x—射线荧光光谱法测定重型催化剂中铂、铕、铈

使用x-射线荧光光谱仪，采用人工合成标样，粉末直接压片和经验系数校正基体效应的方法，建立了重整催化剂中铂、铕、铈含量的测定方法。测定铂、铕、铈的相对标准偏差依次为：0．59％、0．72％、0．75％。     

X-射线荧光光谱法测定加氢催化剂中钼和钴

使用X—射线荧光光谱仪，采用人工合成标样，粉末直接压片和经验系数校正基体效应的方法，建立了加氢催化剂中钼、钴含量的测定方法，测定范围MoO3：4．0％～24．0％，CoO为1．0％～8．0％。该方法不仅快速、简便，而且准确度和精密度较好，测定MoO3和CoO的相对标准偏差均小于1％，满足了科研和工业生产的需要。     

以TritonX-100为增敏剂荧光速率法测定银

基于醋酸钠介质中，银（Ⅰ）催化过硫酸钾氧化荧光素反应，以２，２－联吡啶为活化剂，Ｔｒｉｔｏｎ Ｘ－１００为增敏剂，拟定了测定痕量银的新荧光速率法。本法由于添加 Ｔｒｉｔｏｎ Ｘ－１００表面活性剂，使得灵敏度提高了４倍，测定银含量线性范围为２～３２ μｇ／Ｌ，相对标准偏差为３．１％（ｎ＝９），检出限为１．７６ × １０－３（ｍｇ／Ｌ）。用于测定氯化银的溶度积和光谱感光板中的银，结果满意。     

ARL9800 X射线光谱仪测定烧结矿中氧化亚铁

介绍了用瑞士ARL公司生产的ARL9800X射线光谱仪中配置的X射线衍射（XRD）通道测定烧结矿中氧化亚铁含量，该方法简便，快速，准确，当浓度为10．56％时，相对标准偏差为0．28％。     

普通X—射线荧光光谱仪分辨率的改善

作为改善普通Ｘ－射线荧光光谱仪的分辨率和谱线的低能拖尾现象，于ＰＷ１４０４谱仪上加了可拆卸的限制垂直发散准直器（６．５×２０×５０ｍｍ，片间距０．６５ｍｍ）。实验结果表明，加了限制垂直发散准直器后，谱仪相对分辨率提高１０％，谱仪非对称因子由１．４－１．５改善为１．０－１．１８。为普通Ｘ－射线谱仪用于化学态分析提供了更为有利的条件。     

X射线荧光与粒子激发X射线光谱分析

本文是《分析试验室》定期评述“Ｘ射线荧光光谱分析”系列评论第７篇,简述了１９９６年７月至１９９８年６月国内Ｘ射线荧光光谱分析技术发展的概况,从Ｘ射线荧光光谱仪的研制与改造、特殊激发方式的研究与应用、化学计量学与数据处理方法研究、化学态分析、标准物质与样品制备、测定方法研究与应用６个方面评述了国内Ｘ射线荧光与粒子激发Ｘ射线光谱分析进展。共收录国内学者论文及相关文集１４３篇。     

超细核壳铜-银双金属粉的制备

本文采用置换反应法制备得到了球形、粒径约 50纳米的核壳铜 -银双金属粉末 ,经 X射线衍射和热重分析测试确定其结构为表面点缀结构和完全包覆结构。并用透射电子显微镜和 X射线荧光光谱仪对粉末的形貌和组成进行了测定。     

X-射线荧光光谱法测定白云石中主次量组分

采用粉末压片x-射线荧光光谱法测定白云石中氧化镁、氧化钙、二氧化硅、三氧化二铝、三氧化二铁和二氧化钛含量。采用校正曲线和基体校准一体的回归方程进行谱线重叠干扰校正和基体效应校正。将白云石样品进行磨细处理,在压片机上制成样片,直接在X-射线荧光光谱仪上按照选定的分析条件,以标准样品做工作曲线,利用工作曲线测定样品含量。通过与国家标准化学法以及熔片法对照,分析结果与标准值、熔片法结果吻合,主含量元素测定结果相对误差不超过10％,同一样品12次测定结果相对标准偏差不超过10％。该方法简便、快速、准确、重现性好。     

能量色散X射线荧光法快速测定高冰镍中铁的定量

应用能量色散Ｘ射荧光法速测定高冰镍中铁的含量。以一次射线的康普顿散射线性作内标删采用“负补偿法”校正干扰元素Ｃｕ和Ｎｉ对铁特征荧光的增强作用，取得较好效果，试验表明：本法具有操作简单、速度快、精度较高等优点。对由＾２３８Ｐｕ放射性同位素源、闪烁探测器和双通谱仪组成的测量系统，测定铁一的精度（ＲＳＤ）达到了１．８％，平均绝对误差为０．１６％，单样分析时间为９６ｓ。     

X—射线荧光光谱测定甜瓜中矿质元素

报道了日本理学３０８０Ｅ３型Ｘ－射线荧光光谱仪在测定甜瓜样品旧和微量矿质元素中的的应用。以国家植物标准参考物质（ＧＢＷ）为校准标样，采用真空加热干燥法制备甜瓜样品，所得分析结果与ＩＣＰ－ＡＥＳ对照相吻合。     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described.     

正丁胺对激光染料荧光谱影响的研究

用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在.     

Cu0-catalysed 1,3-dipolar cycloadditions of α-amino acid derived N,N-cyclic azomethine imines to ynones

A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu⁰ as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than Cu^I in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT).     

Synthesis and antioxidative/anti-inflammatory activity of novel fullerene–polyamine conjugates

(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C₆₀, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine.