The research laboratories of scientific and industrial enterprises both in our country and abroad at all stages of industrial development faced all the new problems of materials science: determination of the chemical composition, basic characteristics, structural states, physical and mechanical properties of materials which entailed the necessity of laboratory, bench and field tests. Proceeding from the results obtained, decisions are made on the prospects of the design, development and improvement of traditional structural materials and technologies, as well as on their use in various civil and defense industries. Starting from 1932 the results of these studies are systematically highlighted in the publications of the journal « Industrial Laboratory. Diagnostics of materials» throughout the 90-year history of the journal. An emphasis is made on the key problems of formation of the chemical composition and structure, complex tests and certification of new materials and technologies with the subsequent use of the results in pilot and serial industrial production. Promising scientific directions and results of the implementation of the most important national and international concepts, strategies and programs aimed at ensuring the improved safety and security of man, nature and the technosphere are considered. Still much attention will be paid in the future to the results of complex mathematical, analytical, and digital studies, methodology of physicochemical and mechanical tests, the use of multiparameter methods and diagnostic tools for analysis of materials, substances, and living organisms at nano-micro-meso-macro levels, as well as to the mathematical and physical modeling of both dangerous and effective protective processes in engineering, sociology and management.

A method for the determination of polyorganosiloxanes (by silicon) in water using high-resolution electrothermal atomic absorption spectrometry with a continuous spectrum source and preliminary extraction of polyorganosiloxanes by benzene from the analyzed sample is proposed. The quantitative determination of polyorganosiloxanes (by silicon) was carried out on a contrAA^® 700 atomic absorption spectrometer in a cross-heating furnace. Natural water was used to optimize the parameters of the temperature – time program of the atomizer. To eliminate chemical interference during silicon determination by proposed method, graphite cuvettes were modified with a permanent modifier to form a carbide coating. A solution of sodium tungstate was used as a permanent modifier. Thermal stabilization of silicon in a graphite furnace was achieved in the presence of a mixed palladium-magnesium modifier in the nitrate form. The accuracy of the results was confirmed by spike test. The developed method of analysis was used to determine the content of polyorganosiloxanes (by silicon) in natural water. The metrological characteristics of the method were assessed in the range of determined silicon contents 0.01 – 100 mg/dm³.

We have optimized the method for simultaneous extraction of ethyl methylphosphonic acid ester (EMPA), isopropyl methylphosphonic acid ester (IPMPA), isobutyl methylphosphonic acid ester (IBMPA), pinacolyl methylphosphonic acid ester (PMPA), and methylphosphonic acid (MPA) from soil with their further determination by high performance liquid chromatography — high-resolution tandem mass spectrometry (HPLC — HRMS/MS). The analytes are highly-polar products of nerve agent hydrolysis. The observed ions in the fragmentation mass spectra of deprotonated molecules of EMPA, IPMPA, IBMPA, PMPA, MPA, and their corresponding deuterated molecules, as well as possible structural formulas of fragment ions are presented. Liquid extraction with deionized water followed by concentration by evaporation is used to prepare soil samples for analysis. Separation of the components was carried out using reverse-phase chromatography. The time required for sample preparation and analysis of soil samples does not exceed 1 hour. The detection limits in soil were 0.05 ng/g for EMPA and IPMPA, 0.02 ng/g for IBMPA and PMPA, and 1 ng/g for MPA.

The possibility of using the short-lived radioisotope ¹⁸⁸Re (16.9 h) in the radioactive-tracer technique for estimation of the losses occurred during sample preparation and for analysis of the solutions with a low rhenium content is shown. The radioisotope was obtained in an ¹⁸⁸Re generator, which is a glass column filled with aluminum oxide with a pre-adsorbed parent isotope ¹⁸⁸W (69.4 days) that forms ¹⁸⁸Re during β-decay. The latter in the form of a perrhenate ion was selectively washed into an aqueous solution, which was used to obtain a labeled solution. The values of rhenium losses and their distribution over the stages of sample preparation of carbon-containing raw materials (e.g., high-viscosity oil) including sintering, leaching, filtration and evaporation are estimated. It is shown that the greatest amount of rhenium is lost at the stage of sintering. However, the use of MgO + KMnO₄ mixture minimize the losses occurred at this stage and, hence, the total losses of rhenium. A rapid procedure of rhenium determination using the method of radiometric correction with substoichiometric separation is described. The method is based on the quantitative extraction of a stable complex of tetraphenylphosphonium cation (TPhPh) with the perrhenate ion by dichloroethane. The extraction constant of (C₆H₅)₄PReO₄ complex is (3.03 ± 0.75) × 10⁶. The extraction of the perrhenate ion not complexing with TPhPh does not exceed 1 – 2 %. The developed method provides rhenium determination in the sample at a level of 1 – 100 μg. A 10-fold excess of Zn²⁺ and Ni²⁺ present in a chloride-containing medium affects the determination of rhenium. The anions , , and have the most pronounced interfering effect whereas , , and Cl^– do not interfere with the determination.

Large-sized complex-shaped silicon carbide products can be obtained via liquid silicon infiltration, however, the presence of free silicon in their composition limits the scope of their application. The silicon content can be reduced by forming a fine-grained porous structure of the material and control of the growth rate of the carbide layer on the pore walls during liquid-phase silicification. We present the results of studying the effect of the impurity composition of silicon grade KR00 on the appearance of defects in the structure of fine-grained reaction-bonded silicon infiltrated silicon carbide (The results obtained can be used in the production of tribotechnical parts, valves, etc. on the basis of RGCC.). It is shown that iron contained in industrial silicon KR00 exerted the greatest effect. At a content of Fe below 0.94 %wt., SiSiC samples are almost defect-free with the density not less than 3.00 ± 0.05 g/cm^3. At a Fe content of 1.49 %wt., defects in SiSiC samples are observed in the form of under-impregnated regions, which are probably attributed to the increased solubility of carbon in the silicon melt upon impregnation with technical silicon with an increased iron content and, as a consequence, more intensive growth of the silicon carbide layer on the pore walls with their subsequent overlapping. As the melt moves deeper into the carbonized porous sample, it becomes depleted in silicon with an increase in the content of impurities, primarily Fe and Al, and the formation of SiC, Fe₃C, and FeSi. The theoretical calculation showed that the relative changes in volume for the reactions of SiC and Fe₃C formation upon interaction of 1 mole of carbon with silicon and iron are 134 and 339%, respectively. Moreover, with a significant content of iron in the melt, a significant role in the overlap of capillaries can be played by the volumetric change associated with the formation of Fe₃C. The results obtained can be used in the production of SiSiC-based tribotechnical parts, valves, etc.

The use of in situ diagnostic methods is required to obtain data on the structure and composition of the material in real time when studying condensed substances in the course of chemical reactions and phase transformations. We present the results on the development and application of the time-resolved X-ray diffraction method for the diagnosis of fast processes in heterogeneous condensed media, including self-propagating high-temperature synthesis. An X-ray tube was used as a radiation source. The method is based on the use of high-speed registration of XRD patterns in a wide angular interval and provides obtaining in situ data on the evolution of the crystal structure of the reactants. A high-speed linear detector and reaction chambers, an effective analysis system with a time resolution in the range of 10^–1 – 10² sec has been developed on the base of a powder diffractometer. A complex of object-oriented diffraction techniques has been developed to study the dynamics of phase transitions in self-propagating high-temperature synthesis of inorganic materials, combustion of energy systems and liquid solutions, crystallization of amorphous alloys, in the analysis of the phase composition of materials in the process of heat treatment. The results obtained can be used to identify the mechanism of structural and chemical transformations in condensed matter.

The magnetic anisotropy and magnetic structure of amorphous ferromagnets are largely determined by magnetoelastic interactions due to the absence of magnetocrystalline anisotropy, e.g., in amorphous microwires with a glass sheath, the source of anisotropy is the mechanical stresses that arise in the ferromagnetic core upon manufacturing. Hence, to control the magnetic structure and magnetization reversal processes occurred in amorphous magnetics, it is necessary to know the magnetostriction coefficient of the material. We propose an improved approach to measuring extremely small values of the magnetostriction coefficient of ferromagnetic microwires with an arbitrary type of magnetic anisotropy and magnetic microstructure. The samples of amorphous wires in a glass sheath made of Co₆₇Fe₅B₁₂Si₁₄Cr₃ alloys were studied. The type of magnetic anisotropy of the samples (from axial to circular) was changed using current annealing. The developed method is based on small-angle precession of magnetization around the wire axis, resulted from the effect of the axial magnetic field induced by an alternating current passed through the wire. A voltage signal generated in a detection coil wound around the sample at a frequency doubled with respect to the frequency of the alternating current was recorded using a lock-in amplifier. When exposed to external mechanical loads, the voltage signal changes, and an additional axial magnetic field (bias field) is required to maintain a constant level of this signal. The value of magnetostriction is determined from the dependence of the displacement field on mechanical loads. The maximum sensitivity of measurements in the range of 10^–8 – 10^–7 is achieved at a uniform magnetization, increased frequency of the alternating current, and high value of the ratio between the length and diameter of tested wire samples. The sign and magnitude of the magnetostriction constant change upon current annealing which correlates with modification of the magnetization curves. The results obtained can be used to determine and adjust the parameters of the actuators developed on the basis of the considered microwires (in particular, microsensors of mechanical stresses and microactuators).

A structural-phenomenological concept (SPhC) of monitoring the residual strength of composite materials is proposed. SFK was developed taking into account the kinetics of damage and destruction of polymer composite material (PCM) at the micro-, meso- and macroscale levels, which generate acoustic emission pulses (AE) recorded by the receiving transducers of the antenna array. A correspondence between the ongoing destruction of the composite material structure at the micro-, meso- and macroscale level and the AE pulses recorded at the same time and their weight content provides the possibility of monitoring of the damage kinetics in the loading mode at all structural levels, and, consequently, the possibility of control of the residual strength of the product. An algorithm and software have been developed that made it possible to divide the recorded AE signals into the clusters of lower, middle and upper energy levels corresponding to micro-, meso- and macroscale disruptions of the structure of a composite material, calculate the AE activity and the weight content of location pulses in energy clusters, thus displaying the dynamics of their changes every second. Comparison of the current values of the most informative parameters of the weight content of location pulses in energy clusters with the threshold values recorded during the destruction of the material provides monitoring of the residual strength of the product in the loading mode. The validity of the developed concept, algorithm and software was proved during tests of elementary and structurally similar samples of PCM under different loading conditions. An example of using the developed technique for revealing the areas of the most intense damage accumulation in a MS-21 fuselage panel at a stepwise increase in the compressive load is presented. In addition to the possibility of identification of the area of intensive accumulation of damage and failure of the structure of the composite material, SPhC of the AE diagnostics provides also the possibility of tracing the damage kinetics at different scale-structural levels, controlling the level of the residual strength of the panel upon the stepwise compression.

Modern approaches to processing large bulk of data accumulated as a result of mechanical testing, based on statistical analysis and machine learning methodology are discussed. The factors affecting the strength and durability of pipe products are considered. The stages of the initial data preparation are analyzed and the main steps of basic statistical processing, correlation and variance analyses, approaches to grouping and ranking of test data are discussed. The results of the developed approaches are demonstrated by the example of constructing a classification by steel grades and technical conditions of the pipe production according to the actual mechanical characteristics of the pipe metal. The real effect is shown on the example of the estimating the number of pipe defects that require priority to repair. The presented algorithms can be used as the elements of the formed information base and data banks in the field of pipeline transportation of oil and oil products. The developed approaches require a comprehensive testing and further development towards taking into account the actual loading of the pipe and assessing the failure probability.

The study is aimed at the development and implementation of an experimental setup for treating metal parts with complex geometry to induce compressive residual stresses in the surface layers. Modern methods of surface treatment demonstrated the possibility of increasing the durability of parts by several times through creation of high-amplitude residual compressive stresses. We managed to form the residual compressive stresses up to a depth of 1 mm using the titanium alloy specimens. The developed installation consists of a solid-state laser with a pulse energy of up to 10 J, a six-axis robot manipulator, and a system for measuring residual stresses by hole drilling method. The processing is realized in automatic mode with the possibility of continuous change of specimens. The geometry of parts and processing features are worked out on a digital three-dimensional model of the part. A number of tests have been carried out to reveal the dependence of the values of residual stresses on the processing conditions and demonstrate the necessity of numerical analysis and preliminary modeling of the process of laser shock peening. The distribution of residual stresses was measured by hole drilling method in the specimens before and after laser shock peening under various processing conditions, and the profiles of these stresses in depth were plotted. It is shown that along with the pulse power, the value and distribution of residual stresses are significantly affected by the number of repeated passes, the overlap degree, and the technology of preliminary preparation of the specimen surface. The analysis made it possible to choose the optimal processing mode for titanium alloys providing the values of residual compressive stresses up to 1 GPa.

An approach to creation of an intelligent system for predicting the state of a technological process in real time is presented. The approach is based on the analysis of a video sequence of images obtained as a result of streaming video by cameras installed on the tuyeres of a blast furnace. Algorithms for recognizing video images of tuyere foci, as well as scenario forecasting of the evolution of technological situations are proposed. A historical background regarding the development of methods for automatic control of the blast-furnace process, in particular, the use of artificial intelligence, is presented. The study is aimed at the ability of rapid analysis of the production situation (PS) and prediction of the PS evolution in the course of functioning of the blast furnace process, which will provide the possibility of timely decisions on adjusting control in an automatic or automated mode. Using the developed algorithm for analysis and prediction of the process dynamics and proceeding from the revealed regularities of the change in video data, a method for early detection of a tendency to the occurrence of certain events on tuyeres, including those leading to the destabilization of the blast furnace process, is proposed. The novelty of the presented approach lies in the fact that not only the state of the process at the next moment of time, but also the most probable chain of several subsequent states is predicted. Real-time forecasting algorithms are based on the construction and replenishment of the base of inductive knowledge — regularities revealed through the intellectual analysis of the revealed information — in the course of real functioning. Methods of studying Markov chains, machine learning and wavelet analysis are used for the associative search for patterns. The algorithms developed by the authors can be used in decision support systems for blast-furnace control. The results of practical research, confirming the effectiveness and viability of the proposed approach, are presented.