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7 analyticalchemistry-IR
Infrared spectroscopy (IR) Key words How to obtain the structure of the unknown compound? 1) An examination of IR spectra indicates the various X-H bonds present in the molecule and the presence or absence of triple or double bonds, carbonyl groups, aromatic rings, and other functional groups. 2) This information, together with other data such as elemental analysis, molecular weights, Raman, UV, mass and NMR spectra will suggest various possible structures. How to obtain the structure of the unknown compound? 3) The IR and Raman spectra can then be searched in detail for bands (峰) due to the various groups in the postulated structures. Comparison with published IR spectra of compounds having the suggested or a similar structure should be made. The computer attached to a modern FT-IR spectrometer often has a search routine (程序) and a library of infrared spectra, which may be searched for spectra that most closely match the spectrum of the unknown compound. Preparation of sample A preliminary IR spectrum of a solid is recorded using a hydrocarbon mull (Nujol) or a KBr pellet whereas that of a liquid is recorded as a film between two NaCl or KBr plates. When hydrogen bonding is evident from very broad bands, especially between 3500 and 2500 cm-1, spectra also should be obtained from dilute solutions in CCl4 or from some other suitable solvent. For a detailed study, several spectra may be needed from solutions of various concentrations, from mulls or pellets containing various relative amounts of sample, or from liquid films of various thicknesses. Analysis of the infrared spectra The characteristic absorption peaks arising from vibrations about a single bond generally fall in the region between 660cm-1 and 1600cm-1, those from a double bond in the 1600~2000 cm-1 region, and those from a triple bond in the 2000~2500 cm-1 region. However, the stretching frequencies of the bonds between hydrogen and oxygen, hydrogen and sulfur, and hydrogen and nitrogen are found in
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