Many mixtures important to research consist of hundreds or even thousands of individual components of interest. These types of mixtures are far too complex to separate by a single chromatographic dimension in any reasonable amount of time. However, if a multidimensional approach is used, where a complex mixture is separated by an initial dimension, simpler fractions of that separation are collected and each of those fractions are analyzed individually, highly complex mixtures can be resolved in relatively short amounts of time. This dissertation serves as a guide to multidimensional chromatography, in particular, two-dimension liquid chromatography. There are many aspects of multidimensional separations that have been investigated to show its aspects, drawbacks and potential ability to separate highly complex mixtures. Measurements for the performance of multidimensional chromatography, the effects of the first and subsequent dimensions and the approaches to pairing dimensions are shown with experimental examples. Fundamental and practical features of multidimensional chromatography are explained as well as theoretical discussions on current and future multidimensional chromatography performance. Experimentally, very high peak capacities were obtained (ca. 7000) and an algorithm to predict how to best optimize a two-dimensional separation based on the time used and performance was created for designing experiments
