共查询到20条相似文献,搜索用时 187 毫秒
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给出相对于外磁场不同取向的五氧硼酸钾(KB5)单晶的1HNMR室温谱.发现当外磁场在晶体的bc平面里,1HNMR谱最多有6个峰.而在ah或ac平面里,最多仅有5个峰.用计算机拟合NMR谱表明:在五氧硼酸钾中,氢原子是以羟基和水分子集团的形式存在.在羟基集团中,O—H的距离为0.1005±0.001nm和0.1054±0.001nm;而在水分子中,O—H的距离为0.0983±0.001nm和0.0968±0.001nm,并且H—O—H夹角为108°±1°.这些显示本文的数据与中子衍射结果相近,而X射线衍射所得到的质子位置的数据则与我们的结果相距甚远. 相似文献
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报道了一种热转印色带用黄染料的1H、13C NMR , 应用1H NMR、13C NMR、定量碳谱、DEPT、1H-1H COSY、HMQC、HMBC等确定了其在氘代氯仿中的分子结构, 并对全部谱峰进行了归属, 探索了黄染料在氘代氯仿中的结构对13C、1H NMR谱图化学位移及谱峰裂分的影响. 相似文献
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二氢黄酮糖苷化后产生的R与S构型非对映异构体在1H NMR谱上会呈现一些差别,但文献对其差别描述非常有限.为便于利用1H NMR谱图判断二氢黄酮糖苷的R与S构型非对映异构体,本文首先在植物药皂荚提取物中分离得到一种二氢黄酮苷-柚皮素7-O-葡萄糖苷R与S构型混合物,分析其氘代二甲亚砜(DMSO-d6)溶液的1H NMR、13C NMR、1H-1H COSY、1H-13C HSQC和1H-13C HMBC谱,对其1H和13C NMR谱峰进行了归属;然后,采用手性色谱柱对该混合物进行分离,结合圆二色光谱(CD)技术确定构型;最后,为鉴别R与S构型柚皮素7-O-葡萄糖苷在1H NMR谱中特征差别谱峰,避免葡萄糖残基质子对二氢黄酮苷元质子化学位移的影响,采集了R与S构型柚皮素7-O-葡萄糖苷及其混合物氘代乙腈(CD3CN)溶液的NMR谱,结果显示葡萄糖残基端基质子H-1″化学位移差别最为明显,为9.4 Hz;5-位酚羟基质子化学位移差别为5.8 Hz,C环上3个质子化学位移差也较明显. 相似文献
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HR/MAS高分辨魔角微量探头用于天然橡胶固体1H、13C NMR测试及其与液体BBO探头、固体CP/MAS探头测试的比较 总被引:5,自引:0,他引:5
采用BRUKER高分辨魔角微量探头(HR/MAS),液相宽带BBO探头和固体CP/MAS探头,对天然橡胶固体、乳液以及天然橡胶溶于氘代苯的溶液进行了1H、13C 1D和2D NMR谱的测试和比较. 发现HR/MAS探头用于天然橡胶固体和乳液时可以得到高分辨的1H、13C谱,克服了CP/MAS探头测试固体13C NMR谱或者是固体1H NMR谱时,谱图存在S/N值可能较小、谱峰可能宽化的弱点. 相似文献
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Feng Deng Guoxing Wang Youru Du Chaohui Ye Yuhua Kong Xiaoding Li 《Solid state nuclear magnetic resonance》1997,7(4):281-290
The modification of surface hydroxyl groups with sodium in a series of Na2CO3-γ-Al2O3 catalysts was investigated as a function of both the Na2CO3 loading and the calcination temperature by means of 1H magic angle spinning (MAS) and 1H[23Na] spin-echo double resonance NMR techniques. The 1H NMR experiments revealed that sodium ions are homogeneously distributed over the alumina surface and closely coordinated with the surface hydroxyl groups. In the catalysts calcined at 250 °C, the acidic hydroxyl groups (with a chemical shift of 2.0 ppm) are preferentially associated with sodium ions at low Na2CO3 coverages (5 and 10%), while both the acidic and the basic (0 ppm) hydroxyl groups are accessible for sodium ions at high coverages (15 and 20%). The coordination causes a low-field shift of about 2 ppm in the 1H MAS spectra, and a broad signal at 4.5 ppm appears. It is interesting that the 4.5 ppm signal is completely suppressed in the 1H[23Na] MAS experiments, providing direct evidence that a strong interaction exists between adsorbed sodium ions and the surface hydroxyl groups. Increasing the calcination temperature to 450 °C results in preferential removal of the acidic hydroxyl groups, and only the most basic hydroxyl groups remain when the calcination temperature is raised to 600 °C. This is attributed to the formation of the coordinated species
which enhances the acidity of the surface hydroxyl groups and prompts their dehydroxylation, especially at high calcination temperature. Correlation of the 1H MAS NMR results and catalytic activity measurements indicates that the basic hydroxyl groups are essential for the carbonyl sulfide hydrolysis reaction. 相似文献
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K. Fujiwara K. Ichinose H. Nagai A. Tsujimura 《Journal of magnetism and magnetic materials》1987,70(1-3):184-186
In the hydrides YMn2H3.0, the nuclear magnetic resonance of 1H nuclei has been measured under external fields up to 50 kOe at 4.2 K and three 1H NMR signals have been observed. The 1H hyperfine fields corresponding to these NMR signals can be discussed in terms of the dipole interaction between the H nuclei and the localized moments of the Mn(or Fe) atoms surrounding H atoms. 相似文献
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取代基效应(SCS)与乙烯-α-烯烃共聚物的序列结构——7.氢化丁苯共聚物(HBS) 总被引:1,自引:1,他引:0
测定了两个氢化丁苯共聚物样品的1H、13C NMR谱。通过处理文献中的13C NMR谱数据得到了-C2H5和-C6H5的SCS参数。利用乙烯-α-烯烃共聚物的SCS方法结合DEPT NMR实验技术重新归属了该共聚物的13C NMR谱。明确指出,氢化丁苯共聚物分子链中主链任何一个乙烯单元的两个CH2在序列分布上分属于二元组和三元组。CH则用三元组来表征。最后,对HBS共聚物的序列分布进行了计算。 相似文献
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七叶亭衍生物含有药效性较高的苯二酚基团,具有各种生物活性.本文以七叶亭(化合物1)为母体,通过将苯基引入到4位、将甲氧基与羟基分别引入到5、6、7和8位,得到一系列七叶亭衍生物2~14.首先以七叶亭为例,以DMSO-d6作为溶剂,采集了它的多种核磁共振(NMR)谱图(包括1H NMR、13C NMR、1H-13C HSQC、1H-13C HMBC),并进行了较详细的化学位移归属;然后对七叶亭衍生物2~14的1H和13C NMR进行了全归属;另外,讨论了取代基变化对七叶亭及其衍生物上的1H和13C NMR化学位移的影响;最后,使用GIAO和CSGT两种量子化学计算方法计算了七叶亭及其衍生物上的1H和13C NMR化学位移,并与它们的实测值做了比较. 相似文献
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Bachmann S Hellriegel C Wegmann J Händel H Albert K 《Solid state nuclear magnetic resonance》2000,17(1-4):39-51
Pure organic polyalkylvinyl ether phases were synthesized by suspension polymerization using different ratios and compositions of n-butylvinyl ether (C4VE) and n-octadecylvinyl ether (C18VE) with triethylene glycol divinyl ether or divinylbenzene as crosslinkers, respectively. These phases were investigated by means of solid-state 13C cross-polarization magic angle spinning nuclear magnetic resonance (NMR) spectroscopy and 1H high-resolution magic angle spinning (HR MAS) NMR spectroscopy in suspended-state. A comparison of these two methods showed the substantial advantages of 1H HR MAS NMR measurements. Structure elucidation was achieved using a 2D H,H-COSY NMR experiment performed under MAS conditions enabling full peak assignment of the 1H NMR spectra of these phases. The dynamic behavior of the polyalkylvinyl ether phases was determined by employing temperature-dependent measurements of spin–lattice relaxation times (T1) as well as accumulation of a 2D wide line separation NMR spectrum. 相似文献
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制备了高发射效率的稀土多金属氧酸盐BPOM:Eu及ZrPOM:Eu荧光体,并对其结构及发光性质进行了研究。结果表明样品具有Keggin结构,Eu在两类样品中均有肉眼可见的在红光区的强发射。但在BPOM:Eu中以5D0→7F1磁偶极跃迁发射为主,在ZrPOM:Eu中以5D0→7F2电偶极跃迁发射为主。铕在ZrPOM:Eu中的对称性低于在BPOM:Eu中的对称性。这种差异也使铕离子的激发光谱具有不同的特征。铕在两种多金属氧酸盐中均有浓度猝灭,在BPOM:Eu中浓度为2.0%时发射强度最大;在ZrPOM:Eu中浓度为2.4%时发射强度最大。在ZrPOM:Eu中有较弱的配体到中心铕离子的能量传递,而在BPOM:Eu中却未观测到能量传递现象。 相似文献