A comparative analysis of the behavior of oxides containing Fe (III) and Fe (IV) in redox reactions with organic and inorganic reagents has been carried out. SrFeO_3-x oxide obtained by solid-phase synthesis from SrCO₃ and Fe₂O₃ has been an object to develop test methods. It has been shown that Fe (IV) exhibits the properties of a stronger oxidizer than Fe (III), thus providing a set of reagents which enable identification of Fe (IV): hydrobromic acid, Fe²⁺ complex with V (IV), and Mn (II) salts, and organic reagents, namely, amines (diphenylamine, o-tolidine, benzidine) and dyes (methyl red). Potentiometric method proved stronger oxidative properties of Fe (IV) compared to Fe (III) revealed in different character of changes in EMF during dissolution of the corresponding oxides in HCl. SrFeO_3–x oxide does not oxidize Mn (II) to Mn (VII), Cr (III) to Cr (VI), Ce (III) to Ce (IV) in acidic media, and Cu (II) to Cu (III) in alkaline media. Since the oxide under study oxidize Cl^– = 1.3583 V) and Br^– = 1.087 V) ions to the corresponding halogens, but does not oxidize Mn²⁺ to = 1.51 V), an estimated value of the standard redox potential is ~1.4 V. We have developed for the first time a system of analytical tests for differentiation of Fe (IV) and Fe (III) which can provide monitoring of the synthesis of complex oxides and phase formation in the systems containing iron, alkali and alkaline earth metals.

A technique of the X-ray fluorescence analysis (XRF) based on a linear regression providing correlation between the gold content in the sample and radiation intensities of the elements of the analyzed alloy is developed at the analytical center of the JSC «Krastsvetmet» (laboratory of X-ray spectral analysis) to increase the rapidity of gold determination in gold-based alloys. The regression equation chosen by the methods including the influencing factor (contributor) and estimating correlation between the disparities and influencing factor takes into account the effect of such elements as Ag, Cu, Zn, Ni, and Pd on the gold line intensity. Virtual calibration samples (VCS) — the results of the analysis of real samples (X-ray line intensities of elements and gold values obtained by the assay method) taken from electronic database (DB) are used to form a system of linear algebraic equations (SLAE) which is to be solved for determination the desired linear regression coefficients. VCS for which the line intensities of the elements are close to those measured for the analyzed sample are selected from the database using a specific filter: the filter value is determined for each of the elements (metals) in the sample. The developed and integrated into the laboratory information system (LIMS) multi-version software (MVS) for solving SLAE includes several algorithms implemented in various programming languages. The use of the presented methodology significantly reduces the time of analysis. The error of gold determination does not exceed 0.13% which is comparable with that in the assay method.

When using cathodic protection of steel in sea water, hydrogen can be accumulated on the cathode surface and penetrate deep into the metal. This rather dangerous phenomenon of hydrogen corrosion can lead to hydrogen embrittlement, i.e., to destruction of the metal. We present the results of studying the impact of the temperature and external tensile stresses on the hydrogenation of cathodically protected steel in calm and mobile Baltic sea water. Dependence of the inhibitory hydrogenation on the temperature and applied load under the action of benzenesulfapyridine chloride as an inhibitor was analyzed. An MIP-102 machine (wire samples) and special equipment (half-ring and plate lamellar samples) were used to provide smooth control of the applied load set by the deflection and controlled by dynamometers (lamellar samples were tested under constant deformation). When studying the effect of temperature on steel hydrogenation, the working cell was thermostatically controlled. The wire and plate samples were polarized for 96 h, and half-ring samples for 1 h. The potential was measured with respect to the silver chloride reference electrode. The layered distribution of absorbed hydrogen in the metal was determined using anodic dissolution. It is shown that external tensile stresses increase the hydrogen content in the surface layers of steel. Hydrogen absorbed by a metal changes the potential of the steel surface (the more absorbed hydrogen, the stronger change). It is also shown that hydrogen is absorbed by the metal more actively in moving seawater than in calm water, and an increase in the load contributes to an increase in hydrogen content in the metal both in calm and mobile seawater. However, the load did not affect the hydrogen absorption with the inhibitor present, thus providing reduction of the hydrogen content in the metal under loading.

The results of studying the phase composition of advanced calcium phosphates Ca₁₀(PO₄)₆(OH)₂, β-Ca₃(PO₄)₂, α-Ca₃(PO₄)₂, CaHPO₄ · 2H₂O, Ca₈(HPO₄)₂(PO₄)₄ · 5H₂O using an x-ray diffractometer with a curved position-sensitive detector are presented. Optimal experimental conditions (angular positions of the x-ray tube and detector, size of the slits, exposure time) were determined with allowance for possible formation of the impurity phases during synthesis. The construction features of diffractometers with a position-sensitive detector affecting the profile characteristics of x-ray diffraction peaks are considered. The composition for calibration of the diffractometer (a mixture of sodium acetate and yttrium oxide) was determined. Theoretical x-ray diffraction patterns for corresponding calcium phosphates are constructed on the basis of the literature data. These x-ray diffraction patterns were used to determine the phase composition of the advanced calcium phosphates. The features of advanced calcium phosphates, which should be taken into account during the phase analysis, are indicated. The powder of high-temperature form of tricalcium phosphate strongly adsorbs water from the environment. A strong texture is observed on the x-ray diffraction spectra of dicalcium phosphate dihydrate. A rather specific x-ray diffraction pattern of octacalcium phosphate pentahydrate revealed the only one strong peak at small angles. In all cases, significant deviations are observed for the recorded angular positions and relative intensity of the diffraction peaks. The results of the study of experimentally obtained mixtures of calcium phosphate are presented. It is shown that the graphic comparison of experimental x-ray diffraction spectra and pre-recorded spectra of the reference calcium phosphates and possible impurity phases is the most effective method. In this case, there is no need for calibration. When using this method, the total time for analysis of one sample is no more than 10 min.

Fractographic diagnostics of accidental damage provides data of expert importance which can be used in developing recommendations regarding of accident prevention, improving the reliability and performance of mechanical engineering products and structures in various operating conditions. The goal of the study is fractographic diagnostics of the nature and causes of premature destruction of technical devices and facilities operating in climatic conditions of the North and being the sources of increased technogenic danger, i.e., an automobile gas cylinder and a wind power plant. Using the basic principles of metal science, metal physics, strength and fracture mechanics, the localization of initial cracks we revealed the micromechanisms of crack formation, localization and development and restored the general picture of the fracture. It is shown that the main physical and mechanical causes of the gas cylinder damage are associated with the coarsening and inhomogeneity of the intermetallide phase distribution in the material of the inner metal shell («liner») and with the increased roughness of the internal surface which formed a system of stress microconcentrators. The reason for the collapse of a wind generator was lack of penetration in welded joints of the support structure being the place of origin of the initial cracks. The main fracture mechanism in both cases is time-evolving process of the metal fatigue initiated by technological micro-and macro-defects. The stage of the final destruction of a gas cylinder exhibited a dynamic character realized through the formation of a system of viscous cracks in the liner with their subsequent merging and fragmentation of the liner. The attained critical level of the fatigue crack development caused the onset of the ultimate state of the structure of a wind generator tower resulted in subsequent brittle fracture. The described destructions relate to gradual failures as they are caused by inherent technological defects rather than by external impacts. The results of the study can be used to improve the performance of the considered objects, ensure their operational safety and promote developing of compensating measures.

The residual strength and technical condition of the material of 530-mm steel pipe (14KhGS) of main gas pipeline are estimated to ensure the safety of long-term operation of pipelines in climatic conditions of the North. The mechanical properties are determined using standard methods of mechanical testing in laboratory conditions. A full-scale pressure test up to failure is used to determine the actual values of the fracture toughness and safety factor of the pipe. Full-scale tests were carried out on a test bench, a computer-measuring complex which displayed the reaction of the object to the load. A pipe fragment was cut from the linear part of the main gas pipeline and welded with spherical plugs. The outer surface of the pipe was notched along the pipe axis. The depth of the notch was calculated such that the breaking load on the ligament section at the notch site corresponded to the working pressure of the gas pipeline. No significant changes in the mechanical properties of the pipe metal were revealed in the absence of visible corrosion and deformation damage during long-term operation of the pipe in the North. Impact tests did not reveal embrittlement of the metal of the tested pipes. Full-scale tests of a pipe with an artificially applied defect made it possible to calculate the value of the critical stress intensity factor, which allowed us to estimate the residual strength of a pipe with a longitudinal crack. The value of the strength criterion of the fracture mechanics indicates the preservation of a sufficiently high viscosity of sheet metal pipes. Similar tests of the pipes (of other size and made of other materials) operating in the main gas pipelines should be continued taking into account temperature ranges and material degradation after long-term operation.

Diagnostics of the load bearing capacity of machines and structures, service properties of structural materials are carried out by destructive and non-destructive methods. In the system of non-destructive methods of diagnosing and monitoring of the service properties of materials and products, radiation technologies are of particular importance, since they have instrumental capabilities for diagnosing and controlling changes in the soundness of a solid body at different structural levels. The X-ray diffractometry method provided determination of the stability of the stress-strain state of structural steel samples subjected to prolonged (over 5 years) static loads not exceeding the yield strength of the material. The purpose of the study is to determine experimentally the effect of continuous (since 2013) elastic stress and climatic factors on the change in the half-width of the diffraction line profile. It is shown that the straight-line dependence of the half-width of the diffraction line profile is maintained in the range of elastic stresses not exceeding 0.5σ_t. The results of changes in the microstructural state (micro-strains) identified by the characteristics of the diffraction lines profile are presented and discussed. The results of the experimental study of the effect of small steady elastic stresses reveal that periodic annual fluctuation of temperatures (2013 – 2018) does not cause a significant change in the properties of the diffraction line profile of the 08ps structural steel samples. On the contrary, low climatic temperatures contributed to the elimination of individual instrumental errors attributed to design conditions of the experiment. A sharp change in the true half-width of the diffraction line profile at the stress values σ > 0.5σ_t, probably indicates the minimum margin of safety of 08ps structural steel when setting the permissible stress value (σ). The revealed changes in microplastic deformation observed in structural steels in the range of elastic stresses corresponding to real operational loads require further study and analysis.

The results of studying fundamental and applied problems regarding the formation of boundary layers between diamond and carbide matrix are presented with the goal to develop a highly resistant diamond tool. The new approaches to the synthesis of diamond-carbide materials combining diamond metallization and sintering in a single-stage technology are presented. The developed technology eliminates the re-heating of a metallized coatings which results in their destruction and enhanced graphitization of diamond (these phenomena restrict using metallization procedure to improve diamond retention and synthesis of high-functional composites for diamond tools). The goal of the study is analysis the structural and phase state of the «diamond – carbide matrix» interface in a diamond tool obtained by the new technology and the main factors determining the level of diamond retention in the presence of a metallized coating. Unique opportunities provided by modern high-resolution methods of research were used in the study. The elemental composition and morphological features of the diamond-matrix interface were studied using the methods of scanning electron microscopy, atomic force microscopy, X-ray microanalysis and Raman spectroscopy. Identification of the reaction products, including non-diamond carbon was performed. It is shown that the introduction of the powder-metallizer significantly modified the contact boundaries and provide conditions for improving the chemical and mechanical adhesion of the diamond-matrix system. The formation of the well-developed nano- and sub-microscale roughness of the diamond surface and dense filling of the existing voids with nanoscale layers of metal-infiltrate was revealed. The multilevel organization of highly structured elements of the transition zone with the minimal graphitization ensured the monolithic character and strength of the diamond-matrix bond. Comparative service tests of preproduction and control samples of diamond dressers proved the efficiency of developed hybrid technology (the specific performance of diamond tools increased by 39 – 45%). New fundamental and applied results have been obtained in the field of studying interface zones in crystalline multiphase systems that can be used to regulate adhesion phenomena at the interphase boundaries and develop highly efficient composite materials.

A method for determination of framycetin sulfate in a Framidex preparation (eye and ear drops) by HPLC-UV (λ = 365 nm) using 2, 4-dinitrofluorobenzene as a derivatizing agent has been developed The characteristics of analytical methods determined for the purpose of their validation and relevant criteria for the validity of validated methods with the goal of the quality control of drugs (pharmaceutical substances and drugs) are presented. According to the results of an intralaboratory experiment on the validation assessment of the method by the parameters of the specificity, limit of determination (LOD), linearity, precision and laboratory accuracy, it is shown that the LOD decreases by an order of magnitude, the correlation coefficient is not less than 0.99 correctness (average value — 97.5 – 102.5%; variation coefficient — not more than 2.0%; the confidence range should include 100% of values), convergence (variation coefficient — not more than 1.5%), intermediate precision (variation coefficient — not more than 1.5%). It is shown that the obtained values of metrological characteristics do not exceed the validation criteria and the developed method matches all the well-known requirements of GMP (Good Manufacturing Practice).