Ln(η~6-m-C_6H_4Me_2)(AlCl_4)_3,(Ln=Pr,Er)的合成及Pr配合物的晶体结构

ＬｎＣｌ３（Ｌｎ＝Ｐｒ，Ｅｒ）与ＡｌＣｌ３在二甲苯中反应，合成了η６－（ｍ－Ｍｅ２Ｃ６Ｈ４）Ｌｎ（ＡｌＣｌ４）３这两个新配合物并对其进行了元素分析、红外光谱和质谱的表征。测定了Ｐｒ配合物的晶体结构。该配合物具有扭曲的五角双锥几何构型。二甲苯和一个氯原子处于两个顶点，Ｐｒ配合物属单斜晶系，空间群Ｐ２１／ｎ，晶胞参数为ａ＝９．８７０（３），ｂ＝１６．７９４（８），ｃ＝１６．０２５（７），β＝９４．４０（３）°，Ｖ＝２６４８．５１３，Ｚ＝４。平均Ｐｒ－Ｃ为２．９５（２）。

聚氯乙烯-尼龙6树脂分离富集碘量法测定金精矿中金

采用聚氯乙烯尼龙６树脂分离富集溶解于王水中的金精矿样品中的金，然后用乙二胺溶液洗脱，并用碘量法测金。经标样验证，结果令人满意。

聚氯乙烯-尼龙6树脂富集差示光度法测定金

采用聚氯乙烯尼龙６树脂分离富集溶解于王水金精矿样品中的金，然后用亚硫酸钠和碘化钾的混合溶液洗脱，并用硫代米氏酮显色，同时将普通光度法、差示光度法以及稀释有色溶液的差示光度法结合起来进行测定。通过标样验证，结果令人满意。

Studies on biodegradable poly(hexano-6-lactone) fibers 1. Structure and properties of drawn poly(hexano-6-lactone) fibers

Using high molecular weight (M-n=80,000) Poly(hexano-6-lactone) (PCL'), tough and high tenacity PCL monofilaments with various draw ratios (undrawn to 9 times drawn) were prepared by melt-spinning. The relationship between microstructure and properties of the PCL fibers is described in this current IUPAC Technical Report. Analysis of microstructure of the drawn PCL fibers by wide-angle X-ray diffraction revealed typical c-axis orientation with an increase in crystallinity. It was also supported by sonic velocity measurements. The thermal, mechanical, and dynamic mechanical properties of the PCL fibers were affected significantly by draw ratio. DSC thermograms showed that the melting temperature and the enthalpy of fusion increased with draw ratio. The temperature dependence curves of dynamic viscoelasticity showed that the temperature at tan delta peak of alpha dispersion corresponding to the glass transition temperature shifted toward higher temperature and the peak value of tan delta decreased with draw ratio. The dynamic storage modulus and the sonic modulus increased with draw ratio. These results are due to the increase in crystallinity and molecular orientation with drawing, and are responsible for an increase in tensile tenacity as well as knot tenacity of the PCL fibers.

An eta(6)-toluene complex of neodymium: [Nd(eta(6)-C6H5CH3)(AlCl4)(3)]

The Nd-III ion in hexa-mu-chloro-1:2 kappa(2)Cl;1:3 kappa(2)Cl;1:4 kappa(2)Cl-hexachloro-2 kappa(2)Cl,3 kappa(2)Cl,4 kappa(2)Cl- [1 (eta(6))- toluene] trialuminiumneodymium has distorted pentagonal bipyramidal coordination geometry. Five Cl atoms form the equatorial plane, and the toluene ring and the sixth Cl atom occupy the apical sites. The average Nd-C(eta(6)) and Nd-Cl distances are 2.926 (5) and 2.857 (1) Angstrom, respectively.

Structure and order of the discotic compound 2,3,6,7,10,11-hexakispentyloxytriphenylene as revealed by diffraction and molecular simulation studies

The aggregate structure of the discotic compound 2,3,6,7,10,11-hexakispentyloxytriphenylene (HPT) was studied both for the crystalline state and the liquid crystalline state by using electron crystallography and a molecular simulation approach. In the crystalline state, HPT was found to adopt an orthorhombic P-2212 space group with cell parameters a = 36.73 Angstrom, b = 27.99 Angstrom and c = 4.91 Angstrom. Molecular packing calculations were conducted to elucidate the molecular conformation and mutual orientational characteristics in the different states. Phase transitions and relationships are discussed from a structural point of view.

Effects of molecular weight and interaction parameter on the glass transition temperature of polystyrene mixtures and its blends with polystyrene/poly(2,6-dimethyl-p-phenylene oxide)

The glass transition temperature (T-g) of mixtures of polystyrene (PS) with different molecular weight and of blends of poly(2,6-dimethyl-p-phenylene oxide) (PPO) and polystyrene with different molecular weight (DMWPS) was studied by a DSC method. For the whole range of composition, the curves of T-g vs composition obtained by experiment were compared with predictions from the Fox, Gordon-Taylor, Couchman and Lu-Weiss, equations. It was found that the experimental results were not in agreement with those from the Fox, Gordon-TayIor and Couchman equations for the binary mixtures of DMWPS, where the interaction parameter chi was approximately zero. However, for the blends PPO/DMWPS (chi < 0), with an increase of molecular weight of PS, it was shown that the experimental results fitted well with those obtained from the Couchman, Gordon-Taylor and Fox equations, respectively. Furthermore, the Gordon-Taylor equation was nearly identical to the Lu-Weiss equation when \chi\ was not very large. Further, the dependence of the change of heat capacity associated with the glass transition (Delta C-p) on the molecular weight of PS was investigated and an empirical equation was presented. (C) 1997 Elsevier Science Ltd.

Synthesis, crystal structure and magnetic properties of a series of polymeric lanthanoid-copper complexes [Ln(2)Cu(3){O(CH2-CO2)(2)}(6)].nH(2)O (Ln=La, Nd, n=9; Ln=Er, n=6)

The reaction of diglycolic acid, O(CH2CO2H)(2), with Cu(NO3)(2) . H2O and lanthanoid nitrate hydrate produces a series of novel Ln-Cu mixed metal complexes, [Ln(2)CU(3){O(CH2CO2)(2)}(6)]. nH(2)O (Ln = La, Nd, n = 9; Ln = Er, n = 6), which have been characterized by elemental analysis, i.r. spectroscopy, magnetic measurements and X-ray crystallography. The Ln(3+) and Cu2+ ions are connected by the carboxylate groups of the ligands, resulting in the formation of a complicated network.

PVC-尼龙6树脂应用于天然水中痕量金的价态分析

在王水介质中，ＰＶＣ－尼龙６树脂定量吸附Ａｕ（Ⅲ），而Ａｕ（Ⅰ）基本上不吸附。当存在碘离子时，Ａｕ（Ⅲ）和Ａｕ（Ⅰ）均能形成碘的络阴离子而被树脂定量吸附，从而可分别测出总金和Ａｕ（Ⅲ）的含量并计算出Ａｕ（Ⅰ）的含量。方法的检测限为１．６×１０－１１ｇ／Ｌ，样品加标回收率在８０％以上。为天然水中痕量金的价态分析提供了一个令人满意的方法。

4-羟基偶氮苯与6-氯-5,12-萘并萘醌反应产物的NMR分析

无水碳酸钾存在下6-氯-5,12-萘并萘醌与4-羟基偶氮苯在干燥DMF中反应的主要产物在某些反应条件下不是6[4-(苯基偶氮基)苯氧基]-5,12-萘并萘醌(1)。该未知反应产物2经核磁共振方法研究证实是6-(N,N-二甲氨基)-5,12-萘并萘醌。本文对化合物2的~1H-和~(13)C化学位移、偶合信息和结构作了详细归属,并推测其反应进程,实验结果表明,化合物2是由化合物1与溶剂DMF反应生成。

组成对PA1010/6共聚物熔融行为的影响

用ＤＳＣ研究了ＰＡ１０１０／６共聚物初生态及次生态样品的熔融行为，发现初生态样品的高温熔融峰（Ｔ１）和低温熔融峰（Ｔ２）对组成有不同的依赖关系；首次发现ＰＡ１０１０／６共聚物次生态的冷结晶现象，并讨论了冷结晶温度（ＴＣ）、冷结晶时间（ｔｃ）与组成的关系.

Activation of a ring methyl substituent in pentamethylcyclopentadienyl rhenium(V) compounds: Synthesis and characterization of the 1,2,3,4-tetramethyl-5,6-dihydrofulvene-5,6-dithiolato complex [ReO{(S)(SCH2)C(5)Me(4)}(C(5)Me(5))]

Reaction of the half-sandwich rhenium(v) complexes [Re-Cl-4(C(5)Me(5))] or [Re(O)Cl-2(C(5)Me(5))] with H2S in chloroform in the presence of pyridine leads to the chiral dithiolato complex [ReO((S)(SCH2)C(5)Me(4))(C(5)Me(5))] 1.

Isothermal crystallization studies on neodymium oxide filled nylon 6

Melt mixing of nylon 8 with neodymium oxide particles was carried out with a single-screw extruder. The crystal behaviors of plain nylon 6 and the neodymium oxide filled nylon 6 mixture were studied by means of isothermal crystallization kinetic analysis. Isothermal crystallization thermograms obtained by differential scanning calorimetry (DSC) were analyzed based on the Avrami equation. The neodymium oxide particles acted as a nucleating agent in the mixture. The overall rate of di-isothermal crystallization of the neodymium oxide filled nylon 6 mixture is higher than that of plain nylon 6. The mechanism and modes of plain nylon 6 were the same as those of neodymium oxide filled PA6 mixture.

Electrochemical study of isopoly- and heteropoly-oxometallates film modified microelectrodes .6. Preparation and redox properties of 12-molybdophosphoric acid and 12-molybdosilicic acid modified carbon fiber microelectrodes

The redox behaviours of 12-molybdophosphoric acid (12-MPA) and 12-molybdosilicic acid (12-MSA) in aqueous acid media are characterized at the carbon fiber (CF) microelectrode. The preparation of CF microelectrode modified with 12-MPA or 12-MSA monolayer and the oxidation-reduction properties of the modified electrode in aqueous acid media or 50% (v/v) water-organic media containing some inorganic acids are studied by cyclic voltammetry. 12-MPA or 12-MSA monolayer modified CF microelectrode with high stability and redox reversibility in aqueous acidic media can be prepared by simple dip coating. The cyclic voltammograms of 12-MPA and 12-MSA and their modified CF microelectrodes in aqueous acid solution exhibit three two-electron reversible waves with the same half-wave potentials, which defines that the species adsorbed on the CF electrode surface are 12-MPA and 12-MSA themselves. The acidity of electrolyte solution, the organic solvents in the electrolyte solution, and the scanning potential range strongly influence on the redox behaviours and stability of 12-MPA or 12-MSA monolayer modified electrodes. On the other hand, the catalytic effects of the 12-MPA and 12-MSA and chlorate anions in aqueous acidic solution on the electrode reaction processes of 12-MPA or 12-MSA are described.