Joseph Jack Kirkland: HPLC Particle Pioneer

May 01, 2014
Volume 32, Issue 5, pg 344-353

Joseph Jack Kirkland answered questions from Gert Desmet on his pioneering career in high performance liquid chromatography (HPLC).

Gert Desmet: How did you enter the field of chromatography?

Joseph Jack Kirkland: In the late 1950s I began to use gas chromatography (GC) to solve problems relating to agricultural products that were being developed at DuPont. This effort was triggered by interactions with DuPont's Dr. Steve Dal Nogare, who started the early studies in GC, especially in programmed temperature operation. GC analyses proved to be quite useful, but there were many compounds of interest to DuPont that were not volatile and could not be separated by this technique.

In some cases, I was able to derivatize these materials to produce structures that were sufficiently volatile for GC analysis, but many problems still remained that needed a solution. Around 1960, I attempted liquid chromatography (LC) separations of some nonvolatile compounds using large-particle silica gel columns as the separating medium, a low pressure pump, and a refractometer as a detector. Crude separations resulted, but it was too slow, poorly reproducible, and very frustrating. I really did not know enough to create the desired result. Therefore, this project was not pursued further. However, in 1964, when I was visiting Europe, during a trip to Eindhoven, The Netherlands, I came across Dr. Joseph (J.F.K.) Huber in a laboratory performing what we now call high performance liquid chromatography (HPLC).

Figure 1: Jack Kirkland in his laboratory in 1960.
Huber was using a constant-pressure pump (1000 psi), a small diameter column with ~50 µm diatomaceous earth particles, and an ultraviolet (UV) spectrometer that had been converted into a crude detector. With this arrangement, Huber was demonstrating remarkable (for that time) separations of nonvolatile compounds using a liquid–liquid chromatographic technique. This visit was so interesting that on my return to DuPont, I approached my supervisor and pleaded for the time and resources to begin a program into researching HPLC technology. This request was approved and I then started to develop the materials that were needed to make the technique routine. To improve the technology, I believed that a better column packing was required, together with a reliable and highly sensitive UV detector. Both of these items were subsequently developed, put into use, and a patent and papers on them published.

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