毛细管电泳法测定复方鱼腥草片中的绿原酸和槲皮素

建立了毛细管电泳法分析复方鱼腥草片中绿原酸和槲皮素的方法,通过研究缓冲溶液酸度和浓度、工作电压和进样时间的影响优化了分析条件。在优化的条件下,15min内实现了两种分析物质的良好分离。绿原酸和槲皮素峰高和质量浓度分别在0．05～0．80g／L和0．05～1．00g／L范围内成良好线性。基于迁移时间和峰高的重复性(RSD)分别为：绿原酸,1．91％和4．32％;槲皮素,2．30％和3．18％。绿原酸和槲皮素的检出限(S／N=3)分别为0．014g／L和0．015g／L。通过分析实际样品并做加样回收实验进一步验证了该方法的可行性。     

低场核磁共振信号检测电路设计

核磁共振检测以其快速、不破坏样品、直观反映分子结构等优点在诸多领域有着非常广泛的应用. 针对核磁共振检测仪器价格昂贵、体积庞大、操作复杂、不便于实现现场检测等问题, 设计了一种面向小型化低成本低场核磁共振仪的核磁共振信号检测电路. 所提出的电路使用低噪声前置放大器实现传感信号放大, 基于锁定放大的微弱信号检测技术实现了对核磁共振回波信号的有效检测. 实际测试结果表明, 所设计的电路放大倍数高达20000倍, 在高倍噪声的干扰下能够准确检测出幅度在5μV及以上的有用信号. 所提出的低场核磁共振信号检测电路对于发展低成本核磁共振仪器具有较好的应用价值.     

盐酸萃取火焰原子吸收法测定柴油中钠含量

本文所述方法是用ＨＣｌ（１＋９作为萃取剂萃取柴油中的Ｎａ,然后用火焰原子吸收光谱法测定Ｎａ含量。本法具有简便,快速、准确等特点。相对标准偏差６．２％,回收率为２１０１％－１０５％。     

半整数四极体系中心跃迁的多次激发NMR谱

本文对半整数四极体系中心跃迁的多次激发NMR进行了研究,结果表明该方法能够较大地提高接收信号的强度.另外对多次激发脉冲序列的激发带宽问题作了讨论,在实验上用40% NaCl+60% NaNO₂粉末混合物对以上结论作了验证.     

快扫相关核磁共振波谱学

本文阐述了快扫相关核磁共振的理论、实验条件,提出一种用参考信号作处理的快扫相关方法,可得到不失真的慢通过谱,且不需相位校正。还用计算机与CW谱仪配接成实验系统,实现了快扫核磁共振谱的测量。文中对该技术作了详细讨论,指出了它的特点及其重要应用。     

EXAFS STUDY OF THE LOCAL STRUCTURE NANOCRYSTALLINE FeZrB(Cu) SOFT MAGNETIC ALLOYS

The changes of local structures around Fe and Zr atoms in the nanocrystalline films of Fe₈₅Zr₉B₆ and Fe₈₄Zr₉B₆ Cu₁ alloys during annealing process were investigated by extended X-ray absorption fine structure (EXAFS) technique. It is confirmed that Zr atoms always exist in amorphous phase and do not dissolve in the bcc α-Fe crystalline phase. The addition of 1 at% Cu lowers the crystallization temperature.     

SOLID-STATE VARIABLE-TEMPERATURE NMR STUDY ON THE PHASE SEPARATION OF POLYETHER POLYURETHANE ZWITTERIONOMERS

Polyether-polyurethane zwitterionomers based on 4, 4'-diphenylmethane diisocyanate(MDI), methyl diethanolamine (MDEA), and polytetramethylene oxide glycol (PTMO) werestudied with variable-temperature wide-line ~1H NMR. It is found that upon ionization, degree ofphase separation in the polymer system decreased at first due to the loss of hard segmentregularity, while further ionization increased the degree of phase separation through increasinghard phase cohesion and difference of polarity between hard and soft segments.     

直接进样X射线荧光光谱法测定汽油中痕量锰和铁

将样品直接注入液体杯,用X射线荧光光谱法测定汽油中痕量锰和铁含量,锰、铁的检出限为0.2mg·L-1。采用康普顿散射线作内标,部分地校正了样品间的基体差异。     

数学模型的建立及其应用于聚丙烯树脂的近红外漫反射光谱分析

采用偏最小二乘(PLS)回归法,分别建立了近红外漫反射光谱法测定聚丙烯的正己烷提取物及熔体流动速率的数学模型,并选择了最佳光谱预处理方法、谱区范围及主因子数。正己烷提取物及熔体流动速率数学模型的决定系数(R2)分别为98.03%及96.65%、交叉验证均方差分别为0.0495及0.94。结果表明,预测值与标准法测定值较为接近,方法适用于大批量聚丙烯品质分析。     

A SOLID NMR STUDY OF POLYETHERESTER-UREAS

The morphology of some polyetherester-ureas were studied by ~(13)C CP/MAS and ~1H wide-line NMR spectroscopy. It was found that the HDI and MDI based polymers have well crystallized hard segments, whereas the TDI and HMDI based ones have not. For HDI/MDI based polymers, the presented results suggest that the distribution of two kinds of hard segment units is mainly in a block form. The influences of the different hard segment and chain length on the mobility of the soft segment were also studied.