X射线荧光光谱无标样分析在轻合金中的应用

基于X射线荧光光谱仪,运用其无标样分析软件以及元素灵敏度系数校正,分析了镁合金、铝合金样品的元素组成及其含量。结果表明,X射线荧光光谱仪无标样定量分析镁合金、铝合金,其测量结果具有非常高的可靠性和准确度。通过对元素灵敏度系数的校正,可以进一步提高合金的测量精度。     

偏振式能量色散X射线荧光光谱仪分析高炉渣

在偏振化能量色散型X射线荧光光谱仪上,使用一个HOPG次级靶,成功地对高炉渣中主要成分进行了分析。总的测量时间为120 s。此方法所得分析结果与标样中有关组分的证书值相符,也与工作标样中组分的已知值(化学法测得)一致。     

能量色散偏振X射线荧光光谱法测定生铁中锰和钛

探讨了应用能量色散偏振X射线荧光光谱仪测定生铁中锰和钛进行炉前快速分析的方法.对测定锰及钛时仪器的工作条件,试样的制备以及工作曲线的制作等因素作了较系统的试验,该方法所得测定结果与化学法测定结果或标样标准值相吻合,相对标准偏差小于1.5%,与化学法相比,锰和钛的测定时间由50 min缩短到2 min.     

直接燃烧-红外光谱法测定铁合金中碳和硫--用生铁标样作校正标准

红外碳硫仪是根据红外线吸收理论而设计生产的一种专门测定材料中碳和硫的仪器，目前，文献[1～7]等分别规定了红外吸收法测定铁合金中碳、硫含量的方法。根据这些方法，必须选择三个同类型标样依次进行校正后，才能确认系统的线性，但由于分析过程中有时难以找到含量合适的同类型标样．且由于分析条件的每次改变，所有的曲线都须重新校正，这样，给实际工作带来一定困难。     

新铸光谱标样的制备和定值分析结果

本文叙述了新铸铝光谱标样的制备过程，制备出的标样具有工艺先进，化学成分均匀，定值准确及校准曲线啮合系数高等特点。通过试用分析，结果与化学仲裁分析结果相符，很好地满足了光谱分析铸造铝合金化学成分对标样的需求。     

全国有色金属发射光谱和X射线荧光光谱分析第二次论文报告会部分报告摘要

不锈钢特殊零件中镍、铬、锰、钼、钴和钛的X射线荧光光谱无损分析周建兰(洛阳船舶材料研究所) X射线荧光光谱法可以满足快速无损同时测定多元素含量的要求。为减少误关来源,要有相应的固体标样。並保持试样表面X射线辐照面积一致。为此,选用三个以上的基体相同或成分相近的固体标样,绘制荧光强度-浓度关系曲线。然后根据相同条件下测得的试样中待测元素的特征X射线荧光强度,直接从该曲线上查出相应的浓度。在曲线线性部分的范围内可得到准确结果,此时,加只有一个标样,只要牌号相     

X射线荧光光谱法测定平炉渣中主成分

使用3080E3型X射线荧光光谱仪,采用粉末直接压片制样,研磨克服粉末样品的粒度效应,理论d系数法校正基体效应的方法,建立了平炉渣样品中TFe、SiO2、MgO、Al2O3、CaO、MnO、TiO2、P2O5组分的快速测定方法。研究了制样条件,用内控标样作标准曲线,分析结果的相对标准偏差为0．23％～3．17％,满足日常分析的要求。     

X射线荧光光谱法测定垃圾焚烧炉渣中主要成分

使用X射线荧光光谱仪,采用粉末直接压片制样,以研磨的方式克服粉末样品的粒度效应,理论α系数法校正基体效应,建立了垃圾焚烧炉渣样品中SiO2、Fe2O3、MgO、Al2O3、CaO、K2O、TiO2、P2O5八组分的分析方法.用标准化法进行强度漂移校正,用内控标样制做校准曲线,测定结果的精密度和准确度可以满足日常分析要求.     

直读光谱法测定铸铝115中硅铁镁锌铍

铝合金中化学成分测定常用比色法 [1,2 ]与滴定法 [1] ,这两种方法样品消耗量大 ,且需将样品转化成溶液 ,样品处理工作量大 ,预处理过程繁琐 ,耗时多 ,而且所用化学试剂多 ,化验成本偏高。光谱分析速度快 ,准确度高 ,单个样品从接样到报出结果所需时间不超过 1 0 min,是一种金属化学成分测定的快捷方法。但光谱分析对标准样品要求比较高 ,铸铝 1 1 5材料须分析硅、铁、镁、锌、铍五个元素 ,目前市场上的标样不能覆盖该材料 ,因此需要两套标样 ,本文采用ZLD1 0 1、LC4两套标样 ,用自制的控制试样 ,采取控样法分析铸铝 1 1 5样品 ,消除了因…     

普鲁克分析用于近红外光谱仪的分析模型传递

使用普鲁克分析（Procrustes analysis,PA)统计学方法解决多元校正中的模型传递问题，并研究了PA算法中主要因子数及标样数对传递结果的影响，在5台国产CCD近红外光谱仪上进行了试验，初步获得了令人满意结果。     

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。