Reddit reviews Principles of Instrumental Analysis

For pleasure:

• The Disappearing Spoon
  
• Periodic Tales
  
• Stuff Matters
  
• Molecules of Murder
  
• The Elements of Murder
  
• The Elements
  
• Molecules
  
• Molecules that Changed the World
  
• The Chemistry Book
  
  Undergraduate
  
  
• Organic:
  Organic Chemistry as a Second Language, The art of writing reasonable organic reaction mechanisms
  
  
• Inorganic: Inorganic Chemistry, Molecular Symmetry and Group Theory
  
  
• Analytical: Principles of Instrumental Anlsysis, Fundamentals of Analytical Chemistry
  
  Graduate
  
  
• Organic: Advanced Practical Organic Chemistry, March's Advanced Organic Chemistry, Greene's Protective Groups in Organic Synthesis, Purification of Laboratory Chemicals, Strategic Applications of Named Reactions in Organic Synthesis
  
• Inorganic: Advanced Inorganic Chemistry

First of all, I loved Harris's book.

Secondly, take a look at Skoog, Holler and Crouch's Principles of Instrumental Analysis.

Tip: It's not worth buying at its current price ($258). It should be available in good condition in your department's library.

I'd pick up an instrumental analysis textbook. If you're at a university, their library may have one in circulation, saving you a few bucks. I've used Skoog's text.

That said, I'll give a few pointers to get you started. Of course, a little context on the details of the separation you're trying to accomplish would focus this discussion some. Maybe this is just a classroom exercise. That is, maybe you're not actually trying to perform a separation in the lab. Regardless, I'd follow TurkFebruary's advice and google it. Wikipedia has some good info, too.

• Column/stationary phase type. Depending on the nature of the analytes you're separating, the choice of column packing material is an important one. It seems that reverse-phase is becoming the standard, as it takes advantage of relatively polar mobile phases, in which case water is one of your components. Anyway, you can get polar (normal phase) and nonpolar (reverse phase) columns. Further, if your analytes can be easily separated by size, you may choose a size exclusion column. Also, ion exchange columns are particularly useful for separating charged species or species with charged moieties.
  
  
• Column size. HPLC columns generally fit into 2 categories depending on the scale of the separation to be performed: analytical and prep scales. Analytical columns are shorter, narrower, and as such, contain a smaller volume of stationary phase. Analytical columns provide higher resolution, but have low sample loading capacities (micrograms or even nanograms of solute). Preparative columns are used for larger-scale separations, are greater in length and diameter, and are may effect up to gram-scale separations. The terms are not mutually exclusive, and there are grades between, sometimes called semi-prep.
  
  
• Mobile phase composition. Generally, whether employing normal or reverse phase, some time must be spent developing a method with regard to mobile phase composition. In either of these 2 phases, you're taking advantage of differences in affinity of solutes to both your stationary and mobile phase. If your mobile phase is too strong, all solutes will elute simultaneously, effecting no separation. If you mobile phase is too weak, you'll get effective separation, but will waste time. In some cases, gradient elution is used, which takes advantage of a a proportioning valve and a time program, and begins a separation with a relatively weak mobile phase, and gradually alters the composition to provide improved resolution of early eluting components, and speed up elution of late eluting components.
  
  
• Analytical wavelength. Most HPLC systems use a UV-Vis absorbance detector. Obviously, you need to select a wavelength at which your analytes absorb. This can usually be determined by gathering a UV-Vis spectrum of standard samples of your analytes before beginning any chromatography. Of course, if you're using a photodiode array detector, you can gather a full spectrum of analytes as they elute from the column, generating much richer data. I should note that other detection methods exist, like fluorescence detection. In some configurations, HPLC eluent feeds directly into a mass spec, which is a powerful method for separation and identification.
  
  
• Flow rate. Generally, this will be determined by your column choice, as columns typically have suggested maximum flow rates. Larger columns can typically handle faster flow rates. The concern here is pressure. Faster flow rates require larger system pressures. High system pressures may overtax the mobile phase pump and lead to shorter pump life. In addition, theoretical plate height, and therefore resolution, depends on flow rate. The Van Deemter equation and plot can be used to determine the optimum flow rate for a given column.
  
  This is what comes to mind off the top of my head.

Sorry Skoog A chem book. http://www.amazon.com/gp/aw/d/0495012017?pc_redir=1412086803&robot_redir=1

The example of a $400 textbook is not at all extreme. Consider Principals of instrument analysis, which is $381 new, $120 used, and the previous edition can be found for $9.

This is intended for junior and senior level chemistry students, and covers concepts that have been largely unchanged for the past few decades.

I loved Principles of Instrumental Analysis by Skoog et al.