薁磺酸钠结构确证的波谱学研究

用红外光谱、紫外吸收光谱、一维(1 H、13 C)和二维(1 H-1 H COSY、HMQC、HMBC)核磁共振光谱及质谱对薁磺酸钠进行结构确证。对所有的1 H-NMR和13 C-NMR谱进行了归属;讨论了红外吸收光谱峰所对应的官能团的振动形式,并详细分析了薁磺酸钠质谱图中主要碎片离子的裂解途径,还对样品进行了差热和热重分析。以上研究结果确证了薁磺酸钠的分子结构,并确证其经验分子式为C15H17NaO3S·1/2H2O。     

A Novel siloxane-containing dicarboxylic acid, 1,3-bis(p-carboxyphenylene-ester-methylene)tetramethyldisiloxane,and its derivatives: ester macrocycle and supramolecular structure with a copper complex

The new dicarboxylic acid, 1,3-bis(p-carboxyphenylene-ester-methylene)tetramethyldisiloxane (H₂L, 1) was obtained by treating 1,3-bis(chloromethyl)-1,1,3,3-tetramethyldisiloxane with a mixture of terephthalic acid and terephthalic acid sodium salt in a 1:1 ratio. In this approach, besides the desired compound 1 (33 wt % yield), the condensation cyclic dimer 2 (7 wt % yield) and an oligomer 3 (10 wt % yield) resulted. The reaction between dicarboxylic acid H₂L, where L is the carboxylate ligand, along with imidazole as co-ligand, and copper hydroxide resulted in the formation of a coordination compound [Cu(HIm)₄(H₂O)₂]L·4.5H₂O (4). Single-crystal X-ray crystallography has revealed that the crystal structure of 4 is a self-assembled H-bonded three-dimensional supramolecular structure. FTIR and NMR spectral techniques were also used to characterize the formed structures. Optical and thermal properties of all compounds were studied. The stability of the supramolecular structure in solution (methanol) and with temperature was studied using ATR-FTIR. The ability of the macrocycle 2 to bind potassium cations in solution was investigated by UV–vis spectrophotometry.     

高温下淀粉凝胶化颗粒的结构特征

凝胶化作用是淀粉改性过程中存在的一种现象。采用红外光谱和X-射线衍射方法探讨了淀粉凝胶化颗粒的结构和结晶变化过程。结果表明,在淀粉的高温成型过程中,凝胶化颗粒化学结构没有发生明显的变化,结晶状态则趋于完全无定型化。     

一个新颖的二茂铁羧酸混配合物的制备、晶体结构及电化学性质研究

本文以3-二茂铁羰基丙酸(L1)、1，1′-二茂铁二羰基-3，3′-双丙酸(L2)、2，2′-联吡啶胺(dpa)以及Zn(Ac)₂·2H₂O为原料合成了一个结构新颖的混配合物[Zn₂(L1)₂(L2)(dpa)]。X-射线单晶衍射分析表明，该配合物是一个中心对称的双核配合物，并在N-H…O氢键和C-H…O氢键的作用下形成了二维的超分子化合物。采用差示脉冲对该配合物的电化学性质进行了初步的研究。     

羟丙基-β-环糊精对1-羟基芘与牛血清白蛋白相互作用的影响

在模拟生理条件下,利用荧光光谱、圆二色光谱和紫外-可见吸收光谱探究了羟丙基-β-环糊精(HPCD)对1-羟基芘(1-OHPyr)与牛血清白蛋白(BSA)相互作用的影响及其相关机制.结果表明,291 K下HPCD可使1-OHPyr与BSA的结合常数降低为1.45×10~5L/mol;导致1-OHPyr-BSA体系中BSA的α-螺旋含量恢复,色氨酸(TRP)残基周围微环境的极性变化减弱;致使1-OHPyr及BSA的荧光寿命均延长,且二者的结合距离增大.初步研究结果表明,HPCD与1-OHPyr的包络作用是HPCD影响BSA与1-OHPyr结合的主要原因.     

剪切载荷作用下植物细胞的力学特性分析

根据植物细胞的结构特点,以二维问题为研究对象,在已建立的植物单细胞力学模型的基础上,利用有限元方法和MATLAB计算软件研究了单细胞受到剪切载荷作用时,外力、应力、应变及内压间的相互关系,给出了关系曲线图。得出了在剪切情况下,外力、应力、应变及内压之间的关系是非线性的;细胞内压改变量随外力或细胞变形或细胞壁应力的增加而增加;细胞壁的应力随剪切力的增大而增大;细胞将在哪个方向破裂等6个结论。     

Application of high field spectroscopic imaging in the evaluation of temporal lobe epilepsy

Previous spectroscopic imaging studies of temporal lobe epilepsy have used comparisons of metabolite content or ratios to lateralize the seizure focus. Although highly successful, these studies have shown significant variations within each of the groups of healthy subjects and patients. This variation may arise from the natural differences seen in metabolite concentration in gray and white matter, the complex anatomy seen about the hippocampus, and the large voxels typically employed at 1.5 T. Using a 4.1 T whole body system, we have acquired spectroscopic images with 0.5 cc nominal voxels (1 cc after filtering) to evaluate the regional variation in metabolite content of the hippocampus, temporal gray and white matter, midbrain, and cerebellar vermis. Using a threshold value of 0.90 for CR/NAA, a value 90% of all normal hippocampal voxels lay below, we have correctly identified the presence of epileptogenic tissue in patients with unilateral as well as bilateral seizures. By using comparisons to healthy values of the CR/NAA ratio, this method enables the visualization of bilateral disease and provides information on the extent of gray matter involvement.     

一个素数和两个素数的平方和问题

本文证明了最多有O(N13/30+ε)个例外之外,所有的正的奇整数n≤N,n≡0或1(mod 3)能表示成一个素数和两个素数的平方和.     

铜-康铜热电偶的低温不均匀性实验研究

从冰点到液氮温度的宽低温区内,对随机选取的铜-康铜热电偶进行了重复性精度标定.测试结果表明,多次断偶重复焊接行为将产生约0.272 mV的标准差.这意味着在液氮条件下,温度测量过程的最大误差将达8.98 ℃.所以,对现场、尤其对深冷区的现场进行精确测温实验中出现的断偶故障,重新焊接后必须重新标定才能继续使用.