Head - Cand. of Chemical Sciences Vera Dmitrievna Tikhova
phone +7 (383) 330-98-56
internal phone: 3-33
Microanalytical Laboratory is one of the few laboratories among existing today, which was organized in the early years of the Novosibirsk Institute of Organic Chemistry.
Nikolai Nikolayevich Vorozhtsov, the first Director of the Institute, was well aware that the work relating to the synthesis of organic compounds, and the allocation of natural substances, can not develop without the analytical data. Therefore, in 1959 two female employees of the Institute were entrusted with establishing methods for determining the carbon, hydrogen and nitrogen in organic matter. And in beginning of 1960 “the analytical laboratory” was established with that title until 1967.
Lyudmila Nikolayevna Diakur began to work at the Institute as the head of this laboratory and directed it until her retirement in 1974. With extensive experience in analytical chemistry, as well as having organizational skills, L.N.Diakur has done much to selecting laboratory personnel and to developing required methods of analysis. In the first years classical methods were established for the determination of carbon, hydrogen, nitrogen, halogens, sulfur, and some of the functional groups (alkoxy, acetyl, active hydrogen, etc). In 1967 automatic CHN-analyzer (Hewlett-Packard) and vapor phase osmometer (for determining molecular weight) were purchased for the laboratory. The appearance of CHN-analyzer stimulated studies on the effective oxide catalysts for determining the elements with this device.
In 1975 Valentina Pavlovna Fadeeva became the head of the laboratory. Intensive development of synthetic works in the Institute, particularly in the field of chemistry polyfluoroaromatic, heterocyclic compounds required the development of methods for analysing these compounds. So much time in the laboratory was devoted to developing methods for determining fluorine and other elements in polyfluoroaromatic substances. In the 70th years thermoanalytical method appeared in the lab.It should be noted that our Director Academician N.N.Vorozhtsov always been very attentive to our lab, watching our progress, and help, when necessary. We began to publish scientific papers, organized city seminar on the organic analysis in Novosibirsk. Our laboratory was well equipped and had a good methodological support, thus became known among analysts from the Urals to the Far East. Some analysts from Irkutsk, Tomsk, Krasnoyarsk, Barnaul, Novokuznetsk, Sverdlovsk and other cities come to our laboratory for training.
In 1980, the group of gas chromatography entered into the laboratory, with whom we had been working for almost 20 years. This group has developed the universal methods of analysing polyfluoroaromatic and substituted aromatic compounds, which are now used for routine analysis. In 80’s the laboratory began to analyse working area air, and in the early 90's - the wastewater of the Institute. The results of our research are reported on a variety of analytical conferences, we have been involved in organizing the conference "Analytica of Siberia and the Far East," printed papers in national and international journals. Laboratory carries out tests for many organizations, first and foremost, for the Institutes of SB RAS.Students of NSU and other universities, students of the Novosibirsk Mendeleev Chemical Engineering College do their theses and course works in the laboratory.
The laboratory had been accredited three times since 1995, now it prepares for the next accreditation, that confirms the competence of the laboratory in the field of analysising organic compounds. All developed laboratory techniques for elemental analysis are metrologically certified and entered in the Federal Register of Analytical Techniques. Now our equipment is considerably upgraded, we have new CHNO-and CHNS-analyzers, vapor phase osmometer, termoanalyzer, modern UV-VIS spectrophotometers.
Our laboratory still maintains its status and prestige among analysts. We would like to preserve this tradition. Our work is usually “behind the scenes”. We should always be in the "alert" to run smoothly and with good quality. Not everyone can safely handle such a monotonous and painstaking work, as we have. It requires concentration, attentiveness, neatness. These qualities, as well as a favorable atmosphere are the main secret of our successful work.
Determining the elemental composition of synthetic and natural compounds and materials of various composition and structure by organic elemental analysis and atomic emission spectroscopy; designing and upgrading the analytical procedures. Determining the molecular weight of organic compounds and osmolality of solutions by vapor phase osmometry. Analysis of waste water and workplace air to detect toxic elements and compounds.
- Determining the elemental composition of synthetic and natural compounds and materials of various composition and structure by organic elemental analysis and atomic emission spectroscopy; designing and upgrading the analytical procedures.
- Determining the molecular weight of organic compounds and osmolality of solutions by vapor phase osmometry.
- Analysis of waste water and workplace air to detect toxic elements and compounds.
The Laboratory carries out the determination of the following elements by using both instrumental and chemical methods: carbon, hydrogen, nitrogen, sulfur, phosphorus, halogens (chlorine, bromine, iodine, fluorine), selenium, oxygen.
The Laboratory has the following advanced equipment:
- automatic CHNS and CHNO elemental analyzers EURO EA;
- vapor phase osmometer KNAUER K-7000;
- thermal analyzer STA 409 PC Luxx NETZSCH;
- UV-VIS spectrophotometers Cary 50 and Cary 60 VARIAN;
- Set of balances with different weighing range and sensitivity METTLER and SARTORIUS;
- Conductometer ANION;
- Thermosystem METTLER for determination of melting point.
The main research results in recent years
- The universal oxide catalyst compositions was developed to provide a complete decomposition of various substances and the absorption of interfering elements when determining the carbon, hydrogen, nitrogen, sulfur in automatic analyzers, as well as in the classical method of determining the C and H.
- The method of determining fluorine was developed, including the oxidative degradation of the sample in an oxygen atmosphere, followed by spectrophotometry (for complex-alizarinkomplekson lanthanum fluoride) or potentiometry (with a fluoride-selective electrode), the presence of another halogens, sulfur, phosphorus, metals in analyzed substances does not interfere fluorine determination; the method allows to determine fluorine content when present in the sample to 80%.
- The technique of sulfur determination was developed using potentiometric titration with barium-selective electrode.
- The method of selenium determination in organoselenium materials, based on the combustion of a substance in a flask filled with oxygen, and then determining the resulting Se (IV) extraction-spectrophotometric reaction with aromatic diamines-new reagent 3,4,5,6-tetrafluoro-1 .2-diaminobenzene and the previously known 2.3-diaminonaftalin. The presence of halogens and sulfur in analyzed substances, does not interfere selenium determination.
- The fragment composition of different origin soil and peat humic acids was investigated using a computer system "IR EXPERT”.
- Proposed methods has been successfully applied for analyzing virtually any substance, including hard degradable substances, such as a fully fluorinated, not containing hydrogen, including graphite, sulfur, halogen-, phosphorus-containing aromatic, polycyclic, heterocyclic nitrogen, metallic (complex, intercalation, organometallic, etc.), carbon materials, such as coal, sapropel, bitumens and their products, polymers, industrial oils, petroleum, rocks, etc.
- The vapor phase osmometry is used to determine the molecular weight poorly volatile organic and natural substances.
- Thermoanalytical method is applied for determining the thermal characteristics of the material and the thermal decomposition reaction kinetics. The thermal stability of substituted naphthoquinones, some polyfluoroaromatic compounds, sterically hindered phenols - stabilizers of polymeric materials was investigated.
- The mechanisms of the thermal decomposition of some compounds were suggested. The new software "TERMOGRAF" was developed for the calculation of kinetic parameters of thermolysis.
We are constantly working to improve the methods of analyzing organic compounds and to increase the number of elements determined.
Our studies were supported by the integration project of the Siberian Branch of the Russian Academy of Sciences and held in conjunction with the Institute of Soil and Agrochemistry SB RAS and the Institute of Petroleum Chemistry SB RAS (Tomsk).
The employees of laboratory take part in national and international conferences. The laboratory is preparing for accreditation as part of the Testing Analytical Center IOC SB RAS. The Laboratory constantly analyzes various substances and objects for other organizations of SB RAS: International Tomography Center, Institute of Catalysis, Institute of Inorganic Chemistry, Institute of Soil and Agrochemistry, Institute of Kinetics and Combustion, Institute of Chemical Biology and Fundamental Medicine, etc.
List of priority investigations
- 5.4 "Chemical aspects of modern ecology and environmental management, including the scientific problems of recycling and safe storage of radioactive waste".
- Program V.39.2 «Development of physical and chemical principles of safety of human activities" Green Chemistry ".
- Project V.39.2.5«Development of the research methodology of low molecular weight organic compounds and materials, reactions and processes in living systems using a new highly informative spectroanalytical methods".
- 2013-2016 the laboratory will work on priority:
- V 46. "Physico-chemical basis of environmental management and environmental protection on the basis of the principles of" green chemistry "and high catalytic systems to create new resources and energy saving steel and chemical processes, including the deep processing of hydrocarbon mineral resources of different classes and industrial waste, as well as new technology for processing of spent nuclear fuel and radioactive waste".
- Program V.36.1. "Development of physical and chemical principles and methods of environmental protection and recycling of industrial waste on the basis of the principles of" green chemistry "and catalytic systems".
- Inter-laboratory research project - "Development of an integrative studies of organic matter and synthetic materials, natural and anthropogenic, reactions and processes in living systems and environmental samples".
- V.P.Fadeeva, I.M.Moryakina. The use of different oxidation catalysts for the automatic determination of carbon, hydrogen and nitrogen in organic compounds.Izv. Sib. Otd. Akad. Nauk SSSR, Ser.: Khim., 1981, V.6, N.14, p 113.
- V.P.Fadeeva, I.M.Moryakina. Spectrophotometric determination of fluorine in fluorine-organic substances. Moscow, 1989; dep. in VINITI № 2579-889.
- O.N.Nikulicheva, V.P.Fadeeva and V.A.Logvinenko. Estimation of Thermal Stability of Phenol Stabilizers by Means of Thermogravimetric Analysis. J. Therm. Anal., 44, 329 (1995); Full text
- O.N.Nikulicheva, V.P.Fadeeva and V.A.Logvinenko. Calculation of the kinetic parameters thermal decomposition of some phenol stabilizers on the basis of thermoanalytical data. J. Therm. Anal., 47, 1629 (1996); Full text
- V.D.Tikhova, M.M.Shakirov, V.P.Fadeeva, M.I.Dergacheva. Specific Features of Humic Acids from Various Soils as Studied by Thermal Analysis and 13C NMR. Russian Journal of Applied Chemistry, 1998, N.7, p.1173.
- V.D.Tikhova, M.M.Shakirov, V.P.Fadeeva, M.I.Dergacheva. 31P NMR Study of Soil Humic Acids. Russian Journal of Applied Chemistry, 2000, N.7, p.1206.
- O.N. Nikulicheva, V.P.Fadeeva, V.N.Piottukh-Peletsky , L.M.Pokrovsky, T.F.Bogdanova, N.V.Yudina. An IR and GC-MS Study of Substances Extracted from Peat. Russian Journal of Applied Chemistry, 2005, V.78, N.8, p.1388.
- V.P.Fadeeva, V.D.Tikhova, O.N.Nikulicheva. Elemental analysis of organic compounds with the use of automated CHNS analyzers. Journal of Analytical Chemistry, 2008, V.63, N.11, p.1197.
- V.P.Fadeeva, V.D.Tikhova, O.N. Nikulicheva, I.V.Oleynik, I.I.Oleynik.Composition determination of post-metallocene olefin polymerization catalysts. Journal of Structural Chemistry, 2010, V.51, Supplement 1, p.188.
- V.D.Tikhova; T.F.Bogdanova, V.P.Fadeeva , V.N.Piottukh-Peletsky. Study of Fragment Composition of Humic Acid of Different Origin Using IR-EXPERT Software. Journal of Analytical Chemistry, 2013, V.68, N.1, p.86.