One observes that the early developments in chemistry depended upon the improvement of the balance. Major milestones in chemistry can be related directly to improvements in balance design, precision, and accuracy. In a similar manner, the past three decades have seen dramatic improvements in spectrometers. The development of these instruments has greatly improved our understanding of polymer structure and properties. We discuss our current research in multidimensional spectrometry, imaging, and mapping. How does one determine the structure of molecules? One approach is the infrared and Raman study of the polymer vibrations to understand the structure and interactions so successfully applied by our awardee, Professor Jack Koenig. Historically, in the 1950s, the Perkin-Elmer Corp. introduced an infrared microscope for a limited number of applications. This development stimulated the thought of seeking more information about the microstructure. Today, we have a number of two-dimensional detectors for infrared and Raman studies. However, the expense of this instrumentation tends to limit its utilization. In this article, a new inexpensive approach for mapping molecular structure in polymeric materials is discussed. This new approach includes the combination of interferometers and Hadamard transform techniques to perform multidimensional spectrometry and mapping.