萃取动力学光度法测定活化剂铝——铝(Ⅲ)-过氧化氢-铜(Ⅱ)-邻氨基酚/氯仿体系

研究了在pH 5.5的弱酸性介质中, 利用Al(Ⅲ)对Cu(Ⅱ)催化H2O2氧化邻氨基酚显色的指示反应的活化作用.用萃取平衡控制反应时间、水相中邻氨基酚的浓度和反应进行的程度.通过在424 nm下测量有机相的吸光度,建立了萃取催化光度法测定活化剂铝的新方法.方法的线性范围为0.004～0.25 mg/L,检出限为1.6×10 -6 g/L.用于水样和茶叶中铝含量的测定,结果满意.     

Multivariate resolution of NMR labile signals by means of hard- and soft-modelling methods

One of the difficulties frequently encountered when studying acid–base equilibria with NMR spectroscopy is the labile behaviour of the measured signal, which hinders the application of bilinear multivariate data analysis methods. In this work, a mathematical transformation is proposed for the conversion of NMR labile signals to inert signals, which make possible the application of multivariate data analysis methods, based on bilinear data models. The procedure has been applied to the analysis of NMR data corresponding to the acid–base equilibria of nucleotides dCMP and dGMP. Both hard-modelling (EQUISPEC) and soft-modelling (MCR-ALS) approaches have been applied for the analysis and resolution of transformed bilinear NMR data matrices.     

聚(St-DVB)型整体柱的制备及其对蛋白质的色谱分离性能

苯乙烯(St)为单体,二乙烯基苯(DVB)为交联剂,在致孔剂甲苯和十二醇存在下,直接以Ф4.6×50mm色谱柱管为模具,同时在整个反应过程中通过氩气对反应混合物施加一个恒定的压力,通过原位聚合制备了聚(苯乙烯-二乙烯基苯)(PSD)型整体柱。在聚合过程中对反应混合物施加一定的压力,使制备的整体柱表面光滑无凹痕现象,并且使柱子的两头平整不凹陷,有利于提高柱效。本文对整体柱的孔结构及其对蛋白质的分离性能进行了研究。实验结果表明,整体柱内部含有大量类似渠道的大孔,孔径为2μm~3μm,在流速为5ml/min时,背压为7MPa。而且流速对色谱分离效率的影响小,流速从1ml/min增大到3ml/min时,牛血清白蛋白和溶菌酶这两种蛋白质的总分离效能指标K1的值基本保持不变,保持在3.35左右,说明可以通过提高流速实现蛋白质的快速分离。     

Synthesis of stereocontrolled α,α-difluoro-β-hydroxycarbonyl materials

Synthesis and synthetic utilities of stereocontrolled α,α-difluoro-β-hydroxy-γ,δ-unsaturated carbonyl compounds via enzymatic resolution with lipase PS (Pseudomonas cepacia, Amano Pharmaceutical Co. Ltd.) or lipase MY (Candida rugosa, Meito Sangyo Co. Ltd.) were described, and then the absolute configuration of obtained chiral materials was determined by the modified Mosher's method.     

α-羟基-1-萘乙酸的合成与拆分

以1-萘甲醛为原料,三乙基苄基氯化铵为相转移催化剂,合成了消旋的α-羟基-1-萘乙酸[(±)-2],收率51.4%.以光学活性(R)-( )-N-苄基苯乙胺为拆分剂,拆分(±)-2得(-)-2,拆分率45.5%.     

中性配合物Cr(acac)_3、mer-和fac-[Cr(bza)_3]的光学拆分

本文用新方法合成了Cr(bza)_3,改进了其mer-、fac-异构体的分离方法;增大了Cr(acac)_3的化学拆分量(1.5g)。试制了DBT(二苯甲酰-d-酒石酸)吸附型手性固定相(CSP),并成功地用于色谱拆分标题配合物的对映体,mer-[Cr(bza)_3]的部分拆分是首次发现的,其他配合物的拆分结果均优于文献方法。根据mer-[Cr(bza)_3)拆分流出液前、后组分的CD光谱,指定了其对映体绝对构型。还讨论了DBT吸附型CSP的拆分效能和色谱特性。     

重油催化裂化汽油中含氮化合物的分析

利用酸萃取技术浓缩分离重油催化裂化（RFCC）汽油中的氮化物，比较了两种萃取剂和两种油剂比对分离效果的影响，结果发现选用10％（体积分数）HCl作萃取剂，油剂比为10：1（体积比）时，碱性氮化物的提取率较高；浓缩分离出的氮化物用色谱－质谱联用方法对其进行了检测，结果表明RFCC汽油中的氮化物主要是C0－C2苯胺及少量吡啶类、喹啉类碱性氮化物。     

An Improvement of IAP OGCM for the Pacific Ocean Circulation and Its Simulated Results

Based on the oceanic CCM with standard stratification subtraction but without the rigid-lid approximation designed in Institute of Atmospheric Physics (IAP OGCM) and its numerical modelings for the large-scale ocean circulation, a numerical model for the Pacific Ocean is developed with higher resolution (2.5°×2° in the longitude and latitude, 8 layers in the vertical),the realistic coastline geometry,the smoothed bottom topography and the Richardson number dependent vertical mixing parameterization.The splitting time integration scheme of the barotropic and baroclinic modes is adopted in the model. The numerical simulation under the annual mean atmospheric forcing shows that the model performance is improved substantially compared with the previous low resolution version.This free surface model,in particular, successfully simulates the well-known ridge-trough structure in the sea level, i.e. the equatorial trough, the equatorial ridge near 3°N, the north countercurrent trough between 8°N and 10°N,     

双冠醚研究(Ⅳ)——Schiff碱型和仲胺型双-(苯并15冠-5)对碱金属苦味酸盐的萃取行为

仲胺型双冠醚与四苯硼酸碱金属盐在丙酮溶液中。25℃下的电导说明它们与Na~+可能形成1∶1络合物(冠醚单元∶金属离子),而与K~+、Rb~+、Cs~+离子则形成2∶1络合物。用Schlff碱型和仲胺型双-(苯并15-冠-5)在水-氯仿体系中进行萃取,测量了分配比D和萃取平衡常数K,发现后者的K值均大于前者。双冠醚F_2对K~+的萃取能力最强,选择性最佳。