流动注射在线共沉淀HG-AFS测定痕量铅

建立了流动注射在线共沉淀HG-AFS测定痕量铅的分析方法。方法基于铅在碱性介质中与氢氧化镁共沉淀，沉淀收集在锥形沉淀腔中，用HCl溶洗沉淀和NaBH4反应，产生的氢化物被载气引入原子化器中进行测定。测定铅的RSD为3％(5ng/mL，n=10)，检出限为0．01ng。检出限较直接进样降低了11倍。对国家标准物质中铅的测定结果与标准值相符。     

二吡啶四硝基酞菁钴的合成及光谱—电化学性质研究

本文报道了以钼酸铵为催化剂,将4—硝基邻苯二甲酸酐、脲和氯化铵混合,于220℃加热合成四硝基酞菁钴,将此配合物溶于吡啶,于115℃加热反应6天合成了二吡啶四硝基酞菁钻配合物。并对二吡啶四硝基酞菁钴的氧化还原半波电势、电解氧化还原产物的电子吸收光谱进行了研究。     

Synthesis and anticancer activities of 5,6,7-trimethylbaicalein derivatives

The aim of this study was to develop potential anticancer agents based on a naturally occurring baicalein, a flavonoid from Scatellariae radix. Cinnamic acid derivatives were converted to corresponding chlorides and then condensed with 3,4,5-trimethoxyphenol in the presence of BF(3) x Et(2)O to give chalcones. Intramolecular cyclization of these intermediates by the actions of DMSO/I(2) afforded the desired trimethylbaicalein derivatives. Cell viability after treatment with the tested compound for 2 d was determined by a colorimetric MTT assay. The results indicated that most of the derivatives showed improved inhibition of proliferation of Hep G2 cells. Compound 9 was the most potent, in which the cell viability was reduced to <2% at the 25 microM level. In the case of Hep 3B cells, 8a, 8b and 8f showed moderate inhibition of their proliferation and 25 microM was required to reduce the viability to ca. 30%. On the other hand, prostate DU145 cells were more resistant. Most of the derivatives caused a 60% inhibition of DU145 cells only at a concentration of 100 microM or above.     

8-羟基喹啉-硅胶介质的合成及其在海水中痕量铅检测的应用

详细研究了以大孔硅胶为基质,一步合成8羟-基喹啉(8-HQ)型金属螯合色谱填料的方法,采用正交试验对合成方法进行了优化。与传统合成方法所得的填料进行了比较,从理化指标等方面来看,新的合成方法为佳。将该法用作微柱流动注射(FIA)在线分离、富集和电感耦合等离子体质谱(ICP-MS)分析流程中的固定相,对大洋海水中的痕量铅进行了在线分析,得到了较满意的结果。     

SELECTIVE SYNTHESIS OF DIMETHYLAMINE OVER RARE EARTH MODIFIED MORDENITES

研究了稀土（Ｃｅ、Ｇｄ和Ｙ）改性丝光沸石用作甲醇胺化催化剂在常压固定床反应器中选择性合成二甲胺的催化性能。结果表明，稀土阳离子交换改性能改善丝光沸石的催化性能。丝光沸石经０．１ｍｏｌ／ＬＣｅ４＋溶液处理，与膨润土成型，再于６００℃下焙烧２～３ｈ，这样制得的催化剂在常压４００℃时的活性及二甲胺选择性分别达到９９．８％和５０．３％。此外，详细探讨了不同改性及制备条件对催化剂催化性能及机械强度的影响。     

Collective and individual plasmon resonances in nanoparticle films obtained by spin-assisted layer-by-layer assembly

Nanoscale uniform films containing gold nanoparticle and polyelectrolyte multilayer structures were fabricated by the using spin-assembly or spin-assisted layer-by-layer (SA-LbL) deposition technique. These SA-LbL films with a general formula [Au/(PAH-PSS)nPAH]m possessed a well-organized microstructure with uniform surface morphology and high surface quality at a large scale (tens of micrometers across). Plasmon resonance peaks from isolated nanoparticles and interparticle interactions were revealed in the UV-visible extinction spectra of the SA-LbL films. All films showed the strong extinction peak in the region of 510-550 nm, which is due to the plasmon resonance of the individual gold nanoparticles redshifted because of a local dielectric environment. For films with sufficient density of gold nanoparticles within the layers, the second strong peak was consistently observed between 620 and 660 nm, which is the collective plasmon resonance from intralayer interparticle coupling. Finally, we suggested that, for certain film designs, interlayer interparticle resonance might be revealed as an independent contribution at 800 nm in UV-visible spectra. The observation of independent and concurrent individual, intralayer, and interlayer plasmon resonances can be critical for sensing applications, which involve monitoring of optomechanical properties of ultrathin optically active compliant membranes.     

过渡金属离子与Schiff碱配合物的研究——Ⅰ.双-[N-(4-甲基苯基)水杨醛亚胺]钴(Ⅱ)的晶体结构与电子结构

过渡金属离子与Schiff碱配合物的合成与性质研究始自50年代,并已有不少论文发表。70年代发现Co(Ⅱ)与Schiff碱的配合物具有抗癌和抗肿瘤活性之后,这一领域的研究工作更加活跃,但对其结构和性质关系的研究多数尚通过谱学方法进行,对标题化合物也只有晶胞参数的报导。为了探讨该类化合物的分子结构与生理活性的关系,本文首先报导标题化合物的晶体与分子结构以及其电子结构的量子化学近似计算结果。     

镧对Rhizoctonia solani的毒力及其致病酶活性的影响

采用琼脂平板生长速率法及液体培养基培养测定了La对立枯丝核病菌(Rhizoctoniasolani)的抑制作用和毒力,并测定了其对病菌胞外的果胶酶、蛋白酶和纤维素酶等几种致病酶的活性的影响。结果表明,随着La浓度升高,对病菌菌丝生长的抑制作用增强,固体培养上所测定的对病菌的EC50和EC95分别为171.9和667.7mg·L-1;在液体培养基中所测定的EC50和EC95分别为111 4和500 7mg·L-1。在一定浓度范围内,La提高了单位量菌丝所产生3种致病酶的活性,但由于对菌丝生长量的强烈抑制,使病菌胞外3种致病酶的总量或总活性受到抑制,减低了病菌的致病力。     

倒数示波计时电位法在合金样品测定中的应用

应用倒数示波计时电位法，在含有吸附络合物的溶液中，采用桂汞电极作为极化电极，测定了Ｃｕ＾２＋、Ｎｉ＾２＋、Ｃｄ＾２＋、Ｐｂ＾２＋等几种金属离子的检测下限，并通过沿（ｄＥ／ｄｔ）－１￣Ｅ曲线上的峰高对合金样品进行定量分析，得到满意结果。实现了示波分析由常量到微量的飞跃。     

Synthesis and Magnetic Properties of Binuclear Mn（Ⅱ）Complexes with Alkoxide Bridge

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