有機(jī)化學(xué)中的光譜方法

前言

This book is the sixth edition of a well-established introductory guide to the interpretation of the ultraviolet, infrared, nuclear magnetic resonance and mass spectra of organic compounds. It is a textbook suitable for a first course in the application of these techniques to structure determination, and as a handbook for organic chemists to keep on their desks throughout their career.   These four spectroscopic methods have been used routinely for several decades to determine the structure of organic compounds, both those made by synthesis and those isolated from natural sources. Every organic chemist needs to be skilled in how to apply them, and to know which method works for which problem. In outline, the ultraviolet spectrum identifies conjugated systems, the infrared spectrum identifies functional groups, the nuclear magnetic resonance spectra identify how the atoms are connected, and the mass spectrum gives the molecular formula. One or more of these techniques nowadays is very frequently enough to identify the complete chemical structure of an unknown compound, or to confirm the structure of a known compound. If they are not enough on their own, there are other methods that the organic chemist can turn to: X-ray diffraction, microwave absorption, the Raman spectrum, electron spin resonance and circular dichroism, among others. Powerful though they are, these techniques are all more specialised, and less part of the everyday practice of most organic chemists,We have kept discussion of the theoretical background to a minimum, since application of the spectroscopic methods is possible without a detailed command of the theory behind them. We have described instead how the techniques work, and how to read each of the four kinds of spectra, including each of the most important 2D N-MR spectra. We have included many tables of data at the ends of Chapters 2, 3 and 4, all of which are needed in the day-to-day interpretation of spectra. Finally in Chapter 5, we work through 11 examples of the way in which the four spectroscopic methods can be brought together to solve fairly simple structural problems, and there are 33 problem sets for you to work through for practice.In preparing a sixth edition, we have almost completely rewritten the book, to reflect our experience teaching the subject, and to respond to changes that have taken place, both of emphasis and of fact, since the fifth edition was published. The chapters on UV and IR spectra are more concise, the chapter on NMR is expanded, and the chapter on MS made more specific to the everyday, rather than to the more specialised, applications of this technique. The appearance of IR absorptions, formerly gathered at the end of the chapter, are now illustrated at the relevant points in the text. Conversely, we have moved the tables of IR data to the end of the chapter, where they are more convenient for reference, and match the arrangement we have always used for the NMR and MS chapters. Most significantly, we have replaced all of the 60 MHz spectra used hitherto to explain the fundamentals of NMR spectroscopy with new and carefully chosen examples at 400 MHz or more. We have also chosen several new compounds with which to illustrate better the common 2D NMR techniques.

內(nèi)容概要

　　本書是一本由英國(guó)劍橋大學(xué)D. H. Williams和I. Fleming合著的有機(jī)化學(xué)光譜方法經(jīng)典教材。第1版出版于1966年，本書為第6版。書中講述了近年來迅猛發(fā)展的二維核磁共振（如Tocsy、遠(yuǎn)‘H-13C COSY）、MALDI、FT-ICR、TOF等新技術(shù)。與時(shí)俱進(jìn)，本版較前版在內(nèi)容上做了較大的改動(dòng)，有關(guān)UV和IR光譜的部分講述的更加準(zhǔn)確；豐富了關(guān)于NMR的內(nèi)容；介紹MS的部分更加講求結(jié)合實(shí)際。全書共分為五章，第1章為紫外和可見光譜，論述了電子吸收光譜在測(cè)定有機(jī)基團(tuán)中的應(yīng)用；第2章紅外光譜，闡述了傅里葉紅外和喇曼光譜的樣品制備、光譜選律以及各官能團(tuán)的特征吸收頻率；第3章核磁共振波譜，主要介紹了‘H和13C核磁共振的經(jīng)驗(yàn)參數(shù)、各種二維NMR的具體應(yīng)用；第4章質(zhì)譜，介紹了各種粒子譜以及氣相和液相色譜與質(zhì)譜的聯(lián)用；第5章實(shí)例和習(xí)題，為讀者提供了一些選自研究課題、具有啟發(fā)性的實(shí)例，也為讀者鞏固所學(xué)的知識(shí)提供了練習(xí)。本書理論和實(shí)踐并舉，因此也適合有機(jī)化學(xué)工作者做為手冊(cè)使用?！　∽x者對(duì)象：高校化學(xué)系師生、有關(guān)研究人員。

作者簡(jiǎn)介

作者：(英國(guó)) 威廉姆斯 (Williams.D.)

書籍目錄

PrefaceChapter 1: Ultraviolet and visible spectra  1.1 Introduction  1.2 Chromophores  1.3 The absorption laws  1.4 Measurement of the spectrum  1.5 Vibrational fine structure  1.6 Choice of solvent  1.7 Selection rules and intensity  1.8 Solvent effects  1.9 Searching for a chromophore  1.10 Definitions  1.11 Conjugated dienes  1.12 Polyenes  1.13 Polyeneynes and poly-ynes  1.14 Ketones and aldehydes; π-π* transitions  1.15 Ketones and aldehydes; π-π* transitions  1.16 α,β-Unsaturated acids, esters, nitriles and amides  1.17 The benzene ring  1.18 Substituted benzene rings  1.19 Polycyclic aromatic hydrocarbons  1.20 Heteroaromatic compounds  1.21 Quinones  1.22 Corroles, chlorins and porphyrins  1.23 Non-conjugated interacting chromophores  1.24 The effect ofsteric hindrance to coplanarity  1.25 Internet  1.26 BibliographyChapter 2: Infrared spectra  2.1 Introduction  2.2 Preparation of samples and examination in an infrared spectrometer  2.3 Examination in a Raman spectrometer  2.4 Selection rules  2.5 The infrared spectrum  2.6 The use of the tables of characteristic group frequencies  2.7 Absorption frequencies of single bonds to hydrogen 3600-2000 cm-1  ……Chapter 3: Nuclear magnetic resonance spectraChapter 4: Mass spectraChapter 5: Practice in structure determinationIndex

章節(jié)摘錄

插圖：The energy absorbed by the matrix is transferred indirectly to the sample, which reduces any sample decomposition. The matrix is chosen to have solubility properties similar to those of the sample, in order that the sample molecules are properly dispersed. Higher molecular weight oligomeric 'clumps' are produced as 2M+, 3M+, and so on, but these are usually minor components of the spectrum if a well-matched matrix is chosen.   4.3.3 Electrospray ionisation （ESl） An 'electrospray' is the term applied to the small flow of liquid （generally 1-10 lxl/min） from a capillary needle when a potential difference typically of 3-6 kV is applied between the end of the capillary and a cylindrical electrode located 0.3-2 cm away （Fig. 4.4）. The liquid leaves the capillary as a fine mist at or near atmospheric pressure, and consists of highly charged liquid droplets. The charge on these droplets may be selected as positive or negative according to the sign of the voltage applied to the capillary. ESI is especially useful since it can be used to analyse directly the effluent from an HPLC column.The use of a 'sheath' gas or 'nebulising' gas promotes efficient spraying of the solution of the sample from the capillary. Sample molecules dissolved in the spray are released from the droplets by evaporation of the solvent. This evaporation is accomplished by passing a drying gas across the spray before it enters a capillary. As the droplets are multiply charged, and reduced in size by evaporation, the rate of desolvation is increased because of repulsive Coulombic forces. These forces eventually overcome the cohesive forces of the droplet, and an MH~ （or M - H+） molecular ion free of solvent is finally produced. The charged particles are carried, by an appropriate electric field, through a capillary and into an ion analyser.

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