Successful functioning of expert systems designed for determination of the molecular structure of organic compounds by spectral characteristics requires the availability of most complete initial analytical information. Successful functioning of expert systems designed for determination of the molecular structure of organic compounds by spectral characteristics requires the availability of most complete initial analytical information which necessitates summarizing and using data gained in different analytical methods. We consider prospects of gaining new information about test compounds by the method of resonant electron capture negative ion mass spectrometry using a serial quadrupole mass-spectrometer. A number of phosphorus-containing organic compounds are used to demonstrate a possibility of recording mass spectrum peaks of deprotonated molecules, which is rather important for determination of the molecular mass and, hence, correct identification of the compound. Examples of successful detection of the fragments with positive electron affinity present in the structure of compounds under study are listed. The obtained results substantially differ from that obtained by the “classical” method of electron ionization positive ion mass spectrometry and can be considered as a complementary data about the structure of compounds for the purposes of structural group analysis., We also present the results of experiments in which mass spectra of negative ions were obtained using the advanced cathode power supply device via multiple change in the energy of ionizing electrons during the analysis. The possibility of implementing both analytical methods on the same device is an additional advantage of this approach.

A radically different behavior of oxides — BaBiO₃ and superconducting K_nBa_mBi_m+nO_y (n = 1, 2, 3; m = 1, 3, 4, 5) — and BaO₂ peroxide is observed in reactions of hydrolysis and acid dissolution. Chemical tests and potentiometric analysis did not reveal peroxide-ions present in BaBiO₃ and K_nBa_mBi_m+nO_y, as well as in the products obtained by oxide treatment with water, alkali and acids. Most probably this indicates to the absence of unusual valence states (UVS) of oxygen in the form of peroxide- and superoxide-ions in the structure of oxides under study. Data of potentiometric titration (PT) also proved the absence of oxygen UVS and bismuth in the oxidation state of < + 3 in superconducting K_nBa_mBi_m+nO_y oxides. A number of agents (Mn (II), Cr (III), Cu (II), Ce (III) salts, Arnold’s base, methyl red, chromazurol S, arsenazo III, indigo carmine, and thoron) are revealed which provide Bi (V) detection in BaBiO₃ and K_nBa_mBi_m+nO_y. An experimentally observed behavior of the oxides in chemical reactions regarding agents-reductants is attributed to Bi (V) present in their structure which is much stronger oxidizer compared to peroxide dioxygen.

The results of irradiation of metal (nickel alloy Inconel 718) and semiconductor (silicon single crystal) materials by helium ions and helium plasma pulsed beams using a plasma focus (PF) device “Vikhr” are presented. The damageability and radiation-thermal stability of the materials exposed to high-power pulsed helium ion beams of the working gas and high-temperature plasma have been studied and assessed in a wide range of the radiation power density (pulse duration 10^-8 - 10^-6 sec). Experiments showed that both materials exposed to “soft” irradiation (q = 10⁶ -10⁷ W/cm²), which did not lead to complete surface melting, underwent the process of sputtering mainly in the areas containing mechanical defects. However, for each of the materials, local areas of melting of the surface layer are observed, which is associated with an irregular distribution of the particle density over the cross section of the radiation flux incident on the target sample. A thin film was found on the surface of both materials: SiO₂ oxide on a Si single crystal; and a film resulted from the interaction of the alloy components with residual gases in the PF chamber and chemical elements deposited earlier on the surface of Inconel 718 alloy. Irradiation in a “hard” mode (q = 10⁸ - 10⁹ W/cm²) with a large number of puls shots leads to melting and partial evaporation of the surface layer with the formation of a wave-like relief and microstructural defects such as ridges, craters, bubbles and microcracks after crystallization of the melt. A solidified surface layer becomes very brittle, easily separates from the non-melting Si base and breaks up into small particles like a powder. We have shown that after the beam-plasma treatment, the surface layer of silicon contains the elements occurred in other structural and functional materials located in the PF chamber. At each pulsed discharge, they are deposited on the irradiated surface of Si single crystal. Experiments and studies have also shown that a device “Vikhr” is promising for simulation of extreme conditions of exposing material to ionizing radiation, which are realized in thermonuclear devices with magnetic and inertial plasma confinement, as well as for creating more “soft” radiation regimes characteristic of the radiation fluxes of the space environment.

The results of X-ray diffraction analysis of qualitative and quantitative phase composition of powder and solid polycrysral samples of the system a-WC/W₂C are presented. Powder (nanopowder) samples were obtained by plasmochemical synthesis from tungsten oxide and hydrocarbon. High-density fine-grained structure of ceramics was formed by electropulse plasma sintering (spark plasma sintering) of initial industrial a-WC powders (AlfaAesar). Experimental data were obtained on a Shimadzu XRD-7000 X-ray diffractometer (CuKa, λ = 1.54 Å). The optimal modes of X-ray shooting of the ceramic samples based on tungsten carbide are presented. In the absence of reference standards for initial crystalline phases (WC and W2C), quantitative phase analysis was carried out using the reference intensity ratio (RIR) or corundum number (instead of the method of calibration curve). The required quantitative ratios were calculated using the structural parameters of corundum a-Al₂O₃ and phases a-WC, W₂C. The results of determining the repeatability of the intensity values were used to select the optimal exposure time and width of the receiving slit of the detector of diffracted X-rays. Study of the effect of the quality of sample preparation on the sensitivity of qualitative X-ray phase analysis showed the feasibility of grinding of the surface of solid ceramic samples and their pre-polishing with a diamond paste (grain size not less than 5/3 pm). The accuracy of quantitative phase analysis of powder and sintered ceramic samples was evaluated. The layer-by-layer phase analysis of the ceramic preform revealed a preferential crystallite orientation (texture) in the surface layer and the absence of the impurity phase W₂C. The sensitivity of X-ray phase analysis to the content of a-W₂C phase in nanopowders of tungsten monocarbide has been estimated.

A method and installation for measuring electrode potentials on the local areas of metal surfaces and welded joints are developed. The special of the method and design of the installation is the supply of electrolyte to the metal surface due to the capillary effect of the wick made of fiber material. A gold wire was chosen as a reference electrode. Combination of the capillary supply of the electrolyte and electrode of small diameter provides measuring of the electrode potentials on rather small (up to structural components) surface areas. Change in the electrode position and electrode potential recorded in continuos mode can be visualized and scaled-up on a computer display. The developed procedure provides determination of the electrode potentials on the surfaces of metal materials with electrochemical heterogeneity and can be used to assess the corrosion resistance of materials; electrochemical heterogeneity of the structural components; forecast the service life of the metal structures; simulate the technologies of welding and soldering steel with metal corrosion coatings with a minimal damage to the protective coating and determine the corrosion properties of the products in service to predict their residual life.

The article is focused on the comparison of two approaches to determination of the stress-strain states (SSS) and strength calculations for a thin plate with a stress concentrator in the form of a circular hole subjected to static and cyclic loading by solving the elastic problem (Kirsch problem), and also using deformation criteria of deformation and failure developed in IMASH . Using the new approach, the characteristics of the main mechanical properties, values of the rated stresses and strain fields in the stress concentration zones were varied for the first time (four calculated cases). The data analysis showed that at the sites of the cross section located near the stress concentrator, the elastoplastic stresses and strains occur already at the initial stages of loading. The stresses and strains thus determined differ greatly from those obtained using the elastic solution. The strength analysis of a thin plate with a circular hole carried out according to the strain-based criteria showed that SSS differs significantly from that obtained using the traditional elastic solution. This is true not only for the initial loading in the zone of maximum concentration (on the hole contour) but also for other points of dangerous cross-section of a specimen subjected to cyclic  loading. Using the above method one can calculate the stress and strain kinetics in the stress concentration zones (for a given plate cross section) for any loading cycle and thereby determine the stress-strain state kinetics in the concentration zones, and carry out more precise calculations of cyclic durability with allowance for the scatter of the basic mechanical properties of the structural material.

The data on damage accumulation and service life of the elements of welded metal structures made of 09G2S steel during their operation in the Far North (regions located mainly north of the Arctic Circle) are presented. The mechanism of damage accumulation in steel undergoing a low-temperature ductile-brittle transition was evaluated by measuring the impact toughness of the V-notched specimens (KCV) in the corresponding temperature range. Analysis of experimental data revealed that the most severe loss in the weld plasticity occurs in the heat-affected zone characteristic with stress localization and accelerated accumulation of the defects and crack development resulting in a decrease the lifetime of steel structures at low temperatures. The method for estimating integral damage of steel welded structure subject to a ductile-brittle transition is proposed proceeding from the Kachanov-Rabotnov damage accumulation theory with due regard to the operating time of the material in severe climatic conditions. Comparison of numerical estimates of accumulated damages in the material of the structures operating in extreme conditions of the Republic of Sakha (Yakutia) and in the climate of the Krasnoyarsk Territory of the Russian Federation allows us to conclude that MTBF and lifetime of the structures are largely determined by climatic conditions.

Diagnostics of the emergencies attributed to the pipeline destruction resulted from hydrogen charging and corrosion is one of the important problems of the oil and gas industry. Corrosion and hydrogen charging of the metal lead to formation of holes in the pipe wall at a certain critical ratio of the metal strength and thickness resulted from the impact of the internal pressure of the gas transported through the pipeline. Despite extensive research, many issues related to this problem require further consideration. This concerns, in particular, the issues regarding kinetics of the brittle fracture of metal of the pipeline walls and the role of diffusion-mobile (active) and combined (bound) hydrogen in this process. Electrochemical hydrogenation (saturation) of cylindrical steel samples revealed that the zone of penetration of electrolytic hydrogen match the region of the cleavage crack origin, i.e., the area of the subsurface hydrogen distribution can be considered a local area of micro-cleavage in the peel tests thus making possible the study of kinetics and concentration dependences of steel brittle fracture under the impact of both diffusion-mobile and combined hydrogen, i.e., under conditions of reversible and irreversible hydrogen brittleness. The dependences of the peel resistance (micro-cleavage) on the concentration of diffusion-mobile (active) and bound hydrogen in the micro-cleavage zone are obtained as a result of kinetic studies. Electron-fractographic study of fractures of 18KhGMF steel samples showed that fracture morphology changes in accordance with the stages of brittleness development. The initial ductile fracture is followed by a typically brittle peeling at reversible brittleness. Then, with the development of irreversible fragility, a mixed character of destruction is observed. The obtained three-stage dependence of the peeling strength, taking into account different hydrogen states, proves the different physical nature of the processes at different stages of hydrogen brittleness and connects the known reversible and irreversible hydrogen brittleness with the effect of diffusion-mobile and bound hydrogen, respectively.

A new version of ISO/IEC 17025:2017 released in November 2017, and a new version of GOST ISO/IEC 17025 developed on the basis of this document which is to appear in 2019 are discussed. An emphasis is made on the concept of management and operation of testing industrial laboratories (IL) in quality assurance, including application of the process approach and risk management which are considered the main tools of the quality management system (QMS) of testing laboratories. The goal of the article is to provide practical assistance in ensuring a smooth transition of IL from meeting the requirements of the current GOST ISO/IEC 17025-2009 standard to the new version based on the aforementioned process approach and risk-based thinking, the main focus being on the embodiment of risk management requirements. We consider the stages and objectives of the risk management process and options for a systematic approach to risk management, taking into account the initial and subsequent stages of further improvement of the process. Specific recommendations for risk management implementation in IL with a description of the risk management process in the laboratory within the life cycle of the laboratory products or the main business process are proposed. Examples of risk assessment in IL using effective tools: “brainstorm” and “matrix of consequences and probabilities” are presented. The guidelines of improving risk management and subsequent the transition to a more detailed assessment and management of risks are specified and exemplified in the framework of the IL activity. The directions of further developing the QMS of IL regard-ing setting goals and objectives are outlined taking into account risk assessment and risk management both within the internal context of the laboratory and the enterprise, and with allowance for the external environmental impact.