硅酸及其盐的研究 ⅩⅩⅠ.三甲基硅烷化-气相色谱法测定单硅酸的离解常数

单硅酸的离解常数是表征其基本性质的重要数据,前人已有不少工作,但由于测定的方法和实验条件不同,所得数据很不一致。     

SHAPE MEMORY EFFECT OF PU IONOMERS WITH IONIC GROUPS ON HARD-SEGMENTS

SMPU （shape memory polyurethane） non-ionomers and ionomers, synthesized with poly（c-caprolactone） （PCL）, 4, 4＇-diphenylmethane diisocyanate （MDI）, 1,4-butanediol （BDO）, dimethylolpropionic acid （DMPA） were measured with cyclic tensile test and strain recovery test. The relations between the structure and shape memory effect of these two series were studied with respect to the ionic group content and the effect of neutralization. The resulting data indicate that, with the introduction of asymmetrical extender, the stress at 100% elongation is decreased for PU non-ionomer and ionomer series, especially lowered sharply for non-ionomer series; the fixation ratio of ionomer series is not affected obviously by the ionic group content; the total recovery ratio of ionomer series is decreased greatly. After sufficient relaxation time for samples stretched beforehand, the switching temperature is raised slightly, whereas the recovery ratio measured with strain recovery test method is lowered with increased DMPA content. The characterization with FT-IR, DSC, DMA elucidated that, the ordered hard domain of the two series is disrupted with the introduction of DMPA which causes more hard segments to dissolve in soft phase; ionic groups on hard segment enhance the cohesion between hard segments especially at high ionic group content and significantly facilitate the phase separation compared with the corresponding non-ionomer at moderate ionic group content.     

碳纳米管的最新制备技术及生长机理

结合笔者的工作综述了碳纳米管的制备技术及生长机理的最新研究进展，重点介绍了近两年来碳纳米管制备的进展情况，包括传统制备方法的改进（电弧放电法、化学气相沉积法和激光蒸发法）、新型制备技术、特殊结构的碳纳米管制备；同时探讨了碳纳米管的各种生长机理；最后提出了碳纳米管制备技术和生长机理的发展方向。     

环己烯和2-甲基戊烯-1在几种Y型分子筛上的吸附量热研究

用SETARAM热流式量热计测定了环己烯和2-甲基戊烯-1于室温下在NaY、CaY、R_EY和HY等几种分子筛上的微分吸附热。我们又用Benson基团加合法计算得到了生成仲碳离子和叔碳离子时的吸附热。根据实验测得的于不同吸附量时环己烯和2-甲基戊烯-1的吸附热之差值, 对它们在上述几种Y型分子筛上的吸附机理进行了讨论。     

Conformational identification and dipole moment of 4-fluoro-1-butene by microwave spectroscopy

The microwave spectrum of 4-fluoro-1-butene has been recorded in the frequency region 26.5–40.0 GHz. A-type rotational transitions in the ground vibrational state have been assigned. The effective rotational constants and centrifugal distortion constants were determined to be A = 19 196 ± 323, B = 2132.48 ± 0.01, C = 2112.52 ± 0.01 MHz, D_J = 0.70 ± 0.03 and D_JK = −26.16 ± 0.05 kHz. Analysis of the measured Stark effects gave a dipole moment of 1.80 D with components of |u_a| = 1.62 ± 0.01, |u_b| = 0.68 ± 0.05 and |u_c| = 0.39 ± 0.14 D. From the experimental rotational constants and dipole moments, it is suggested that the assigned spectra have resulted from the skew—trans conformer.     

2,6—双（1′—苯基—3′—甲基—5′—氧代—4′—甲酰吡唑）吡啶稀土配合物的合成

在乙醇－水溶液中合成了１４种２，６－双（１′－苯基－３′－甲基－５′－氧代－４′－甲酰吡啶）吡啶稀土配合物，元素分析确定其化学组成的ＲＥ２Ｌ３．ｎＨ２Ｏ并用紫外可见光谱、红外光谱，核磁共振谱，热分析，荧光光谱，摩尔电导等进行了表征。     

用ICP研究鹿科动物骨质疏松症的微量元素特征

鹿科动物的骨质疏松症是近几年出现的一种疾病，它影响鹿的生长发育和繁殖，病重者死亡。我们采集梅花鹿和白唇鹿的毛，血样，用低温灰化方法和温法消解处理样品，用ＩＣＰ分析了毛，血清中微量元素的含量。病梅花鹿毛样中Ｍｇ，Ａｌ，Ｃａ，Ｔｉ，Ｆｅ，Ｃｕ，Ｚｎ的含量比正常组高，Ｔｉ，Ｃｕ，Ｚｎ的偏差率大于１５％，而Ｓｉ，Ｍｎ，Ｐ，Ｐ，Ａｇ，Ｂａ，Ｌａ，Ｃｅ，Ｐｂ比正常组低，Ｖ，Ａｇ，Ｂａ，Ｌａ，Ｃｅ，Ｐｂ存在...     

Investigation on chiral capillary columns and their application in separation of enantiomers

Six chiral diamide stationary phases (CSPs), namely N-(3-carbobenzoxypropionyl)-L-Val-tert-butylamide (CSP-1), N-undecenoyl-L-Val-S-α-phenylethylamide (CSP-2), N-undecenoyl-L-Val-R-α-phenylethylamide (CSP-3), OV-225-L-Val-tert-butylamide (CSP-4), XE-60-L-Val-tert-butylamide (CSP-5) and polycyanoethyl vinyl siloxane-L-Val-tert-butylamide (CSP-6), were inves-tigated and CSP-6 was crosslinked within narrow bore (70 μm) fused silica capillary columns. Theseparation of amino acid enantiomers on this narrow bore column by gas chromatography (GC) isillustrated.     

反相高效液相色谱分离-安培法检测酚类化合物

本文报道了RP-HPLC-安培法检测测定酚类化合物的条件。在Shim-pack CLC-C_8柱上用含0.05mol/L NaH_2PO_4缓冲溶液的5％甲醇水溶液洗脱分离,于E+1.0V处检测。线性范围在0～7μg/ml,检测限达ng/ml。