双波长分光光度法测定混合组分

双波长分光光度法测定单组分,倘若以显色试剂吸收峰为参比波长,配合物吸收峰为测量波长(即双峰双波长法)可显著提高灵敏度,将该法用於混合组分体系的测定还未见报导。本文对双波长分光光度法测定混合干扰体系进行了研究,导出了双波长分光光度线性方程,对轻、重稀土-二甲酚橙-CTMAB体系及钴、镍-PAR体系进行了测定,采用直线回归及最小二乘两种方法处理实验数据。理论及实验均表明,采用此法测定混合组分体系,灵敏度较通常的单波长测定法有所提高。     

三波长分光光度法研究：Ⅰ.K系数法测定混合三组份

本文提出利用三波长分光光度法测定混合三组份中的单一组份。在适宜的测量波长组合下,使共存的两种干扰组份的差吸光度为零,消除其干拢,而△A=A_(λ1)-K(A_(λ2)+A_(λ3))只与待测组份的浓度成正比。可直接测定三种组份或某一组份,无需进行分离和繁杂的计算,简便实用,可获得较好的准确度和精密度。讨论了选择波长组合的方法,并编制了程序,用计算机来选择最佳波长组合。     

双波长K系数－标准加入分光光度法同时测定重油中的钴、

本文提出一种同时测定两组分的新方法，即双波长Ｋ系数－标准加入分光光度法。该法同时进行两组的标准加入，以两个组分的最大吸收波长为测定波长，又互为参比波长，以一套吸光度数据同时完成两个组分的测定。本法已用于重油中钴、镍的同时测定，结果满意     

双波长K系数-标准加入-导数分光光度法同时测定重油中的钴镍

本文提出了一种同时测定两组分混和物的新方法，即双波长Ｋ系数－标准加入－导数分光光度法，该法同时进行两组分的标准加入，以两个组分的峰值波长为测定波长，又互为参比波长，利用Ｋ系数法以一套吸光度数据同时完成两个组分的测定。本文以ＯＰ－５－Ｂｒ－ＰＡＤＡＰ为显色体系，同时测定了重油中的钴、镍，结果令人满意。本方法简便，灵敏度高。     

多波长线性回归-矩阵法同时测定乙二醛、乙醛酸、草酸的含量

根据实验得出的乙二醛、乙醛酸、草酸三组分混合物中各组分在特定波长下呈现出的良好的线性关系,建立起三组分质量浓度与混合吸光度的回归方程组,形成了多波长线性回归-矩阵法,实现了乙二醛氧化制备乙醛酸体系中反应产物乙二醛、乙醛酸、草酸含量的同时测定.研究结果表明:当乙二醛检测下限为1.024 mg/L时,回收率为94%~98%...     

双波长K系数—导数吸光光度法同时测定重油中钴和镍

提出了双波长K系数-导数吸光光度法,以样品中两组分的峰值波长互为测定波长和参比波长,以一套导数值数据进行两组分的同时测定,具有简便、灵敏度高的优点.以三正辛胺萃取分离干扰离子,OP—5-Br-PADAP显色体系同时测定了重油中的钴、镍.结果令人满意.     

比值导教光谱法同时测定苯酚间苯二酚对苯二酚

以比值导数光谱法对苯酚、间苯二酚、对苯二酚的二组分和三组分混合体系进行了分析。方法以混合物的波谱除以干扰组分的波谱得到比值波谱,再用“减(加)法技术”以比值波谱对波长求导得到比值导数波谱,方法兼具导数光谱法能消除低频背景和高频噪声干扰的优点。由此得到的比值导数波谱可完全消除干扰组分的吸光度的贡献。此法可很方便对二组分体系进行测定。进一步以求得的比导数波谱对波长二次求导,可对三组分体系进行分析,用此法对以上的二组分和三组混合体系进行分析均得到较好结果。     

双波长K系数—标准加 入分光光度法同时测定重油中的钴,镍

本文提出了一种同时测定两组分的新方法，即双波长Ｋ系数－标准加入分光光度法。该法同时进行两组的标准加入，以两个组分的最大吸收波长为测定波长，又互为参比波长，以一套吸光度数据同时完成两个组分的测定。     

吸光光度多组分同时测定方法研究——MR和PLS法测定钴、镍、铜三组分混合体系

用偏最小二乘法(PLS)和多元线性回归法(MR)分别对钴、镍、铜三组分混合体系进行同时测定,证明PLS法对光谱重叠严重的体系较MR法有更好的预报准确性.着重讨论了校正集样品数n、波长数,和特征变量数d等测定参数对预报结果的影响.     

双波长K系数—标准加入—导数分光光度法同时测量重油中的钴镍

本文提出了一种同时测定两组分混和物的新方法，即双波长Ｋ系数－标准加入－导数分光光度法，该法同时进行两组分的标准加入，以两个组分的峰值波长为测定波长，又互为参比波长，利用Ｋ系数法以一套吸光度数据同时完成两个组分的测定。     

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.     

A carbanion induced synthesis of highly congested pyrazole and imidazole containing heterocycles

An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.     

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.     

Selective synthesis of 4,5-dihydroimidazo- and imidazo[1,5-a]quinoxalines via modified Pictet–Spengler reaction

An efficient tandem approach for the selective synthesis of 4,5-dihydroimidazo[1,5-a]quinoxalines 6a–g and imidazo[1,5-a]quinoxalines 7a–h by the reaction of 2-imidazolyl anilines 4a–c with aryl aldehydes 5a–k under mild reaction conditions is described. Introduction of electron releasing alkyl groups in substrates 4a–b was found to be instrumental for the success of the reaction.     

Understanding the Diels-Alder reactivity of 1,2-azaborine analogues

The Diels-Alder reactivity of 1,2-heteroborines (H₄C₄B(H)X, X?=?NH, PH, AsH; O, S, Se) has been computationally explored by means of Density Functional Theory (DFT) calculations. The influence of the HB?=?X fragment on the reactivity of the system has been quantitatively analyzed in detail by means of the so-called Activation Strain Model (ASM) of reactivity. It is found that the interaction between these species and the dienophile is significantly stronger than that computed for their all-carbon isoelectronic counterpart, benzene. In addition, the strain energy plays a key role in the observed reactivity trends. The role of the aromaticity strength of these heteroarenes on the reactivity is also assessed.