾－＾１，－６３．１ｋＪ．ｍｏｌ．ｍｏｌ＾－＾１和－２６．２ｋＪ．ｍｏｌ＾－＾１（     

液芯光纤长光路法在水溶液中测定Cr,Cu

测量了低折射率液体和水溶液液芯光纤的导光特性和光谱特性，研究了液芯光纤长光路法在７０％乙醇－水溶液体系和５０％二氧六环－水溶液体系中测定Ｃｒ（Ⅵ）、Ｃｕ（Ⅱ）的方法。液芯光纤长１１０ｃｍ时，测定Ｃｒ、Ｃｕ的灵敏度分别为０．０５２、０．０１７ｎｇ．ｍＬ＾－１；线性范围０－２５、０－２５ｎｇ／ｍＬ；ＲＳＤ值为１．０％－４．８％。对国标ＧＳＢＥ５０ ００９－８８样品和明胶中铬的测量值与标准值或ＡＡＳ测量     

硫堇衍生化自组装膜修饰金电极的电化学性质及其对抗坏血…

将硫堇共价键合到自组装在金电极表面的半胱胺单分子层上，制成了衍生化自组装单分子膜修饰电极，并用电化学方法研究了它的电化学性质，循环伏安图显示其在ｐＨ＝７．７的磷酸盐缓冲液中，于－０．４５～＋０．５０Ｖ（ｖｓ．ＳＣＥ）范围内有２对氧化还原峰，峰电位分别为Ｅｐａ＝２１４ｍＶ，Ｅｐｃ＝８２ｍＶ，Ｅ＾２ｐａ＝－７５ｍＶ，Ｅ＾２ｐｃ－－１６０ｍＶ（ｖｓ．ＳＣＥ），ｐＨ在５．０～９．０范围内，峰１有２个质子参     

噻利洛尔的吸附伏安行为

在ＮＨ３－ＮＨ４Ｃｌ底液中,噻利洛尔在汞电极上有一线性扫描还原峰,电位Ｅｐｃ＝－１．３１Ｖ（ｖｓ,Ａｇ／ＡｇＣｌ）,该峰具有明显的吸附性。当ＣＥＬ浓度较小时,扫描较快,搅拌富集时间较长时,电极反应完全为吸附态的ＣＥＬ的还原所控制,吸附粒子为ＣＥＬ中性分子,测得ＣＥＬ在汞电极上的饱和肿附量为１．０３×１０＾－１０ｍｏｌ／Ｌ,每个ＣＥＬ分子所占电极面积为１．５７ｎｍ＾３,ＣＥＬ在悬汞电极上的吸附符合Ｌ     

六氟磷酸二（4,4‘—二甲基—2,2’—联吡啶）.（2,2‘—联吡啶—4,4’—二羧？…

用＾１Ｈ ＮＭＲ和＾１３Ｃ ＮＭＲ谱研究了新型电化学发光探针六氟磷酸二（４,４’;－二甲基－２,２‘－联吡啶）．（４．４’－二羧酸－２,２‘－联吡啶）合钌的立体结构,通过＾１Ｈ ＾１Ｈ ＣＯＳＹ,＾１３Ｃ－＾１Ｈ ＨＥＴＣＯＲ谱对其氢谱和碳谱中的各谱峰进行了归属,并给出了氢谱和碳谱峰的化学位移值。     

1—羟基蒽醌及其稀土络合物的红外光谱分析

制备了稀土离子Ｌｎ＾３＋（Ｌｎ＝Ｌａ，Ｃｅ，Ｐｒ，Ｎｄ，Ｓｍ，Ｅｕ，Ｇｄ，Ｔｂ，Ｄｙ）与１－羟基蒽醌的络合物，测定了它们和氘代１－羟基蒽醌在４０００￣５０ｃｍ＾－１范围内的红外光谱，对观察红外吸收带进行分析和归属。发现了某些对金属离子敏感的谱带，确定了配位键的伸缩振动。     

金属键有机化合物的研究—非对称型η^5—取代环戊二烯…

通过η＾５－Ｒ＾１Ｃ５Ｈ４（ＣＯ）３ＭＨａ与η＾５－Ｒ＾２Ｃ５Ｈ４（ＣＯ）２ＭＮａ（Ｍ＝Ｍｏ，Ｗ）以及η＾５－Ｒ＾１Ｃ５Ｈ４（ＣＯ）３ＭｏＮａ与η＾５－Ｒ＾２Ｃ５Ｈ４（ＣＯ）３ＷＮａ在Ｆｅ２（ＳＯ４）３醋酸水溶液作用下的交叉氧化偶联反应，合成了７个新的非对称型金属单键化合物η＾５－Ｒ＾１Ｃ５Ｈ４（ＣＯ）３Ｍｏ－Ｍｏ（ＣＯ）３Ｃ５Ｈ４Ｒ＾２－η＾５（Ｒ＾１，Ｒ＾２：Ｃ（Ｏ）Ｍｅ，ＣＯ２Ｅｔ），η＾５     

模板分子TMEDA成CF—3及ZSM—39沸石笼中的位置及其与骨…

用ＸＲＤ、ＦＴＩＲ、ＴＧ－ＤＴＡ、＾１３Ｃ魔角固体核磁共振表征用四甲基乙基二胺（ＴＭＥＤＡ）为结构异向剂合成的高硅沸石ＣＦ－３及ＺＳＭ－３９．ＴＭＥＤＡ不同基团的＾１３Ｃ化学位移，共振峰相对强度在交叉极化（ＣＰ）及高功率去偶（ＨＰＤＥＣ）核磁共振谱中的变化，揭示出模板分子在尺寸不同的沸石笼中的位置、运动状态及其与骨架的相互作用。在ＺＳＭ－３９沸石中的ＴＭＥＤＡ分子，它的－Ｃ２Ｈ４－基团＾１３Ｃ共振     

一种新型含酞侧基聚芳醚砜的稀溶液性质研究（I）——溶解行…

制备了窄分布的含酞侧基聚芳醚砜（ＰＥＳ－Ｃ）级份样品，用光散射法测定样品的重均分子量，粘度法测定样品在ＤＭＦ，ＣＨＣｌ３和１，２－Ｃ２Ｈ４Ｃｌ２中的特性粘数和Ｈｕｇｇｉｎｓ参数ｋ＾’值，Ｋ＾’值远大于０．５反映了体系中存在特殊的溶解行为，得到了ＰＥＳ－Ｃ在３种溶剂中的Ｍａｒｋ－Ｈｏｕｗｉｎｋ方程，（η）＝２．７９×１０＾－２Ｍ＾０．６１５ｗ，ｒ＝０．９９９８（ＤＭＦ，２５℃）（η）＝３．９６×１０     

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.     

探究“铁的锈蚀条件”实验创新设计

设计了铁的锈蚀实验,说明了铁钉的处理方法,增加了温度、酸、碱的影响条件,实现了铁跟蒸馏水及空气中氧气快速反应而生锈,使实验在5 min左右就能够得到准确的结果。