rus
Professor I.A.Platonov, head of the chemistry department of the Samara State Aerospace University named after academician S.P.Korolev, doctor of sciences in engineering, tells about creation of the first Russian micro-chromatograph and around
Professor Igor Artemyevich Platonov, doctor of sciences in engineering, had led the chemistry department of the Samara State Aerospace University (SSAU) named after academician S.P.Korolev in 2010. Since that time, staff of the department has achieved a lot. The analytical equipment park was essentially updated and expanded due to latest instruments enabled measurements at the up-to-date level; a new, promising specialist preparation direction “Nanoengineering” was established; two cross-university research and educational centers were created and successfully operate; a joint research laboratory for material corrosion, aging, and biodeterioration was organized in collaboration with All-Russian Institute for aviation materials (VIAM). The department is involved in research projects in the field of chemistry, materials science and analytical instrumentation together with other units and research institutions of the University. In 2015, members of the department had developed a unique micro-chromatograph, which is generally unparalleled in both Russia and abroad.
In order to know more about achievements of scientists and plans for the future, we addressed to professor Igor Artemyevich Platonov, doctor of sciences in engineering, head of the chemistry department of SSAU.
Igor Artemyevich, in Aerospace University you are head of the chemistry department, which is aimed to research studies in chromatography and analytical instrument engineering. What connects the chromatography and space?
Many things, beginning from the history. One may remember that the history of global aviation and space exploration had begun from the flight of Wright brothers in 1903, and in the same year Russian scientist Mikhail Semyonovich Tsvet had discovered the chromatographic method for separation of substances and thereby laid the foundation for all types of chromatography in the world. Today it is one of the main analytical tools being in wide use for separation of complicated mixtures and determination of their composition. It is indispensable requisite in any research laboratory dealt with physical, chemical, or biological studies, where chromatographic systems rightfully take their place alongside of other complex analytical equipment. Nowadays, chromatographic systems are widely used for both in-lab and field routine measurements, for example, product quality or ecosystem status control, rather than only in scientific researches. We have no doubt that chromatographs will enter in category of common household devices used, for example, to control the “home environment”. Research modules of aircrafts or spacecrafts are usually equipped with various types of portable gas chromatographs and gas analyzers to analyze gas composition of both terrestrial and extraterrestrial objects. For example, since 1982, both Russia and United States began to equip their spacecrafts with portable gas chromatographs, which for the first time had analyzed atmosphere composition on the planets Venus and Mars.
Thus, chromatography is one of the techniques that are used in space exploration. But in the case of our chemistry department of SSAU, this research direction is simply a logical continuation of our activities aimed on the development of new devices and materials for aerospace engineering. To understand this, let us make a little excursion into our history.
It was mentioned above that SSAU had grown from the Kuibyshev Aviation Institute (KAI) that was founded in the most stressful time of the Great Patriotic War, in the year 1942. In that time, Samara was considered as the second, reserve, capital, and several dozen enterprises and organizations of the aviation industry were evacuated here from Moscow, St. Petersburg, and, in particular, Voronezh, to start up the production of new, up-to-date aircrafts such as, for example, the legendary ground-attack plane IL-2. The task assigned to KAI in that time included not only training of required specialists, but also scientific support for design and development projects. Naturally, basic departments for this task were selected among those where not only mathematical and physical disciplines, but also chemistry was taught, because it was expected that just chemistry will create new aviation materials and improve the existing ones.
It should be noted that the studies at the chemistry department ever since its foundation have been an integral part of total research activity aimed to solution of the general problem facing the university, and were carried out in very close cooperation with other departments. Team of the department was responsible for development of new effective chemical and analytical technologies needed in aerospace industry. This policy has remained in force in spite of all rearrangements at the department as well as changes of heads and requirements to activity results.
In the initial period, when the department was headed by its founder B.V.Erofeyev, member of Academy of Sciences of Belorussian SSR and USSR State Prize laureate, all research efforts were focused on the development of a layered material, methyl methacrylate-based Plexiglas transparent armor, and some special types of aircraft glazing. Later, already after the war, during 45 years the department was headed by professor N.G.Chovnyk, worldwide recognized specialist in the field of solid electrodes polarography in the salt melts. During this period, focus of studies had shifted to development of unique high-temperature corrosion-resistant coatings, which are used in aircraft and rocket engineering until now.
Later, under leadership of professor G.D.Malchikov, a new research direction had started. He reorganized the laboratory of polarography research techniques founded by N.G.Chovnyk in such a way as to concentrate its studies on the task-oriented synthesis of functional noble-metal disperse systems including powders, thin or island films, amorphous coatings, etc. From here, it was naturally to change for research directions “Microscopic materials” and “Nanomaterials” being actual until today. Our department together with “Nanoengineering” and “Metallurgy and aircraft material science” departments teaches students and trains specialists in specialty “Nanotechnologies and nanomaterials” for more than three years now. The educational program for this specialty organically combines knowledges and skills from a number of disciplines such as diffraction microoptics and nanooptoelectronics, synthesis of nanomaterials, microsystem technology and nanoscale measurements, which are conducted using chromatography techniques among others.
At present, radical transformations take place in our University. Since 2013, SSAU participates in the Program for competitiveness enhancement, which is conducted among world leading higher-school centers, with the aim to reinforce position of the University as one of technical education leaders in Russia. In 2015, within the framework of the Program, SSAU had been integrated with Samara State University. Now breakthrough research directions include aircraft and rocket engineering, propulsion engineering, optoelectronics, and basic studies in the field of perspective technologies. Our chemistry department takes a full-value part in each of these directions, although research themes concerned with conceptually novel technological approaches in analytical instrument engineering and nanotechnologies still stay most inherent for it.
Igor Artemievich, tell us more about these promising technologies.
Within the simplest meaning, nanotechnologies assume the process monitoring and control at a level close to molecular, creation of materials and devices having dimensions within the nanoscale and performing measurements with nano-precision. To perform analyses, i.e., measurements at this level, the SSAU Chemistry Department is equipped quite enough. This allows to develop research areas related, in particular, to plasma-chemical etching, sputtering, magnetic-impulse processing, diffusion and semi-diffusion welding. The Department has several different spectrometers, spark and ICP, which allows measuring the content of almost all elements of the Mendeleev’s Periodic Table. We have force microscopes, nanohardness tester, HPLC and capillary electrophoresis systems, gas chromatography assemblies with mass spectrometry detectors. All these devices are used in full for the research activity performed both by the Chemistry Department itself and in cooperation with other departments of the University.
As an example, a series of studies may be mentioned concerning one advanced technology, the study of antioxidant properties and development of innovative food stuffs implemented in the REC. We are talking about extraction of biologically-active substances and ones with antioxidant activity from various medicinal plants using solvents in sub- and supercritical state. This approach has the advantage that chemical technologies are created, which comply with the “green chemistry” concepts involving rejection of organic solvents and environmentally dangerous substances in them.
Synthesis of new catalysts is another promising research area of the Department: for oxidation, complete and selective hydrogenation of unsaturated and aromatic hydrocarbons and other processes in petrochemical, organic and inorganic synthesis; for the purification of exhaust gases emitted by industrial facilities, power plants, internal combustion engines from hydrocarbons, nitrogen and carbon oxides; for the development of the low-temperature catalytic combustion plants and catalytic heat generators. However, it is not enough to improve production processes and technologies to protect the environment from chemical pollution. It is necessary to perform permanent environmental monitoring over large areas and to accumulate the collected data for the case study, quick response and prevention of emergencies.
Application of the system containing miniature analytical devices capable to carry out remote and permanent monitoring and to transmit the obtained results is an effective solution for this problem. A similar device was engineered at our Department; it is a microfluid gas chromatograph. We have dedicated this project to Professor M.S.Vigdergauz, who is the founder of the chromatography scientific school in Samara and headed the Department of General Chemistry and Chromatography at Samara State University.
What is this miniature microfluid chromatograph?
This is a hand-held remote-controlled gas chromatograph in compact 220 × 145 × 55 mm housing and a weight of 1.2 kg. All major device units: a detector, an injector, chromatographic columns – are made as separate microfluid devices. The instrument is equipped with an electronic control system and the wireless data link (Wi-Fi or Bluetooth) adapter to connect to an external computer. There is no any similar device in Russia or abroad.
The central component of the instrument comprises a flat plate with a branched channel system having complex microrelief – actually, substances are fractioned in it and transported through capillaries in the eluent laminar flow. The unique mono- and poly-channel configuration is formed in a plane in our chromatographs per each kind of substances. Micro-channels may be formed on glass, aluminum plates, silicon substrates, etc. A wide range of technologies is used per each type of materials: 3D printing, mechanical milling, electrospark treatment, plasma-chemical and chemical etching, ablation by laser. Such microcapillary column has a high separating capacity depending on the channel size, shape and structure. These parameters are calculated mathematically and selected in such a way that the micro-chromatographic system is comparable by the number of theoretical plates with the one having usual dimensions.
Nanodispersed sorbents are used as a stationary phase including silica, new polymeric sorbents, thermally-graphitized carbon black. It is obvious that it is quite difficult to fill micro-capillary columns with them – creation of such techniques is also the research area of the Chemistry Department.
All components of a micro-fluidic chromatograph − injection, sample preparation, concentration and detection systems − also have miniature dimensions. All together, this allows us to make an assay in record time – from several minutes to seconds. Thus, for example, the duration of the test when separating a mixture of С1–С5 hydrocarbons including isomers is at most 12 seconds that is by 30 times less than for the chromatographic systems usually applied for this purpose.
A few particular words about detectors. They should have the sensitivity allowing to measure small concentrations of substances at their extremely small dimensions. We have developed two types of such devices, each of which takes about 1 mm2 on the surface of a silicon plate. The first-type detector is a micro-catharometer capable to detect nanograms of the analyte content that is almost an order of magnitude lower than its large counterpars. The second type is a thermo-catalytic device, which detection limit is comparable to the capabilities of a flame ionization detector, one of the most sensitive.
The specific feature of our device is that it can be fabricated in various configurations, for specific analytical task. In general, this approach is feasible. As it is shown by practice, multi-task chromatographs are used in most cases for just one analytical technique. Indeed, re-configuration of a chromatograph, selection of separation conditions is a task for research laboratories while the manufacturing process requires continuous assay. Therefore, each our miniature device has only one, maximum two operating algorithm that provides the ultimate application ease. You can control them wirelessly from any computer, even from a smartphone.
I would like to stress that creation of our first microfluid chromatograph was preceded by huge work, which included 30 years of preliminary studies carried out at different universities and research institutes of Moscow, St. Petersburg, Novosibirsk and Samara. Creation of a microfluid gas chromatograph became possible owing to the integration of achievements in chromatography, microelectronics and nano-engineering as well as association of scientific potential of fifteen departments at SSAU.
Do you plan the arrangement of industrial production of micro-fluid chromatograph?
We are approaching to this objective. Our projects are brought to their logical conclusion and allow manufacturing of gas micro-chromatographs, which are much smaller than their conventional laboratory counterparts. There is a need in such devices. After all, they are intended mainly for continuous, routine measurements. And owing to small dimensions, they allow for make assays even in the field. We cooperate with almost all industries that use GC including geological exploration, petrochemical manufacturing, pharmaceutical, forensics and medicine.
In what direction do you expect to develop the study in future?
Now we are working on a multimodal system, which solves the problems of comprehensive and the most demanded analytical techniques. Such a multi-module microfluid system can replace an entire chromatographic room with all its wiring and utilities. And such analytical unit may become a competitor to the usual universal chromatograph in terms of routine analytical measurements made in a very short, up to three minutes, intervals.
If we talk about the more specific tasks of microfluid chromatography, then, of course, we will move toward increasing the test speed − from express methods to hyper-fast that allows measurements within seconds and even faster. This will require development of mathematical models describing the complex channel geometry, the plate sealing technology. Basically, yet now there is an issue as per creating quite micro-devices, which may be applied not only in chemical and chromatographic laboratories but also for completely practical purposes. For example, as a complement to mobile phones with an appropriate software that allows you to maintain a continuous analysis and monitoring of the environment − at home, in offices, in the working area, to control industrial emissions and atmospheric conditions on basic crossroads. We are open to new ideas and actively cooperate with international groups, Russian and foreign partners. We have a lot of ideas and energy.
Thank you very much for your interesting story.
Interviewed by K.Gordeev,
O.Shakhnovich
Professor Igor Artemyevich Platonov, doctor of sciences in engineering, had led the chemistry department of the Samara State Aerospace University (SSAU) named after academician S.P.Korolev in 2010. Since that time, staff of the department has achieved a lot. The analytical equipment park was essentially updated and expanded due to latest instruments enabled measurements at the up-to-date level; a new, promising specialist preparation direction “Nanoengineering” was established; two cross-university research and educational centers were created and successfully operate; a joint research laboratory for material corrosion, aging, and biodeterioration was organized in collaboration with All-Russian Institute for aviation materials (VIAM). The department is involved in research projects in the field of chemistry, materials science and analytical instrumentation together with other units and research institutions of the University. In 2015, members of the department had developed a unique micro-chromatograph, which is generally unparalleled in both Russia and abroad.
In order to know more about achievements of scientists and plans for the future, we addressed to professor Igor Artemyevich Platonov, doctor of sciences in engineering, head of the chemistry department of SSAU.
Igor Artemyevich, in Aerospace University you are head of the chemistry department, which is aimed to research studies in chromatography and analytical instrument engineering. What connects the chromatography and space?
Many things, beginning from the history. One may remember that the history of global aviation and space exploration had begun from the flight of Wright brothers in 1903, and in the same year Russian scientist Mikhail Semyonovich Tsvet had discovered the chromatographic method for separation of substances and thereby laid the foundation for all types of chromatography in the world. Today it is one of the main analytical tools being in wide use for separation of complicated mixtures and determination of their composition. It is indispensable requisite in any research laboratory dealt with physical, chemical, or biological studies, where chromatographic systems rightfully take their place alongside of other complex analytical equipment. Nowadays, chromatographic systems are widely used for both in-lab and field routine measurements, for example, product quality or ecosystem status control, rather than only in scientific researches. We have no doubt that chromatographs will enter in category of common household devices used, for example, to control the “home environment”. Research modules of aircrafts or spacecrafts are usually equipped with various types of portable gas chromatographs and gas analyzers to analyze gas composition of both terrestrial and extraterrestrial objects. For example, since 1982, both Russia and United States began to equip their spacecrafts with portable gas chromatographs, which for the first time had analyzed atmosphere composition on the planets Venus and Mars.
Thus, chromatography is one of the techniques that are used in space exploration. But in the case of our chemistry department of SSAU, this research direction is simply a logical continuation of our activities aimed on the development of new devices and materials for aerospace engineering. To understand this, let us make a little excursion into our history.
It was mentioned above that SSAU had grown from the Kuibyshev Aviation Institute (KAI) that was founded in the most stressful time of the Great Patriotic War, in the year 1942. In that time, Samara was considered as the second, reserve, capital, and several dozen enterprises and organizations of the aviation industry were evacuated here from Moscow, St. Petersburg, and, in particular, Voronezh, to start up the production of new, up-to-date aircrafts such as, for example, the legendary ground-attack plane IL-2. The task assigned to KAI in that time included not only training of required specialists, but also scientific support for design and development projects. Naturally, basic departments for this task were selected among those where not only mathematical and physical disciplines, but also chemistry was taught, because it was expected that just chemistry will create new aviation materials and improve the existing ones.
It should be noted that the studies at the chemistry department ever since its foundation have been an integral part of total research activity aimed to solution of the general problem facing the university, and were carried out in very close cooperation with other departments. Team of the department was responsible for development of new effective chemical and analytical technologies needed in aerospace industry. This policy has remained in force in spite of all rearrangements at the department as well as changes of heads and requirements to activity results.
In the initial period, when the department was headed by its founder B.V.Erofeyev, member of Academy of Sciences of Belorussian SSR and USSR State Prize laureate, all research efforts were focused on the development of a layered material, methyl methacrylate-based Plexiglas transparent armor, and some special types of aircraft glazing. Later, already after the war, during 45 years the department was headed by professor N.G.Chovnyk, worldwide recognized specialist in the field of solid electrodes polarography in the salt melts. During this period, focus of studies had shifted to development of unique high-temperature corrosion-resistant coatings, which are used in aircraft and rocket engineering until now.
Later, under leadership of professor G.D.Malchikov, a new research direction had started. He reorganized the laboratory of polarography research techniques founded by N.G.Chovnyk in such a way as to concentrate its studies on the task-oriented synthesis of functional noble-metal disperse systems including powders, thin or island films, amorphous coatings, etc. From here, it was naturally to change for research directions “Microscopic materials” and “Nanomaterials” being actual until today. Our department together with “Nanoengineering” and “Metallurgy and aircraft material science” departments teaches students and trains specialists in specialty “Nanotechnologies and nanomaterials” for more than three years now. The educational program for this specialty organically combines knowledges and skills from a number of disciplines such as diffraction microoptics and nanooptoelectronics, synthesis of nanomaterials, microsystem technology and nanoscale measurements, which are conducted using chromatography techniques among others.
At present, radical transformations take place in our University. Since 2013, SSAU participates in the Program for competitiveness enhancement, which is conducted among world leading higher-school centers, with the aim to reinforce position of the University as one of technical education leaders in Russia. In 2015, within the framework of the Program, SSAU had been integrated with Samara State University. Now breakthrough research directions include aircraft and rocket engineering, propulsion engineering, optoelectronics, and basic studies in the field of perspective technologies. Our chemistry department takes a full-value part in each of these directions, although research themes concerned with conceptually novel technological approaches in analytical instrument engineering and nanotechnologies still stay most inherent for it.
Igor Artemievich, tell us more about these promising technologies.
Within the simplest meaning, nanotechnologies assume the process monitoring and control at a level close to molecular, creation of materials and devices having dimensions within the nanoscale and performing measurements with nano-precision. To perform analyses, i.e., measurements at this level, the SSAU Chemistry Department is equipped quite enough. This allows to develop research areas related, in particular, to plasma-chemical etching, sputtering, magnetic-impulse processing, diffusion and semi-diffusion welding. The Department has several different spectrometers, spark and ICP, which allows measuring the content of almost all elements of the Mendeleev’s Periodic Table. We have force microscopes, nanohardness tester, HPLC and capillary electrophoresis systems, gas chromatography assemblies with mass spectrometry detectors. All these devices are used in full for the research activity performed both by the Chemistry Department itself and in cooperation with other departments of the University.
As an example, a series of studies may be mentioned concerning one advanced technology, the study of antioxidant properties and development of innovative food stuffs implemented in the REC. We are talking about extraction of biologically-active substances and ones with antioxidant activity from various medicinal plants using solvents in sub- and supercritical state. This approach has the advantage that chemical technologies are created, which comply with the “green chemistry” concepts involving rejection of organic solvents and environmentally dangerous substances in them.
Synthesis of new catalysts is another promising research area of the Department: for oxidation, complete and selective hydrogenation of unsaturated and aromatic hydrocarbons and other processes in petrochemical, organic and inorganic synthesis; for the purification of exhaust gases emitted by industrial facilities, power plants, internal combustion engines from hydrocarbons, nitrogen and carbon oxides; for the development of the low-temperature catalytic combustion plants and catalytic heat generators. However, it is not enough to improve production processes and technologies to protect the environment from chemical pollution. It is necessary to perform permanent environmental monitoring over large areas and to accumulate the collected data for the case study, quick response and prevention of emergencies.
Application of the system containing miniature analytical devices capable to carry out remote and permanent monitoring and to transmit the obtained results is an effective solution for this problem. A similar device was engineered at our Department; it is a microfluid gas chromatograph. We have dedicated this project to Professor M.S.Vigdergauz, who is the founder of the chromatography scientific school in Samara and headed the Department of General Chemistry and Chromatography at Samara State University.
What is this miniature microfluid chromatograph?
This is a hand-held remote-controlled gas chromatograph in compact 220 × 145 × 55 mm housing and a weight of 1.2 kg. All major device units: a detector, an injector, chromatographic columns – are made as separate microfluid devices. The instrument is equipped with an electronic control system and the wireless data link (Wi-Fi or Bluetooth) adapter to connect to an external computer. There is no any similar device in Russia or abroad.
The central component of the instrument comprises a flat plate with a branched channel system having complex microrelief – actually, substances are fractioned in it and transported through capillaries in the eluent laminar flow. The unique mono- and poly-channel configuration is formed in a plane in our chromatographs per each kind of substances. Micro-channels may be formed on glass, aluminum plates, silicon substrates, etc. A wide range of technologies is used per each type of materials: 3D printing, mechanical milling, electrospark treatment, plasma-chemical and chemical etching, ablation by laser. Such microcapillary column has a high separating capacity depending on the channel size, shape and structure. These parameters are calculated mathematically and selected in such a way that the micro-chromatographic system is comparable by the number of theoretical plates with the one having usual dimensions.
Nanodispersed sorbents are used as a stationary phase including silica, new polymeric sorbents, thermally-graphitized carbon black. It is obvious that it is quite difficult to fill micro-capillary columns with them – creation of such techniques is also the research area of the Chemistry Department.
All components of a micro-fluidic chromatograph − injection, sample preparation, concentration and detection systems − also have miniature dimensions. All together, this allows us to make an assay in record time – from several minutes to seconds. Thus, for example, the duration of the test when separating a mixture of С1–С5 hydrocarbons including isomers is at most 12 seconds that is by 30 times less than for the chromatographic systems usually applied for this purpose.
A few particular words about detectors. They should have the sensitivity allowing to measure small concentrations of substances at their extremely small dimensions. We have developed two types of such devices, each of which takes about 1 mm2 on the surface of a silicon plate. The first-type detector is a micro-catharometer capable to detect nanograms of the analyte content that is almost an order of magnitude lower than its large counterpars. The second type is a thermo-catalytic device, which detection limit is comparable to the capabilities of a flame ionization detector, one of the most sensitive.
The specific feature of our device is that it can be fabricated in various configurations, for specific analytical task. In general, this approach is feasible. As it is shown by practice, multi-task chromatographs are used in most cases for just one analytical technique. Indeed, re-configuration of a chromatograph, selection of separation conditions is a task for research laboratories while the manufacturing process requires continuous assay. Therefore, each our miniature device has only one, maximum two operating algorithm that provides the ultimate application ease. You can control them wirelessly from any computer, even from a smartphone.
I would like to stress that creation of our first microfluid chromatograph was preceded by huge work, which included 30 years of preliminary studies carried out at different universities and research institutes of Moscow, St. Petersburg, Novosibirsk and Samara. Creation of a microfluid gas chromatograph became possible owing to the integration of achievements in chromatography, microelectronics and nano-engineering as well as association of scientific potential of fifteen departments at SSAU.
Do you plan the arrangement of industrial production of micro-fluid chromatograph?
We are approaching to this objective. Our projects are brought to their logical conclusion and allow manufacturing of gas micro-chromatographs, which are much smaller than their conventional laboratory counterparts. There is a need in such devices. After all, they are intended mainly for continuous, routine measurements. And owing to small dimensions, they allow for make assays even in the field. We cooperate with almost all industries that use GC including geological exploration, petrochemical manufacturing, pharmaceutical, forensics and medicine.
In what direction do you expect to develop the study in future?
Now we are working on a multimodal system, which solves the problems of comprehensive and the most demanded analytical techniques. Such a multi-module microfluid system can replace an entire chromatographic room with all its wiring and utilities. And such analytical unit may become a competitor to the usual universal chromatograph in terms of routine analytical measurements made in a very short, up to three minutes, intervals.
If we talk about the more specific tasks of microfluid chromatography, then, of course, we will move toward increasing the test speed − from express methods to hyper-fast that allows measurements within seconds and even faster. This will require development of mathematical models describing the complex channel geometry, the plate sealing technology. Basically, yet now there is an issue as per creating quite micro-devices, which may be applied not only in chemical and chromatographic laboratories but also for completely practical purposes. For example, as a complement to mobile phones with an appropriate software that allows you to maintain a continuous analysis and monitoring of the environment − at home, in offices, in the working area, to control industrial emissions and atmospheric conditions on basic crossroads. We are open to new ideas and actively cooperate with international groups, Russian and foreign partners. We have a lot of ideas and energy.
Thank you very much for your interesting story.
Interviewed by K.Gordeev,
O.Shakhnovich
Readers feedback
