波长色散X射线荧光光谱仪和多晶X射线衍射仪联用技术鉴定进口铜矿和含铜物料

首次研究进口可利用含铜物料与进口铜矿属性的不同特性并建立了鉴定方法,采用X射线荧光光谱法和X射线衍射光谱法联用技术建立铜矿和含铜物料属性的鉴别方法。通过X射线荧光光谱法对铜矿和含铜物料中元素进行定性半定量分析,再用X射线衍射光谱法对铜矿和含铜物料的特征谱峰进行扫描,与X射线衍射仪中标准卡片比对分析,能够确定铜矿和含铜物料的物相组成。结果显示,X射线荧光光谱法测定的铜矿和含铜物料的共同特点是铜的含量较高,达到冶炼铜对原料的要求;硅、铁、钠、钙和镁元素都能够检出;差异性在铅和锌元素在含铜物料中较高,在铜矿石中基本未检出;用X射线荧光光谱法检测出的金属元素,通过X射线衍射仪扫描后与标准图片比对,各元素以不同的形式存在于含铜物料中,且有规律可循。     

应用波长色散X荧光仪和多晶X射线衍射仪联用技术 鉴定进口铜矿和含铜物料

本文首次研究进口可利用含铜物料与进口铜矿属性的不同特性并建立鉴定方法,采用X荧光光谱法和X射线衍射光谱法联用技术建立铜矿和含铜物料属性的鉴别方法。通过X荧光光谱法对铜矿和含铜物料中元素进行定性半定量分析,再用X射线衍射光谱法对铜矿和含铜物料的特征谱峰进行扫描,与X衍射仪中标准卡片比对分析,能够确定铜矿和含铜物料的物相组成。结果显示：X荧光光谱法铜矿和含铜物料的共同特点铜的含量较高,达到冶炼铜对原料的要求,硅、铁、钠、钙和镁元素都能够检出。差异性在铅和锌元素在含铜物料中较高,在铜矿石中基本未检出;在X荧光光谱法检测出的金属元素,通过X衍射仪扫描后与标准图片比对,各元素以不同的形式存在于含铜物料中,且有规律可循。     

尿微量白蛋白的多波段多光程光谱检测

为研究多光程光谱法检测尿微量白蛋白含量的可行性,利用多光程光谱的非线性特性,设计自动微位移测量装置,实现对尿液样品可见波段和近红外波段的多光程(0～4.0 mm)光谱快速采集.采用偏最小二乘法,分别对样本的可见波段、近红外波段、可见-近红外双波段的多光程吸收谱与尿液中白蛋白实际含量建立回归模型,其中,可见-近红外双波段...     

第二近红外窗口荧光Ag2Te量子点的合成

以巯基辛烷为表面配体, 通过调控Ag前体和Te前体的比例, 制备了第二近红外窗口荧光Ag₂Te量子点. 采用透射电子显微镜(TEM)、 X射线衍射光谱(XRD)、 X射线光电子能谱(XPS)、 紫外-可见-近红外吸收光谱和荧光光谱等对产物进行了表征. 结果表明, 制得了粒径均一、 分散性好的油溶性Ag₂Te量子点, 其最大荧光发射波长位于1320 nm, 荧光量子产率高达4.2%.     

皖南西坑Ag—Pb—Zn矿床烯土元素地球化学研究

对比研究了皖南西坑银多金属矿床中赋矿围岩蓝田组地层、成矿有关的花岗岩、矿石、矿床蚀变岩等地质体的稀土元素化学特征,借以示踪成矿物来源。结果表明,西坑银多金属矿床成矿热液、成矿物质主要来源于花岗岩浆作用,成矿热液和富碳酸盐岩地层水岩反应使蚀变岩相对富集重稀土。     

辐照对竹纤维素聚合度及其结晶结构的影响

采用60Coγ射线对高聚合度的造纸用竹纤维素浆粕进行辐照处理,用铜氨溶液法测定辐照前后竹纤维素浆粕的平均聚合度,并采用红外光谱法及X射线衍射法研究其结晶结构的变化。结果表明:竹纤维素的平均聚合度随辐照剂量的增加而下降,当辐照剂量达到15 kGy时,聚合度的下降趋势变缓;但在研究的辐照剂量范围内,竹纤维素的结晶结构未被破坏。     

煤中矿物质及其燃烧后的变化分析

以淮北煤田6煤层煤为样品，采用中子活化法、化学方法、X射线衍射及扫描电镜等方法对煤及其灰样品中的矿物质、微量元素进行了分析，在此基础上，研究了样品中主要矿物的种类及其形成时的影响因素，分析了它们在燃烧前后的主要变化。通过分析可知，样品中主要含有高岭石、石英、方解石和黄铁矿以及多种微量元素；在燃烧过程中，微量元素的含量以及矿物的种类发生了变化，并形成高温稳定的矿物种类。     

聚合物材料结晶度（上）

本文介绍了结晶度概念及IUPAC高分子专业委员会最近有关结晶度各述语的一些规定,几种常用的结晶度测定方法,如X射线衍射、量热法、密度测量、红外光谱法等,对X射线衍射方法作了重点叙述.     

进出口工业碳酸钙粉体的属性鉴定

采用红外光谱法、X射线荧光法、X射线粉末衍射法等多种鉴别技术手段及亲水亲油性实验和沉降体积测定等理化检验方法,对进出口贸易中常见的碳酸钙粉体样品进行属性鉴定研究.讨论了样品不同的检测结果在《进出口税则》商品归类中的应用,并结合进出口报关查验和归类化验实际案例,阐述了该类商品的海关实验室化验方法和税则归类过程,可为进出口工业碳酸钙粉体的属性鉴定,以及确定该类商品在《进出口税则》中的商品编码提供技术参考.     

乙烯-四氟乙烯共聚物的结构表征

利用傅里叶变换红外光谱(溴化钾压片法与衰减全反射法)、X射线衍射和X射线光电子能谱法对粉末状和薄板状两种形态的乙烯-四氟乙烯共聚物(ETFE)进行了结构表征。傅里叶变换红外光谱法分析结果表明:ETFE粉末有明显的-CH2和-CF2吸收峰;X射线衍射法分析结果表明:ETFE薄板的分辨率优于ETFE粉末;X射线光电子能谱法分析结果表明:ETFE粉末与ETFE薄板的-CH2和-CF2基团含量基本一致。X射线光电子能谱分析结果显示:ETFE薄板存在有机硅类脱膜剂的污染,同时ETFE粉末存在更多吸附氧。     

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。     

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.     

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.     

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.     

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。     

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。