Meanwhile, I began modeling all the stages of the experiment to study the “breakthrough” effect, as Bogomazov had requested. From my previous experience, I knew only too well that technologists often underestimate the importance of choosing the right analytical method, and of using highly skilled personnel for tests. I decided to look into the analytical process control in much more detail.
At first glance, it looked like everything was being done well enough. Gas samples were taken from the adsorption tube outlet that modeled a gas-mask filter, with a special gas-tight syringe. Then, the samples were analyzed in a Tsvet-100 chromatograph with a flame-ionization detector. There was an instrument that recorded the chromatograms, and the results showed a number of so-called peaks corresponding to different compounds. The distance of the interval from the start point of the chromatogram to the peak is a characteristic parameter of each compound. So once you have measured this interval for each compound (in its pure form or mixed with an inert gas), it can be used for the identification of peaks in chromatograms of unknown mixtures, in order to determine the composition of the mixture.
This is the theory and it’s a good one, but in practice everything is much more complicated. Very often a sample contains some additional compounds, which can give the same or nearly identical peak intervals in the chromatogram. When a chromatographic analysis is being conducted using a nonselective flame-ionization detector, the probability of error is rather high, due to several overlapping chromatographic peaks of the organic compounds. It should be said that really experienced specialists almost never used these intervals, because the recorders couldn’t move the paper tape at a constant rate. Instead, real specialists used a stop-watch to time the emerging chromatographic peaks (measurement was taken at the maximum value), and they got much more precise and reliable measurements. Modern devices now take highly precise measurements automatically, with the help of computers.
Once I suggested to Aleksander Dmitriev that we use a stop-watch during the experiments. The first result showed chromatograms with registered peak times for various samples of soman. Then, for comparison, we took the same measurements on the same chromatogram using a mixture of inert nitrogen and the thionic analog of soman.
It turned out that the peak time of the compound emerging from the dynamic adsorption set, which Sasha believed to be the peak of the thionic analog, did not coincide with the peak of the same analog in nitrogen. The difference was very significant and it left no doubt that these peaks belonged to different organic molecules.
It quickly became clear to me that we were dealing with a fundamental error. However, my discovery didn’t make any impression on the MACD graduate, because he was coached to trust only his boss.
I didn’t know whether or not he reported our results to his scientific boss, but I was preparing to analyze the same samples in a Perkin Elmer GC with a flame photometric detector. Deep down inside, I was already sure that all those folks who had made this sensational discovery were in for a huge disappointment. Even though this could adversely affect my career and complicate my doctoral dissertation work, I was thrilled to realize that this terrible menace to people was not real.
On the outside, it seemed that nothing had happened. I continued preparing my experiments and began my own research in the comparative analysis of the kinetics of the adsorption of chemical agents on active carbon and other adsorbents used for concentrating admixtures and the necessary follow-up, along with further chromatographic analysis. Additionally, I was studying the kinetic performance of the catalytic adsorbents used in modern gas masks.
I worked practically alone (only rarely did Bogomazov give me a laboratory assistant for help), and I got tired of the long drawn-out experiments in which I had to take gas samples every 5 minutes and analyze them over a 3-4 hour period. However, some kind of inspiration was pushing me forward and I was getting a lot of satisfaction from my work. I obtained unique data that allowed me to understand what processes were taking place in the concentrating columns and to choose the right adsorbent for them.
The research on the kinetic performance of gas-mask filters also produced very interesting results. For the first time ever, we obtained adsorption fronts for chemical agents on the gas masks used by the Soviet Army.
During the course of that research, I developed a series of methods for concentrating small quantities of chemical agents in the air and in liquids. My developments were registered and I received patents for them.
By that time, I understood that I would not be able to defend my doctoral thesis as it was. I would have to revise and rewrite it. I knew that would be tremendous work, but I was not afraid of it. I began writing my thesis again – at home, in my apartment. For that purpose, I invented a special system of codes for all the chemical agents mentioned in the work. That way, the theoretical calculations, diagrams, and charts did not contain any secret information, and I did not violate confidentiality. I could write late at night and on my days off, without running to the institute’s First Department for special permits to work at GOSNIIOKhT in the evenings.
It was time for a more thorough examination of the results showing breakthrough for the thionic analogs of soman and sarin.
To the great regret of the authors of the discovery, and to my greatest joy, the analysis of the samples, carried out with the help of my chromatograph with a selective detector, showed no breakthrough effect for a 10 minute period after the air with the chemical agents began flowing through the filter. Repeating the tests always gave the same result.
By the middle of the summer of 1983, Bogomazov finally acknowledged his mistake, but he continued to play the role of a great inventor saying that it was possible there could have been some experimental error in my work. But there was no error.
You had to give Bogomazov credit for his initiative and enterprising abilities. He soon established good relationships with other research institutes that were working on the “Foliant program” and developing individual means of protection.
Along with Bogomazov, I visited the Elektrostal Technological Research Institute (ENITI) for the first time. It was the leading scientific institution that was developing gas masks and filters for military equipment and installations (command posts, air-raid shelters, and so forth).
ENITI’s director, Vladimir Smirnov impressed me favorably with his proficiency in very different areas of the adsorption processes, chromatography, and adsorption material production technology. All the research fellows at ENITI who I later worked with were very well informed. I’m very grateful to them for their help with my research. Although science in Russia is going through very tough times now, I am sure that ENITI will survive and continue doing science, because it makes peaceful products for people’s protection.
In 1985, I asked Smirnov to be one of my official opponents, at the defense of my doctoral thesis, and he agreed at once. He wrote a very favorable review, which played a great part in my successful defense.
Dubov and Bogomazov got out of their thorny situation, by putting a positive spin on the failure of the “breakthrough”. From what I know, they asked the UNKhV to relax the requirements for the initial concentration of chemical agents, and naturally their request was rejected. This made it look as though GOSNIIOKhT had developed a method for breaking through the gas mask filter, but they could not meet the requirements of the capricious military.