Further conventions for NMR shielding and chemical shifts (IUPAC Recommendations 2008)

IUPAC has published a number of recommendations regarding the reporting of nuclear magnetic resonance (NMR) data, especially chemical shifts. The most recent publication [Pure Appl. Chem. 73, 1795 (2001)] recommended that tetramethylsilane (TMS) serve as a universal reference for reporting the shifts of all nuclides, but it deferred recommendations for several aspects of this subject. This document first examines the extent to which the (1)H shielding in TMS itself is subject to change by variation in temperature, concentration, and solvent. On the basis of recently published results, it has been established that the shielding of TMS in solution [along with that of sodium-3-(trimethylsilyl)propanesulfonate, DSS, often used as a reference for aqueous solutions] varies only slightly with temperature but is subject to solvent perturbations of a few tenths of a part per million (ppm). Recommendations are given for reporting chemical shifts under most routine experimental conditions and for quantifying effects of temperature and solvent variation, including the use of magnetic susceptibility corrections and of magic-angle spinning (MAS). This document provides the first IUPAC recommendations for referencing and reporting chemical shifts in solids, based on high-resolution MAS studies. Procedures are given for relating (13)C NMR chemical shifts in solids to the scales used for high-resolution studies in the liquid phase. The notation and terminology used for describing chemical shift and shielding tensors in solids are reviewed in some detail, and recommendations are given for best practice.     

高能火花光源激发钢铁和铜合金中铝的看谱分析

采用高能火花光泊激钢铁和铜合金试样,借以进行铝的看谱分析,研究了在高能火花光源激发下光谱出现和其强度变化的规律以及以５６９．６５ｎｍ光谱区域的干扰情况。从而制 钢铁和铜合金中铝的看谱分析方法,并将其应用于生产实践中获得了令人满意的结果。是一种既经济简便及快速实用的分析测定方法 。     

利用近红外光谱检测多层组织血氧饱和度的研究

利用近红外光谱无创检测生物组织血氧饱和状态,是一种极富研究和应用前景的检测技术,在临床检测中被广泛应用.但常规临床检测应用于指端仅反映局部血氧饱和度信息,在使用中具有局限性,信号的可信度也存在质疑.该文提出了一种采用反射式脉搏血氧饱和度检测技术检测生物多层组织氧合状况的新方法,该方法通过调节入射光强以适应解剖学中生物组织多层结构的检测.应用该方法针对手指结构的实验结果表明,随着入射光强的改变,反映血氧饱和状态的光电脉搏波信号有显著变化.结合手指解剖学分析表明,光电脉搏波信号的变化与手指的多层面组织结构相对应,反映不同层面血氧饱和状态.这一特点表明,通过此法可以针对生物组织的多层结构进行测量.     

铁磁绝缘层对正常金属/铁磁绝缘层/正常金属/p波超导结隧道谱的影响

在正常金属/铁磁绝缘层/正常金属/自旋三重态p波超导隧道结中,考虑到铁磁绝缘层的磁散射和粗糙界面散射,运用Bogoliubov-de Gennes(BdG)方程和Blonder-Tinkham-Klapwijk(BTK)理论模型,研究了铁磁绝缘层对隧道结微分电导的影响.研究表明:(1)对于px波,粗糙界面散射和磁散射都能使零偏压电导峰变低,能隙处凹陷升高;随着磁散射的增强,谱线的尖锐峰消失,宽峰逐渐变为凹陷;(2)对于py波,粗糙界面散射和磁散射都能使零能凹陷上移,能隙峰变低,随着粗糙界面散射的增强,两能隙峰间距减小;随着中间正常金属层厚度的增加,能隙内电导随外加偏压呈现振荡行为,能隙外电导仅与普通势垒有关;(3)对于px+ipy波,随着粗糙界面散射的增强,零偏压电导峰被压低,双凹陷处的值逐渐增大为小的能隙峰,而磁散射并不改变谱线中各凹陷处的电导值.     

双钙态矿Sr_2Fe_(1-x)Mn_xMoO_6体系的磁性和磁输运性质的研究(英文)

我们用X射线光电子能谱、以及相关的电性和磁性测量研究了Sr2Fe1-xMnxMoO6(0相似文献   

SSIMS表征催化剂的表面状态和结构层次

自Benninghoven。A 提出静态二次离子质谱(Static Secondary Ion Mass Spectrometry或SSIMS)方法以来,它就成为一种极灵敏的表面分析技术。近年来,SSIMS技术在多相催化研究中的应用日益广泛。我们曾成功地用SSIMS表征过MoO_3-NiO-P_2O_5/γ-Al_2O_3催化剂的表面结构层次.本工作中,我们应用SSIMS,并结合XPS对新型催化剂MoO_-CoO/TiO_2-Al_2O_3的表面结构层次和表面状态作了研究.实验结果和我们原先用PASCA(Positron     

A Study of Ca-Mg Silicate Crystalline Glazes ——An Analysis on Forms of Crystals

In the study on Ca-Mg silicate crystalline glazes, we found some disequilibrated crystallization phenomena,such as non-crystallographic small angle forking and spheroidal growth, parasitism and wedging-form of crystals, dendritic growth, secondary nucleation, etc. Those phenomena possibly resulted from two factors:(1) partial temperature gradient, which is caused by heat asymmetry in the electrical resistance furnace,when crystals crystalize from silicate melt; (2) constitutional supercooling near the surface of crystals. The disparity of disequilibrated crystallization phenomena in different main crystalline phases causes various morphological features of the crystal aggregates. At the same time, disequilibrated crystallization causes great stress retained in the crystals, which results in cracks in glazes when the temperature drops. According to the results, the authors analyzed those phenomena and displayed correlative figures and data.     

Pt(111)单晶电极上乙二醇解离吸附反应动力学

运用电化学循环伏安和程序电位阶跃方法研究了乙二醇在Pt(111)单晶电极上的解离吸附过程.动力学研究的定量结果指出,乙二醇解离吸附反应的平均速率随电极电位变化呈火山型分布,其最大值在0.10 V(vs SCE)附近.测得在含2×10－3 mol•L－1乙二醇的溶液中,最大初始解离速率vi为4.35×10－12 mol•cm-－2•s－1.     

35Cl NMR研究溶液中离子对和离子缔合

测量了Sr和Ba高氯酸盐在乙腈和乙醇中0.5 mol·L~(-1)溶液的~(35)Cl NMR峰宽Δv和粘度η。按核四极矩弛豫机理, 结合文献中Mg~[1]和Ca~[2]盐的数据, 一种溶剂中各盐的Δv/η之比当反映~(35)Cl核处的电场梯度平方之比。按接触型离子对假设, ~(35)Cl处电场梯度平方之比应等于(r_++r_-)~(-6)。测得各盐的Δv/η之比与计算的(r_++r_-)~(-6)吻合, 论证了在乙腈与乙醇中为接触型离子对。同时文中报告了Δv/η和盐的摩尔电导随水或DMF加入的变化。     

酸性介质中1,2-丙二醇在铂电极上吸附和氧化过程的原位FTIR反射光谱研究

应用电化学循环伏安和原位FTIR反射光谱研究1,2-丙二醇在Pt电极上吸附和氧化过程。结果指出1,2-丙二醇的电氧化可按双途径进行。其一经1,2-丙二醇在Pt上解离吸附产物氧化至CO_2。但在较低电位下这些解离吸附产物(红外检测为CO_(ad)、?C=CH_2]_(ad)等)累积吸附于电极上,毒化Pt表面抑制其它反应。当电位大于0.3V后它们一经生成即氧化脱附,从而使1,2-丙二醇得以在未毒化Pt表面经反应中间体氧化至CO_2。在实验条件下,原位FTIR反射光谱检测到的反应中间体可能有HOC-CHOHCH_3(或CH_2OHCOCH_3)和HOOC-COCH_3(或HOOC-CHOHCH_3)等物种。