My dissertation focuses on (i) the development of new analysis tools and methodologies for analyzing X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS) data, and (ii) the comprehensive characterization of materials (nanodiamonds) using a multi-instrument approach. Chapter 1 contains (i) a discussion of the two techniques I focused on most in my work: XPS and ToF-SIMS, (ii) a discussion of the common chemometrics techniques used to analyze data from these methods, and (iii) the advantages/rationale behind the multi-instrument characterization of materials. Chapter 2 describes various good practices for obtaining reasonable peak fits in XPS, which can also be applied to peak fitting data from different techniques. To address the issue of user subjectivity/bias in XPS peak fitting, I introduce two less biased mathematical functions for characterizing XPS narrow scans, namely the equivalent width (EW) and the autocorrelation width (AW). These functions are discussed in Chapters 3 and 4. In Chapter 5, I then introduce uniqueness plots as simple and straightforward graphical tools for assessing the quality of XPS peak fits and for determining whether fit parameters are correlated. This tool is extensively used in spectroscopic ellipsometry, and the mathematics behind it is known in XPS. However, to the best of my knowledge, this graphical tool has never been applied to XPS. ToF-SIMS data analysis is somewhat challenging due to the enormous amounts of data that are collected, and also the matrix effect in SIMS. This amount of information is significantly increased when depth profiles are performed on samples. Chapter 6 discusses a new chemometrics tool that I introduce for analysis of complex data sets, with emphasis on XPS and ToF-SIMS depth profiling data. The new approach is called the Information Content (IC) or entropy, which is adapted from Claude Shannon's work on Information Theory. Chapter 7 then contains a presentation of the comprehensive characterization of five nanodiamond samples used to manufacture particles for liquid chromatography. The advantages of a multi-instrument approach for material characterization and the lack of comprehensive material characterization in the literature are emphasized. To the best of my knowledge this is the most comprehensive characterization of nanodiamonds that has been reported in the literature. Chapter 8 presents conclusions of my work and future work. This thesis also contains six appendices. Appendix 1 contains an article from a scientific magazine that I wrote to highlight the importance and applications of the EW and AW to characterize XPS narrow scans. Appendices 2-5 are application notes I wrote on separations I performed on a nanodiamond based HPLC column. Finally, Appendix 6 describes the ToF-SIMS analysis of the tungsten species in the nanodiamond samples characterized in Chapter 7.