基于FTIR和XRD法分析阜新长焰煤结构特征

为了研究阜新长焰煤的大分子结构,通过测定12个煤样品的工业分析和元素分析,选取最接近平均值的煤样CYM-9作为实验样品,采用傅里叶红外光谱(FTIR)、X射线衍射(XRD)和单轴压缩实验对煤样进行研究,通过与抚顺长焰煤结构特征进行对比,进一步分析煤的微晶结构参数及其力学特性。研究结果表明:CYM-9煤样的基本结构特征参数芳氢率(farH)为0.47,氢碳原子比(H/C)为0.858,芳碳率(farC)为0.747,脂肪烃支链长度(CH3/CH2)为0.617。与抚顺长焰煤结构相比,其芳碳率较大,芳香核缩合程度较大,芳香结构单元排列秩序较规则;煤样XRD图谱具有002峰和100峰两条明显的峰,层间距(d002)为0.3816nm,层片堆砌高度(Lc)为1.2462nm,层片直径(La)为1.0136nm,芳香堆砌层数(N)为4.26;煤样的平均峰值强度为9.24MPa,达到峰值强度时平均应变值为23.58×10-3,平均弹性模量为405MPa。     

两种溶剂精制煤(SRC)的组成和结构 Ⅱ.芳烃馏份的核磁共振波谱及FT红外光谱分析

利用~(13)C-,~1H-n.m.r.(包括多脉冲自旋回波~(13)C-n.m.r.)及FT红外光谱对大同和抚顺两种煤的SRC芳烃馏份进行了分析。对芳烃样品的有关谱图进行了定性分析,并采用~(13)C-,~1H-o.m.r.联合推导平均分子结构的方法计算了各样品的平均结构参数。研究表明,两种煤SRC芳烃的组成结构有显著差别:抚顺SRC芳烃的芳核具有敞开式构型,稠合芳环数小(约3个),脂环发达。大同煤SRC衍生的两个芳烃馏份都具有较高的芳香度,其中DT-2A环数3-4,缩合度高,含较多的芘和荧蒽的同系物,DT-2B为6芳环的渺位缩合多环芳烃。     

薁磺酸钠结构确证的波谱学研究

用红外光谱、紫外吸收光谱、一维(1 H、13 C)和二维(1 H-1 H COSY、HMQC、HMBC)核磁共振光谱及质谱对薁磺酸钠进行结构确证。对所有的1 H-NMR和13 C-NMR谱进行了归属;讨论了红外吸收光谱峰所对应的官能团的振动形式,并详细分析了薁磺酸钠质谱图中主要碎片离子的裂解途径,还对样品进行了差热和热重分析。以上研究结果确证了薁磺酸钠的分子结构,并确证其经验分子式为C15H17NaO3S·1/2H2O。     

抚顺烟煤的固体核磁共振 X射线衍射和电子能谱的研究

用高分辨固体核磁共振,X射线衍射和光电子能谱等近代物理方法,研究了抚顺西露天矿长焰煤的镜煤质,以及该镜煤质的吡啶不溶物,吡啶可溶苯不溶物和超临界抽提后的残煤的大分子结构。获得了上述样品的芳香度参数(fa)、碳原子分布、微晶参数(dr,dm,da,dc)及碳、氧、氮元素的结合形态。并对抚顺西露天长焰煤的大分子结构提出了一些初步的看法。     

基于苯并咪唑-5-羧酸和对苯二甲酸配体构筑的二维镉配位聚合物的合成、晶体结构及荧光性质(英文)

水热条件下利用苯并咪唑-5-羧酸,1,4-对苯二甲酸和Cd(NO3)2·4H2O为反应物合成出了一个配位聚合物{[Cd(Hbic)(bdc)1/2]·H2O}n(1),并分别用元素分析,红外谱图,热重分析,X-射线粉末衍射和X-射线单晶衍射对其结构进行表征。结构分析表明该化合物为二维层状结构,其中每个独立的层都是由两种芳环羧酸配体连接链状的[Cd(COO)]n次级构筑单元所构成,有趣的是在二维层中还存在着笼状的空腔结构。邻近的二维层之间通过分子间氢键和π-π堆积作用进一步扩展为三维超分子结构。荧光谱图表明常温固态下配合物1发射绿色荧光,最大发射峰位于506 nm。     

麦草造纸黑液中木质素的提取及结构分析

采用有机溶剂萃取的方法从麦草造纸黑液中提取木质素,并采用红外光谱（FT—IR）、^1H NMR、紫外光谱等方法对其结构进行了表征．试验表明,所提取的木质素具有明显的紫丁香基和愈疮木基苯环结构．同时测定了木质素的元素组成和甲氧基含量,并计算得到经典的C9结构模型,其结构形式为C9H8.89O1.17（OCH3）1.39.     

山西高阳焦煤碳结构研究与谱学表征

煤是由多种官能团、多种化学键组成的复杂有机结构大分子物质,有机质碳是煤结构的骨架,是构成煤中有机质及形成焦炭的主要元素。研究炼焦煤中的碳结构,对构建炼焦煤大分子结构模型,认知炼焦煤结构及反应性具有重要意义。分别利用Peakfit V4和XPS Peak4.1软件对~(13)C CP/MAS-NMR、FTIR和XPS谱图进行拟合解析,对比研究不同测试方法的解析结果,探索炼焦煤中碳结构的主要特征,获取芳碳率、芳氢率、芳核平均结构尺寸等煤结构单元基本参数。山西高阳焦煤芳碳率的~(13)C CP/MAS-NMR、FTIR和XPS分析结果基本一致,分别是0.81、0.83和0.81。FTIR分析结果表明,芳香结构主要包括苯环二取代、苯环四取代和苯环五取代,占比分别是39.63%、32.24%和28.13%。脂肪结构主要以亚甲基形式存在,含量达到77.43%,甲基、次甲基含量依次减少,脂肪烃碳链长度较短为0.11。因此,山西高阳焦煤中存在较多的烷基侧链。根据~(13)C CP/MAS-NMR拟合结果,获知甲基碳f_(al)~*_、亚甲基碳/次甲基碳f_(al)~H_、氧接脂碳f_(al)~O、羰基碳/羧基碳f_a~C、芳烃碳f_a′、烷基取代芳碳f_a~S、芳香桥碳f_a~B、氧接芳碳f_a~P分别为0.06、0.06、0.04、0.05、0.76、0.10、0.28、0.03,计算得到芳碳率f_a、脂碳率f_(al)、质子化芳碳f_a~H、非质子化芳碳f_a~N和芳核平均结构尺寸X_b分别为0.81、0.19、0.35、0.41和0.37。XPS和~(13)C CP/MAS-NMR分析结果表明,山西高阳焦煤中羰基、醚氧键和酚羟基等碳氧官能团含量约占碳结构的5%。     

NiO在USY分子筛、γ-Al2O3及其 混合载体上的NO吸附行为和分布规律

运用红外技术和高斯函数对红外谱图进行分峰拟合,研究了对NiO在USY分子筛、γ-Al     

峰峰矿烟煤超临界流体抽提产物的结构分析

选用了峰峰矿不同变质程度的三种烟煤为原料，在20MPa,340℃条件下，以甲苯为溶剂进行超临界抽提。采用溶剂萃取和硅胶色谱法将抽出油分为F1－F6六个馏分，从各馏分的^1H-NMR谱图、^13-C-NMR谱图和IR光谱图分析了它们的组成、结构；由元素分析和平均分子量数据，采用^1H-NMR谱和^13C-NMR谱相结合的计算方法，获得了各馏分的平均结构参数。实验结果表明：随着变质程度的不同三种烟煤的组成结构存在着差异，焦煤抽出物中的油含量较高（35.6%)，瘦煤抽出物中的沥青烯含量较高（67.7%)；三种烟煤中煤的芳碳率最高，而肥煤比焦煤、瘦煤有较长的烷基侧链。     

含肽键芳酰腙镧(Ⅲ)配合物的合成、表征及对四种作物病害的抑制作用

合成了未见文献报道的镧(Ⅲ)与含肽键芳酰腙配体(2-羰基丙酸水杨酰腙)的配合物,经化学分析、元素分析及摩尔电导率等表征推测其组成为:La(H2L)(HL)·H2O(H3L为2-羰基丙酸水杨酰腙C10H10N2O4)。通过红外、紫外及荧光的研究表明配体以羧基氧、羰基氧和亚氨基氮与La3+三齿配位,形成了两个共边五元环的稳定结构。盆栽活体试验表明该配合物对四种作物病害都有不同程度的抑制作用,其中对小麦条锈病的防治效果最好,防治效果达80.8%。     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.     

Calculation of enthalpies of hydrogenation of hydrocarbons

Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。