邻氯苯甲酸稀土配合物中金属－氧键振动的研究

研究了邻氯苯甲酸稀土配合物ＭＬ３·Ｋ２Ｏ（Ｍ＝Ｙ，Ｌａ～Ｌｕ；ＨＬ＝ｏ－ｃｈｌｏｒｏｂｅｎｚｏｉｃａｃｉｄ）的远红外光谱，归属了金属－氧振动的波数（ｖＭ－ｏ）．并发现ｖＭｏ随镧系原子序数的增大而增加，ｖＭ－ｏ与稀土离子基态角量子数Ｌ呈“斜Ｗ”关系。     

氢化物发生—冷阱捕获—色谱分离—原子吸收法测定天然水中坤的形态

研究建立了氢化物发生－冷阱捕获－色谱分离－原子吸收方法测定天然水中四种主要砷形态，测试系统自行组装，色谱柱填料采用ＣｈｒｏｍｏｓｏｒｂＧＡＷ－ＤＭＣＳ（粒径０．３～０．４５ｍｍ），其上涂布３％ＯＶ－１０１。方法的检出限以砷计分别为：Ａｓ（Ｖ）０．５１ｎｇ，Ａｓ（Ⅲ）０．４３ｎｇ，ＭＭＡ０．３８ｎｇ，ＤＭＡ０．６７ｎｇ；１２ｎｇ砷标准偏差为Ａｓ（Ⅴ）４．２１％，Ａｓ（Ⅱ）３．５６％，ＭＭＡ３．２３％     

水果中三唑酮残留量的气相色谱和气相色谱—质谱分析

水果中三唑酮残留用丙酮提取，经液－液分配净化，用气相色谱－电子捕获检测器测定，并用相色谱－质谱进行确证以ＨＰ－５大口径毛细管柱和ＨＰ－５ＭＳ毛细管柱为分离柱，选择出合适的色谱条件。三唑酮的分离效果良好。     

五加成C60氮杂丙酸衍生物的合成

Ｃ６０和β－叠氮丙酸在氰苯中回流，产物经柱色谱分离、ＦＤ－ＭＳ证实为五加成Ｃ６０衍生物，＾１３Ｃ ＮＭＲ、ＦＴ－ＩＲ和ＵＶ光谱对产物结构进行了表征。     

乙基基聚硅氧烷共聚反应竞聚率的测定及其对复合粒子形态的影响

用Ｆｉｍｅｍａｎ－Ｒｏｓｓ法处理数据，测定了乙烯基聚硅氧烷与苯乙烯，甲基丙烯酸甲酯和甲基丙烯酸正丁酯的共聚反应的竞聚率，结果为ｓｔ＝１，４５和ｒｓｖ＝１．０８，ｒＭＭＡ＝０．７８和ｒｓｖ＝２．１，ｒａ－ＢＭＡ＝０．４６和ｒｓｖ＝３．４９。以含ＳＶ的乳液作为种子进行烯类单体的乳液聚合，单体和ＳＶ共聚反应对复合粒的形态有很大影响。     

异丙基桥连的希夫碱及其锰（Ⅲ）络合物催化剂的红外光谱

研究了异丙基桥连的希夫碱及其锰（Ⅲ）络合物催化剂的红外光谱（３８００￣１５０ｃｍ＾－１），对一些主要吸收谱带进行了经验归属。配体内氢键谱带出现在３４４６ｃｍ＾０１附近（以ＬＨ为例），ｖｃ－０谱带在１７２４ｃｍ＾－１附近（以ＬＣ为例，下同），ｖｃ＝Ｎ谱带在１６４９和１６２９ｃｍ＾－１附近，苯环的特征谱在１６０１，１４７０和７５３ｃｍ＾－１附近，ｖＭｎ－Ｎ为主的复合振动在３６３ｃｍ＾－１附近，δＭｎ－     

湘泉酒气相色谱法分析探讨

湘泉酒气相色谱法分析探讨李杜,周继红,詹益兴（湖南教育学院化学系长沙４１００１２）（长沙市化工研究所长沙４１０００７）１实验气相色谱仪：ＧＣ－１４Ａ,ＦＩＤ检测器;色谱柱：ＰＥＧ－２０Ｍ石英交联毛细管柱,５０ｍ×０．２５ｍｍ;柱温：４５℃（５ｍｉｎ）...     

水溶性卟啉还原甲基紫精动力学的研究

利用跟踪法测定了碘化四－（对甲基异烟酰基苯基）［ＴＭＩａｐｐＩ］等五种水溶性卟啉在还原甲基紫精过程中［ＭＶ＾＋］深度的变化，获得了［ＭＶ＾＋］／［Ｐｏ］～ｔ及［Ｍｖ＾＋］／［Ｍｖ＾２＋］～ｔ的关系曲线。由稳态近似原理推出的动力学方程求得了几种求得了几种卟啉的动态学参数Ａ、诱导时间ｔｉ及起始速率ｖ０。通过稳态转化率得知５种水溶性卟啉的光敏强度有如下顺序：ＺｎＴＭｐｙＰ＞ＺｎＴＭＩＡＰＰＩ＞ＺｎＴＭＮ     

柱后衍生高效液相色谱法测定鸡肉中莫能菌素残留量

样品用甲醇－水溶液匀浆、提取后过滤,再用二氯甲烷进行液－液萃取,然后通过Ｓｅｐ－Ｐａｋ柱进一步净化。净化后的样液与香兰素衍生试剂在酸性和加热条件下进行柱后衍生,反应产物在５２０ｎｍ波长处测定。衍生剂：香兰素３０．０ｇ＋浓硫酸２０ｍＬ＋甲醇９５０ｍＬ,流速：０．７ｍＬ／ｍｉｎ;色谱柱：μ－ＢｏｎｄａｐａｋＴＭＣ１８３．９ｍｍｉ．ｄ．×３００ｍｍ,或相当的色谱柱;流动相：Ｖ（甲醇）Ｖ（水）Ｖ（磷酸）＝９４０６０１,流速０．７ｍＬ／ｍｉｎ;柱后反应室：体积大于１．４ｍＬ的不锈钢管（３００ｃｍ×１ｍｍｉ．ｄ．）。     

C60O结构和电子光谱的理论研究

用ＩＮＤＯ系列方法研究Ｃ６０Ｏ的两种结构：一是桥氧加在２个六元环之间的键上为Ｃ２ｖ构型；另一个是桥氧加在１个五元环和１个六元环之间的键上为Ｃｓ构型。计算表明，从总能量、ＨＯＭＯ－ＬＵＭＯ能级差和光谱性质看，Ｃ６０Ｏ的稳定构型都应是Ｃ２ｖ构型，该Ｃ２ｖ异构体具有环氧结构（桥Ｃ１５－Ｃ３０键长为０．１５１８ｎｍ，键序为０．８７４４），其电子光谱计算结果与实验值较好地符合。     

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。