N,N,N′′-三取代氨基甲酰脲类化合物的合成

N，N－二取代脲和取代三氯乙酰胺反应合成了10种未见文献报道的标题化合物，产物结构经元素分析、IR和^1H NMR确证。初步生物活性测定表明多数化合物具有明显的除草活性。     

O／W微乳液中聚吡咯超微粒子的制备

选择合适的ＳＤＢＳ／吡咯／Ｈ２Ｏ三组分Ｏ／Ｗ微乳液与吡咯单体共存的两相体系，以单体相为单体源，在Ｏ／Ｗ三组分微乳液中进行了吡咯聚合，所得聚吡咯粒子大小仅为２～３ｎｍ，分布较均匀，且具有较好的导电性能．     

化学镀钴基合金镀液中钴的快速测定

研究了采用显色剂 苦胺酸偶氮变色酸对化学镀钴基合金镀液中钴含量进行测定的试验条件,在pH11的氨 氯化铵缓冲溶液中,钴与显色剂配合物的最大吸收峰在650nm波长处,钴(Ⅱ)在0～60μg/25ml范围内服从比耳定律,表观摩尔吸光系数为3.1×104L·mol-1·cm-1。该法测定钴的选择性好,在大量镍存在下,也能准确测定,对镀液样品进行了测定,相对标准偏差小于1%,结果满意。     

Multiple melting behavior of poly(butylene succinate)

The multiple melting behavior of poly(butylenes succinate) (PBS) isothermally crystallized from the melt was investigated using differential scanning calorimetry (DSC), temperature modulated DSC (MDSC) and polarized optical microscopy. PBS exhibits at most four melting endotherms (denoted as T_m1, T_m2, T_m3, and T_m4 from high to low temperatures) and a crystallization exotherm (denoted as T_re) in the DSC heating trace. Multiple melting endotherms were observed even at high heating rates. The origins of each endothermal and exothermal peak were discussed in detail. It is suggested that: (i) the crystallization exothermic peak, T_re, relates to the recrystallization of the melt of the crystallites with lower thermal stability; (ii) the T_m1 is ascribed to the melting of crystallites formed through recrystallization; (iii) two crystal populations with different thermal stability are responsible for the T_m2 and T_m3; (iv) the T_m4, which is the annealing peak, represents the transition of the rigid amorphous fraction (RAF) from solid-like RAF into liquid-like amorphous fraction.     

Synthesis and crystal structure of inclusion compounds: Trans-9,10-dihydro-9,10-ethanoanthracene-11,12-dicarboxylic acid with boric acid and tetrabutylammonium salt

Two new inclusion compounds (n-C₄H₉)₄N⁺C₁₈-H₁₃O₄ ⁻·B(OH)₃ (1) and (n-C₄H₉)₄N⁺C₁₈H₁₃O₄ ⁻ (2) were prepared and characterized by X-ray crystallography. Crystal data: compound 1, monoclinic P2(1)/c, a = 1.569 9(1) nm, b = 0.995 5(6) nm, c = 2.293 3(1) nm, β = 109.962(3)°, Z = 4, and R ₁ = 0.0434, wR = 0.075 9; compound 2, monoclinic C2/c, a = 1.400 5(3) nm, b = 1,282 1(2) nm, c = 1.765 7(3) nm, β = 100.388(1)°, Z = 4, and R ₁ = 0.0584, wR = 0.096 6. In the crystal structure of 1, the tetramers formed by two trans-9,10-dihydro-9,10-ethanoanthracene-11,12-dicarboxylic acid (EADA) anions and two boric acid molecules were connected through O—H⋯O hydrogen bonds to generate a channel type host lattice. The tetra-n-butylammonium cations were stacked to give two columns within each channel with cross-sectional size of about 2.30 nm × 0.93 nm. In the crystal structure of 2, similar honeycomb host lattices with big size were also formed along the [101] direction by three-dimensional accumulation of EADA anions. The tetra-n-butylammonium cations were accommodated in a zigzag fashion within each channel. Translated from Acta Chimica Sinica, 2006, 64(18): 1904–1910 [译自: 化学学报]     

超声引导椎旁神经阻滞治疗带状疱疹后遗神经痛的疗效及可行性分析

本文对超声引导椎旁神经阻滞治疗带状疱疹后遗神经痛（post-herpetic neuralgia，PHN）的疗效及可行性进行了分析。研究对象为2015年12月~2017年12月于我院就诊的94例PHN患者，按就诊顺序随机均分为两组，对照组给予普瑞巴林常规治疗，观察组在此基础上联合超声引导椎旁神经阻滞治疗，连续治疗4周。本文比较了治疗前、治疗1周、2周、4周后的匹兹堡睡眠质量指数（PSQI）评分、疼痛视觉模拟（VAS）评分，并评价了治疗后的综合疗效，记录了治疗期间发生不良反应情况。结果显示，较治疗前，治疗1周、2周、4周后两组VAS评分均逐渐降低，且观察组治疗后各时间点的VAS评分显著低于对照组，差异具有统计学意义（P<0.05）；较治疗前，两组治疗1周、2周、4周后PSQI评分均逐渐降低，且观察组治疗后各时间点的PSQI评分显著低于对照组，差异具有统计学意义（P<0.05）；观察组治疗总有效率为89.36%，对照组为78.72%，观察组显著高于对照组，差异具有统计学意义（P<0.05）；两组治疗期间各项不良反应发生率差异无统计学意义（P>0.05）。本文证实了超声引导椎旁神经阻滞治疗PHN能显著改善患者神经疼痛症状，提升睡眠质量，同时具有安全性保障。     

Electron-rich radicals by neutralizationreionization mass spectrometry. Generation, dissociations and energetics of the hydrogen atom adduct to acetamide

Protonated acetamide exists as two planar conformers, the more stable anti-form (anti-1(+)) and the syn-form (syn-1(+)), DeltaG(degree) (298) (anti-->syn) = 10.8 kJ mol(-1). Collisional neutralization of 1(+) produces 1-hydroxy-1-amino-1-ethyl radicals (anti-1 and syn-1) which in part survive for 3.7 micros. The major dissociation of 1 is loss of the hydroxyl hydrogen atom (approximately 95%) which is accompanied by loss of one of the methyl hydrogen atoms (approximately 3%) and loss of the methyl group (approximately 2%). The most favorable dissociation of the OH bond is calculated to be only 34 kJ mol(1) endothermic but requires 88 kJ mol(-1) in the transition state. Other dissociations of 1, e.g., loss of one of the amide hydrogens, methyl hydrogens, and loss of ammonia are calculated to proceed through higher- energy transition states and are not kinetically competitive if proceeding from the ground doublet electronic state of 1. The unimolecular dissociation of 1 following collisional electron transfer is promoted by large Franck-Condon effects that result in 8090 kJ mol(-1) vibrational excitation in the radicals. Radicals 1 are calculated to exoergically abstract hydrogen atoms from acetamide in water, but not in the gas phase. The different reactivity is due to solvent effects that favor the products, (.)CH(2)CONH(2) and CH(3)CH(OH)NH(2), over the reactants.     

FT-IR and FT-raman spectroscopy study of the cyclic anhydride intermediates for esterification of cellulose: I. Formation of anhydrides without a catalyst

In recent years, extensive efforts have been made to find nonformaldehyde durable press finishes to replace the traditional formaldehyde-based reagents for producing wrinkle-free cotton fabrics. 1,2,3,4-butanetetracarboxylic acid (BTCA) has been the most effective nonformaldehyde crosslinking agent. Our previous research has indicated that a polycarboxylic acid esterifies cellulose in two steps: the formation of a 5-membered cyclic anhydride intermediate by the dehydration of two adjacent carboxyl groups, and the reaction between cellulose and the anhydride intermediate to form an ester linkage. In this research, we used Fourier transform infrared and Fourier transform Raman spectroscopy to study the formation of cyclic anhydride intermediates by BTCA and other polycarboxylic acids without the presence of a catalyst. We found that BTCA and other polycarboxylic acids in a crystalline state start to form 5-membered cyclic carboxylic anhydrides when the temperature reaches the vicinity of their melting points with the exception of bifunctional acids, which form cyclic anhydrides at temperatures much higher than their melting points. Intermolecular hydrogen bonding between carboxylic acid groups prevents the formation of the cyclic anhydride intermediates at lower temperatures. We also found that polycarboxylic acids in an amorphous state form cyclic anhydrides at much lower temperatures.     

Effect of Neck Formation on the Measurement of Dynamic Interfacial Tension in a Drop Volume Tensiometer

Dynamic interfacial tension values obtained by drop volume tensiometry will be affected under certain experimental conditions by the formation of a neck between the drop and the capillary tip. This phenomenon must be accounted for to obtain accurate values of interfacial tension. In this work, neck formation for a water–mineral oil system is studied under conditions where hydrodynamic effects can be neglected. A model originally developed for the determination of the surface tension of a suspended drop is modified for application to dynamic interfacial tensions of surfactant-containing liquids. The model relates apparent values of interfacial tension calculated from drops possessing necks to actual values. Experiments with Span 80 (sorbitan monooleate) and sodium dodecyl sulfate (SDS) surfactants in a mineral oil–water system are used to test the validity of the developed model. For the small tip diameter used, good agreement is obtained for Span 80 up to the critical micelle concentration, and for low concentrations of SDS, when the surfactant adsorption is diffusion-limited. In both cases, the neck diameter of the growing drop can be considered constant over the range of dynamic interfacial tensions tested.     

神光-Ⅱ装置三倍频实验中靶场单元技术的改进

 主要介绍为了满足神光-Ⅱ高功率激光装置三倍频光（351nm，3ω）的物理实验要求，靶场三倍频模拟光源和瞄准监视系统两个主要单元技术的改进，即三倍频模拟光源由基频光（1 053nm，3ω）通过腔外的KTP+BBO晶体倍频获得，再经八路分光系统和主激光耦合；瞄准监视系统由透射式光学系统改进为反射式光学系统，避免原系统存在较大的色差，提高瞄准精度。