人尿中异黄酮的高效液相色谱分析

建立了测定人尿中异黄酮组分(大豆苷原、黄豆黄素、雌马酚、染料木黄酮)含量的反相高效液相色谱法。在尿样中加入黄酮作为内标,异黄酮经酶解后在pH=7.0中性条件下用乙酸乙酯(1∶1)提取,然后用0.02%TFA-M eOH-ACN三元梯度洗脱的方法分离异黄酮。在该条件下,大豆苷原、黄豆黄素、雌马酚、染料木黄酮的检出限分别为12.9 nmol/L、13.9 nmol/L、71.6 nmol/L和11.8 nmol/L;回收率均在89%以上。本方法具有测试步骤简单、准确度高、重现性好等优点,适合大批量样品测定。     

贝克曼离心机故障排除两例

简要介绍贝克曼离心机触摸键盘失控和控制参数显示混乱两例故障的故障现象、故障分析以及故障排除方法。     

锗钨酸分子间化合物的合成和结构研究

以锗钨酸和4-甲基吡啶为原料合成了分子间化合物H₄GeW₁₂O₄₀·5C₆H₇N·CH₃CN。单晶X-射线分析表明，属正交晶系，空间群P2₁2₁2₁, 晶胞参数a=13.533(5),b=20.835(5), c=21.859(7)?，V=6164(3)?³。Dc=3.650 Mg/m³, Z=4。对3934个可观察到的衍射点进行全矩阵最小二乘法修正后，可靠性因子R=0.0534。     

时间分辨激光荧光光谱分析方法研究——Ⅰ.铽、镝配合物共存时的分辨原理实验

本文对镝存在时铽的测定,进行了时间分辨激光荧光光谱分析方法的原理性实验。选择Tb、Dy-Sal乙醇溶液体系,测量了Tb~(3+)离子浓度范围为0.01～10μg/ml。Dy~(3+)离子浓度为0.1～100μg/ml范围内的荧光寿命。并得到了此范围内配合物离子浓度与荧光强度具有线性关系的结果。     

Preparation of Nano-Sized γ-Al2O3 Supported Iron Catalyst for Fischer-Tropsch Synthesis by Solvated Metal Atom Impregnation Methods

Two types of small iron clusters supported on γ-Al2O3-RT(dehydroxylated at room temperature) and γ-Al2O3-800 (dehydroxylated at 800 ℃) were prepared by solvated metal atom impregnation (SMAI) techniques. The iron atom precursor complex, bis(toluene)iron(0) formed in the metal atom reactor, was impregnated into γ-Al2O3 having different concentrations of surface hydroxyl groups to study the effect of surface hydroxylation on the crucial stage of iron cluster formation. Catalysts prepared in this way were characterized by TEM, M(o)ssbauer, and chemisorption measurements, and the results show that higher concentration of surface hydroxyl groups of γ-Al2O3-RT favors the formation of more positively charged supported iron cluster Fen/γ-Al2O3-RT, and the lower concentration of surface hydroxyl groups of γ-Al2O3-800 favors the formation of basically neutral supported iron cluster Fen/γ-Al2O3-800. The measured results also indicate that the higher concentration of surface hydroxyl groups causes the rapid decomposition of precursor complex, bis(toluene)iron(0), and favors the formation of relatively large iron cluster. Consequently, these two types of catalysts show different catalytic properties in Fischer-Tropsch reaction. The catalytic pattern of Fen/γ-Al2O3-RT in F-T reaction is similar to that of the unreduced α-Fe2O3 and that of Fen/γ-Al2O3-800 is similar to that of the reduced α-Fe2O3.     

APPLICATION OF THE MOMENT METHODS TO ANALYSIS OF X-RAY DIFFRACTION LINE PROFILE FOR PA1010-BMI SYSTEM

Pure X-ray diffraction profiles have been analysed for polyamide 1010 and PA1010--BMI system by means of multipeak fitting resolution of X-ray diffraction.The methods ofvariance and fourth moment have been applied to determine the particle size and strainvalues for theparacrystalline materials.The results indicated that both variance and fourthmoment of X-ray diffraction line profile yielded approximately the same values of theparticle size and the strain.The particle sizes of(100)reflection have been found todecrease with increasing BMI content,whereas the strain values increased.     

用WAXD和SAXS研究辐照聚酰胺1010结构

用ＷＡＸＤ和ＳＡＸＳ方法研究了聚酰胺１０１０的聚集态结构和结晶结构的辐射损伤过程和机理。辐射交联与裂解主要在非晶区和结晶表面或中间相发生；辐射损伤并从这里开始，随辐射剂量增大，非晶化逐渐向晶区伸展，有氢键的（０１０）晶面损伤几率高于（１００）晶面；辐射后效应导致新的交联与裂解生成，主要影响（０１０）晶面的形成与完善，使Ｌ１００及Ｗｃ变小。     

Highly efficient, one-step macrocyclizations assisted by the folding and preorganization of precursor oligomers

Highly efficient, one-step macrocyclizations leading to the formation of macrocyclic hexa(aramides) in high yields (69-82%) are described. The one-step macrocyclizations were facilitated by the preorganization or folding of the backbones of uncyclized precursors in the course of macrocyclization. The preorganization of backbones was achieved by the presence of localized three-centered hydrogen bonds that were adopted in the design of a class of closely related, backbone-rigidified foldamers. The macrocyclization involved reactions between diacid chloride 1 and diamine 2. The crude reaction mixtures and products were conveniently examined by mass spectrometric method (MALDI-TOF). Compared to most traditional one-step macrocyclizations that usually require high dilution conditions and often lead to very low overall yields of the desired products, cyclic hexamers 3 were obtained as the overwhelmingly major product under a variety of reaction conditions, suggesting the generality of this approach.     

影响白砂糖色值测量结果的原因探讨

研究了水质、滤膜、溶液浓度、糖液ｐＨ值、混浊度的变化与白砂糖色值的关系。研究结果表明，溶液的ｐＨ变化影响最严重。不调整糖液ｐＨ与用ＨＣｌ或ＮａＯＨ调整糖液ｐＨ对比所得白砂糖色值的结果是满意的。标准偏差１１２～１８６，相对标准偏差１１６％～２２５％，调ｐＨ使结果偏高，导致产生系统误差。因此：测定白砂糖色值不宜调整糖液的ｐＨ。     

电解沉积压电频移分析的理论与验证

提出了控制电位电解和恒电流电解两类电解沉积的压电频移分析法测定的理论公式,用实验结果验证了它的正确性.