Expanded problems, including integrated problems involving all four spectroscopies, are provided. Additional descriptions of new fragmentation techniques are presented, including electron capture dissociation (ECD), electron transfer dissociation (ETD), and infrared multi-photon dissociation (IRMPD). New discussion of sample preparations is added, including gel separation approaches. A new section on proteomics applications is included. A new chapter on quantitation (Chapter 10), including isotopic-labeling strategies, has been added to this revision. A significantly revised section on nuclear magnetic resonance (NMR) now offers: Expanded treatment of chemical shift basics Coverage of solvent effects Expanded coverage of the influence of rate processes on NMR spectra, the nuclear Overhauser effect, and INEPT-related pulse sequences A new section on shaped pulses New material on the pulse sequences Heternonuclear Single Quantum Correlation (HSQC), Heteronuclear Multiple Bond Correlation (HMBC), and Parallel Acquisition Nuclear magnetic resonance All-in-one Combination of Experimental Applications (PANACEEA), which enable faster determination of structures Numerous new problems, always drawn directly from the literature Sections on infrared and on ultraviolet-visible spectroscopy have been condensed in this revision, while retaining all fundamental information and extensive tables.