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1.
提高灵敏度与改善选择性一直是光度分析研究的重要课题,为此近年来提出了许多方法,但部分改善选择性的方法如双波长[1]及三波长法等往往导致灵敏度下降。标准加入双波长光度法[2]是基于等吸收双波长法原理及标准加入法的特点而设计的,该法可消除干扰、改善选择性且不致降低灵敏度。本文在弱酸性介质中,以络天青S(CAS)为显色剂,采用标准加入双波长光度法,建立了同时测定微量铝、铁的方法。本法Al(Ⅲ)的测定范围0.01~0.35mg·L-1,Fe(Ⅲ)的测定范围0.05~0.40mg·L-1,用于二元混合物中铝、铁的同时测定,结果的准确度和精密度均较高。1…  相似文献   

2.
应用双波长标准加入法可消除共存物干扰.改善选择性.扩大了标准加入法应用范围,弥补了等吸收法的某些不足.本文以5-Br-PADAP为显色剂,测定食品、生物材料中Cu(Ⅱ)与Fe(Ⅲ),获得满意结果.  相似文献   

3.
简讯     
双波长标准加入吸光光度法同时测定锌汞国防科技大学研究了一种利用化学计量学原理改善分析方法选择性的计算分析方法——双波长标准加入吸光光度法(简称双标法)。双波长吸光光度法用于多组分相互干扰体系的测定,主要有等吸收点法和系数倍率法等。这两种方法通常是测量信号下降以消除共存物干扰,改善选择性,但在一定程度上  相似文献   

4.
标准加入双波长光度法测定微量锌   总被引:3,自引:0,他引:3  
锌和钴可在弱碱性溶液中与5—Br-PADAP形成紫红色络合物,但吸收峰严重重迭。当两者共存时,虽可用常规双波长法进行选择性测定,但在消除钴的干扰时,测量信号下降而在一定程度上导致灵敏度降低。本文利用标准加入双波长光度法的原理,建立了在钴共存时,不用分离即可选择性测定锌的方法,达到既改善选择性又不降低灵敏度的目的。同时,由于采用标准加入法测定,测量次数增加,使随机误差降低,精密度与准确度均得到提高,而且在进行数据处理时,还可利用两个波长下测得的两条回归直线交点的纵坐标估计出共存钴的浓度,这是常规双波长法所不及的。试验表明,在pH=9.2缓冲溶液中,有表面活性剂OP存在时,以5-Br—PADAP为显色剂可选择性测定微量锌,对合成样品的测定,与常规双波长法相比,结果令人满意。  相似文献   

5.
双波长K系数-标准加入-导数分光光度法同时测定钴、镍   总被引:1,自引:0,他引:1  
1引言双彼长分光光度法通常采用等吸收点法和K系数法,存在灵敏度较低,测量点少而使误差较大的缺点;曾有人提出用双波长标准加入法来提高双波长法的灵敏度,但存在要求具有等吸收点的局限性,操作上也较麻烦.本文将双波长K系数法,标准加入法和导数法三者有机结合,并且独特地同时进行两组分的的标准加入,以一套数据即可完成两组分的同时测定。本方法具有灵敏度高,准确度好,操作简便,适用范围广的优点。2方法原理设样品中有a、b两组分。浓度分别为Ca、Cb,峰值波长对应于λ1、λ2,同时加太浓度为C、C的a、b标准溶液,则波长λ1、…  相似文献   

6.
分光光度法测定微量钡的报导不多,且方法的灵敏度低,选择性大都不好,偶氮磺Ⅲ在pH2.6—7.7可与锶、钡反应,但选择性不佳,未见用于实际样品分析。DBC-偶氮氯膦(以下简称DBC-CPA)是测定稀土元素的新显色剂,我们发现它在高酸度下能与钡生成灵敏的紫色配合物,反应的灵敏度高,用双波长法测定时可消除大量钙的干扰,且等量的钡和锶的△A相等,可方便地测定钡、锶合量,三十余种其它离子允许存在较大量。本法用于多种化学试剂及孕育剂等样品中钡(锶)的测定获得较好结果,方法简便、快速。  相似文献   

7.
用二乙胺二硫代甲酸钠测定Cu(Ⅱ)和Bi(Ⅲ)的新萃取光度法   总被引:3,自引:0,他引:3  
解联立方程法是分光光度法中测定多组分最常用的方法。采用双波长分光光度计,通过波长的适当选择,可以消除共存干扰组分的影响,大大简化了混合物同时测定的手续及其数据处理,并可提高测定的灵敏度和准确度。但是,目前双波长分光光度计甚少,根据双波长系数倍率法原理,我们研究了用单波长分光光度计同时测定相互干扰组分的新方法——倍  相似文献   

8.
双波长分光光度法测定混合组分   总被引:9,自引:3,他引:6  
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。  相似文献   

9.
1 引言 双波长分光光度法由于具有原理简单,测定点数少、计算量小、可消除干扰组分等优点,故仍受到广大分析工作者的青睐。该法的关键是最佳测定波长对的选择和系数K的确定,这可根据所限定的条件由计算机选择。双波长分光光度法多用于分析两组分的复方制剂,但三组分以上的定量检测报道很少。本文应用双波长  相似文献   

10.
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。  相似文献   

11.
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.  相似文献   

12.
KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.  相似文献   

13.
The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.  相似文献   

14.
Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.  相似文献   

15.
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.  相似文献   

16.
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.  相似文献   

17.
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.  相似文献   

18.
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.  相似文献   

19.
20.
Zhanhui Yang  Shiyi Yang  Jiaxi Xu 《Tetrahedron》2017,73(23):3240-3248
Regiospecific and direct imidation of the methyl C(sp3)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.  相似文献   

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