Ron Majors, Part I: LCGC’s 2018 Lifetime Achievement in Chromatography Award Winner Discusses His Early Career

Ron Majors, the 2018 LCGC Lifetime Achievement in Chromatography award winner, has an outstanding reputation worldwide as a leader, teacher, and chromatography ambassador. Early in his career at Varian, Majors published his pioneering work on the successful packing of microparticulate (5-µm) high performance liquid chromatography (HPLC) columns and studies on the effect of particle size distribution. In fact, he was the first to efficiently pack and commercialize a 5-µm HPLC column. Later, Majors became well known as a columnist for LCGC and through his work teaching short courses worldwide. As a result, Majors is often one of the first names chromatographers come to know during their education, and he is quite famous in the chromatography community. Here, Majors discusses his humble beginnings, career highlights, and more.

Were you always interested in a scientific career?

In my early years, I was interested in art and languages. In all, I took five years of Latin but in junior high I started to drift toward science. I loved biology-dissecting the frog and all that. In my junior year of high school, I took a chemistry class and that was it. Basically, having a great teacher who inspires you when you show more-than-average interest is a great help. My teacher asked me to stay involved in chemistry my senior year. I was her lab tech, preparing solutions, helping the students in chemistry lab, and so on. It was downhill from there.

How did you get started working with chromatography?

In undergraduate school, I began doing early research in inorganic chemistry, on pseudohalogen synthesis. My analytical professor got me involved with spectroscopy. An outside hospital wanted ultraviolet (UV) spectra done for some research that they were doing, and I earned a bit of money running the spectrophotometer. I developed a keen interest in analytical chemistry after taking a quantitative analysis course. I went to work in a quality control (QC) lab doing pesticide formulation analysis while going to undergrad school, which gave me a good introduction into industrial work. However, I didn’t really get deeply involved with chromatography until I went to work with Professor L.B. “Buck” Rogers at Purdue in 1963. Around me were other graduate students doing work in gas chromatography (GC) and liquid chromatography (LC); my own research was involved in surface chemistry, which is closely related to chromatography. So, after that I was hooked on working in chromatography. My first job at the Celanese Research Company in Summit, New Jersey, involved managing a chromatography laboratory. This was in 1968 just before the new technique of HPLC evolved, and I immediately adopted this technique to various nonvolatile samples encountered in the central research lab.

How did you get involved with sample preparation? What did you like about it?

I was trained in analytical chemistry by a classical analytical chemist who instilled in us students the importance of sampling and sample theory. Collecting the wrong sample in the right way or collecting the right sample in the wrong way negatively affects the final analysis, no matter how sophisticated the analytical technique afterwards. Basically, if you don’t have a sampling plan, then how do you know if you are obtaining a representative sample? Think of a polluted landfill. If you collect a sample at one end of a field, how do you know that it represents the entire field? The same with water sampling. Just lowering a bucket into a lake and using that as your final sample doesn’t ensure that that portion of the lake represents the entire lake water. Often, the job of sample collection is given to the lowest skilled worker in the laboratory or plant. As an analytical chemist, how do you know that person has brought a representative primary sample to the laboratory? Even the secondary sample, carried out in the lab before analysis, must further represent the primary sample collected in the field. After that, the fun begins of getting the sample into a form to put into the analytical instrument for final analysis. That is when you get to play with these neat expensive instruments.

Who was the biggest influence on your career when you were just getting started?

In my career, there were four key people who influenced my decision to become a chemist, especially an analytical chemist. First was Mrs. Rogers, my junior year high school chemistry teacher at Roosevelt High in Fresno, California. She recognized my keen interest in chemistry and encouraged me to go to the next level. She made chemistry sound exciting in both the lecture room and in the laboratory. She kept me as a “lab tech” my senior year where I helped prepare solutions and other chemicals for the chem lab and helped (or tried) to instill a love of chemistry to the junior students. Second was Dr. George Kaufmann, an inorganic chemistry professor at Fresno State, who encouraged me to do “research” in my freshman year in his lab and urged me to give talks at regional American Chemical Society (ACS) student affiliate meetings. Those talks gave me the confidence to stand up in front of a group to deliver a scientific lecture. Third was Professor Ray Bremner, also of Fresno State. He was my quant professor and saw my interest in analytical chemistry, so he encouraged me to do research in this area and instilled in me the importance of sampling and sample preparation. Finally, fourth was Professor L.B. “Buck” Rogers, my Purdue University graduate supervisor, who taught me to “think outside the box” and how to do the critical experiments necessary to prove one’s hypothesis. He also instilled in me the importance of writing up my results-if you can’t put in writing what you have accomplished, he said, then nobody will ever know what you have done and contributed to the science.

Did you ever consider an academic career?

When I graduated from Fresno State, I was kept on as a summer instructor in freshman chemistry and organic chemistry. I had complete control over my classes. I worked very hard to teach the students and to be fair in grading their work. When the class was completed, I had put together my “curve,” and another professor came to me asking that I change my grades so that I matched his distribution. I refused and stood my ground, but it left a bad taste in my mouth for academics. My work in various industrial labs during undergrad and grad school further convinced me that my direction should be in that sector.

What has been the most challenging work you have undertaken? What has been the most rewarding?

Probably my biggest challenge was when I worked at Varian in the late 1970s in Walnut Creek, California, in the liquid chromatography instrument group. Varian had stuck with high-pressure syringe pumps in the 1970s, and these pumps lost their luster compared to reciprocating pumps, which are in widespread use today. I had just returned from an overseas assignment in Europe and was embarking on a management career in the GC/LC application lab in Palo Alto, California. Varian’s market share in LC had slipped and they were in a desperate situation to have a more competitive product. Management decided to get all the LC expertise together in one place as a “crash project” to develop a more competitive HPLC system. I was transferred to Walnut Creek along with several others. We were all put altogether (design, software, mechanical, and electrical engineers; research & development [R&D] and application chemists; manual writers; and finance-just about anybody needed on the project goal) to develop an innovative, cost-effective HPLC system in less than 24 months. Normally, such a major project would take double the time or even more.

The team sat in an open environment with partitions chest high where one could access another team member in a close cubicle-no four-walled offices. This type of environment was pretty new in the ’70s. However, it was easy to quickly get to another team member to discuss some innovation or an aspect of the requirements. We worked our tails off and were very focused; not only did we beat the 24-month goal but we came up with one of the first integrated LC systems that had a built-in keyboard and a microprocessor: the LC5000. All components were inside the same box, and the keyboard could control the pump, gradient, detector, oven, and autosampler. The only separate piece was a new high-powered data system that came a bit later. In the next 18 months, Varian’s LC market share tripled and they were back in the game again. This project taught me that it takes a motivated, closely knit, and directed team to accomplish a goal; none of us could have accomplished this “mission” by him- or herself.

What is an accomplishment that you’re proud of, but that often gets overshadowed by your better-known achievements?

What many folks don’t know is that I was the first chromatographer to successfully pack a stable and reproducible microparticulate HPLC column. And the first 5–10 µm commercial column, Micropak. I gave the entire detailed story in an earlier article (1) so I will give the short form here. This all happened in 1971 just at the beginning of HPLC. Earlier, superficially porous packings (SPPs, sometimes called pellicular or porous-layered beads) were the rage since they outperformed the older large porous particles (over 100 µm). However, these SPPs lacked the sample capacity of the silicas of yesteryear, but there weren’t any commercial microparticulate silicas in the small particle size range with a narrow distribution required to provide greater efficiencies. Fortunately, E. Merck in Darmstadt, Germany, had size-separated one of the finely divided thin-layer chromatography (TLC) silicas and sent some to Brinkmann, their U.S. distributor at the time. Somehow, Brinkmann gave my boss at Varian this sample. It sat around for months with my boss bugging me to try to pack it. I finally relented and, like others who had experimental small particle porous silicas, tried to dry-pack this 5–10 µm material, the regular packing technique for SPPs. I quickly found out that this wasn’t the way to pack these highly statically charged particles and looked around for an alternative. I did find a technique used for packing large-particle size-exclusion chromatography packings-the slurry technique. A slurry is prepared by soaking the silica in a solvent, which disrupts the static charges, and then forcing it into a column blank under higher pressure than the column would be operated at. I tried a number of common solvents without realizing the potential efficiency that these small particles should generate, most likely because they were settling in the column while the packing process was going on. I looked around further for an alternative solvent system and came upon a balanced-density approach. Here, using very viscous solvents, the silica particles could be packed without longitudinally separating during the packing process. The solvents were very dense, tetrabromoethane and tetrachloroethylene, and somewhat toxic. After finding the right blend, I was able to get a silica gel column that significantly outperformed the large-particle SPP and dry-packed columns. The rest is history, as many chromatographers and companies began developing small irregular and spherical sized particles using slurry packing to achieve high efficiency columns. The technique is still in general use today.

Are there any particular things you learned from your early jobs before you joined Agilent?

I already talked about the learnings from the “crash project” at Varian that taught me a lot about teamwork and being focused. Since I had already decided not to pursue an academic career, the first summer of graduate school, I decided to seek an industrial position and took on an assignment at the Monsanto Organic Chemicals Division in St. Louis. This laboratory was a state-of-the-art facility in terms of the latest equipment and a very professional staff of analytical chemists. Working with infrared and nuclear magnetic resonance (NMR) spectroscopists, polymer specialists (size exclusion), chromatographers, and scientists from other disciplines gave me a good perspective on what to expect after my PhD, which was a long way off!

My first job out of grad school in 1968 was with the Celanese Research Co., in Summit, New Jersey. This central research laboratory provided a wide variety of samples including carbon fiber, organic chemical, paper products, polymer fibers, and others. Being in a central analytical laboratory, I was given the job of managing a chromatography laboratory. Of course, GC was still the main chromatographic technique, but this new technique of HPLC was on the horizon. Fortunately, having very experienced GC technicians, I really didn’t have to spend much time on that technology so I built up LC expertise, built my own instrument (commercial ones weren’t quite available yet), and started solving problems that couldn’t be done by GC. It was a good foundation, and I published and gave oral presentations that caught the attention of Varian, who asked me to come for an interview. Thus, my next move was to return to my “home state” of California to begin a lifelong career in HPLC. The last job that I had before Hewlett-Packard (later Agilent) was being a general manager at EM Science in New Jersey. This job gave me vast management experience with direct sales of HPLC instrumentation, selling chromatography products through distributors. It was a short stint, then I was off to Agilent to start my new job in sample prep.

For more from Ron Majors, see part II of this interview in an upcoming edition of our newsletter “E-separation Solutions.”

Reference

• R.E. Majors, LCGC North Am. 33(s11), 10–27 (2015).