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Industrial laboratory. Diagnostics of materials

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Vol 90, No 9 (2024)
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SUBSTANCES ANALYSIS

5-14 247
Abstract

Currently, the problem of selenium determination in various objects attracts a large number of scientists. Interest in this area is attributed to the biological importance of selenium, since it is both an important nutrient and has a toxic effect on the body, depending on its amount and the properties of the compounds in which it is contained. Checking the purity of selenium-containing organic compounds (both determination of impurities and analysis of the basic composition), which is carried out by methods of elemental analysis, is an important task, however, in modern literature there is lack of information regarding this problem. The purpose of the presented study is to develop a method for the determination of selenium in the basic composition of synthetic polyheteroatomic organic compounds by microwave plasma atomic emission spectrometry. Various selenodiazole derivatives were mainly used for analysis. Optimal conditions for sample preparation and atomic emission determination of the selenium content were specified. To mineralize the substances under study, oxygen flask combustion was used with the addition of potassium nitrate, which improves combustion and prevents the formation of soot. Hydrochloric acid at a concentration of 0.1 M was used as an absorption solution. It is noted that before measurements it is necessary to purge the monochromator and optimize the pressure in the atomic emission spectrometer nebulizer and optimize pressure in the atomizer. In addition, the number of replicates and sampling time were increased to optimize selenium measurement. Under specified conditions, the metrological characteristics of the technique were determined: the detection limit and quantitation limit, intra-laboratory precision and accuracy. Selenium was determined in 11 synthetic organic compounds with selenium content ranged from 12 to 51%. The error of the analysis did not exceed 0.3%, which meets the requirements of organic elemental analysis.

15-23 251
Abstract

The methodology of arranging laboratory studies of oil-contaminated soils, soils and bottom sediments to determine the source and composition of hydrocarbon contamination is described. The complex approach to laboratory analysis of samples of oil-contaminated soils, soils and bottom sediments is proposed, which allows a highly reliable identification of the potential source of contamination and/or making conclusions about the identity of the contamination of adjacent territories. The proposed complex of analytical methods includes infrared spectrometry, gas chromatography with mass-selective detection, thin-layer chromatography with flame ionization detection and elemental analysis (C, H, N, S, O). Application of the proposed integrated approach allows highly reliable determination of the nature of oil contamination of soils, estimation of the total gross content of oil products and their hydrocarbon composition, and identification of the potential source of pollution. Possible errors in the interpretation of the results of determining the identity of contamination of territories and the importance of using an integrated approach in drawing conclusions about the source (culprit) of pollution are shown using real soil samples taken from oil-contaminated objects and adjacent territories. The importance of taking into account the losses of volatile oil products at the stage of sample preparation for soil contamination with light oil fractions is demonstrated. The use of standard methods of sample preparation (drying of the samples under study) leads to errors in assessing the level of contamination of territories with volatile hydrocarbons and in the choice of methods of remediation of contaminated territories. To minimize losses of volatile hydrocarbons (petrol and naphtha fractions) at the stage of soil sampling and transportation the use of sorbent is proposed. Addition of a sorbent to the soil contaminated with oil products can reduce losses of volatile hydrocarbons by 15 – 20% in the analyzed samples. Application of the developed complex approach makes it possible to determine the features of the individual hydrocarbon composition, group and elemental composition of petroleum products and identify hydrocarbon indicators (markers) inherent only to a certain type of petroleum product.

24-31 325
Abstract

Redox titration is one of the most common classical methods widely used in practice for the determination of total iron. A well-known procedure ISO 2597-1 (GOST 32517) includes the decomposition of a sample with dissolution, the reduction of Fe3+ to Fe2+ using a SnCl2 solution and its titration with a K2Cr2O7 solution in the presence of sodium or barium diphenylaminosulfonate as an indicator. We propose to use potassium tetrahydroborate KBH4 as a reducing agent for Fe3+ to Fe2+ instead of SnCl2 to modify a titrimetric method of total iron determination. The features of the well-known and considered methods are studied when using sintering for sample decomposition during the analysis of a large number of samples. Application of the developed method for the analysis of standard samples and technogenic materials with a high copper content, namely, Waelz slag showed a satisfactory accuracy and reproducibility of the obtained values of the total iron content. The results obtained indicate the possibility of the application of this method to the iron determination in the samples with a high copper content without an additional step of the iron separation from copper. A high productivity of the analysis (apart from the absence of the separation stage) is achieved due to the simplicity of the reduction process occurred at room temperature, no need for the control of the added amount of the reducing agent, and the possibility of holding the solutions for a long time before the titration. These advantages along with the no need for using toxic mercury compounds during the analysis make the method attractive for the analysis of a large number of samples.

TESTING OF STRUCTURE AND PARAMETERS. PHYSICAL METHODS OF TESTING AND QUALITY CONTROL

32-38 128
Abstract

Among the reasons for the rejection of products made of polymer materials manufactured using HF electrothermy, an important place is occupied by the lack of available reference data on the modes of their processing. The inaccuracy of some electrical parameters, e.g., the dielectric loss tangent (tan δ) and the dielectric constant (ε) are attributed to neglecting the effect of gaps in granular multicomponent polymer materials or technological system, as well as subjective factors of the control process. We present the results of studying the impact of gaps of a technological system on the electrophysical parameters of polymer and composite materials. We studied samples of granular materials «Bimodal polypropylene» and «Basco» stabilizing additive which are used in production of UV-resistant films for packaging. It is shown that a resonance method with the possibility of using two- and three-electrode system is most appropriate when determining the electrophysical parameters of polymer materials, their multicomponent mixtures and the optimal frequency of exposure. Refined (determined with allowance for gaps) electrophysical data for the materials under study obtained at a frequency of 27.12 MHz and heating to 120°C are presented. Comparison of the results obtained with and without taking into account the impact of gaps revealed that the difference reaches up to 12 (for tan δ) and 9% (for ε) of their absolute value. Note that the parameter tan δ has the greatest effect on the heating efficiency. The optimal temperature of polymer heating at which tan δ reaches the maximum value is 50°C. The results obtained can be used to improve the quality of products produced from a wide range of multicomponent polymer and composite materials by optimizing the modes of their electrothermal processing.

39-47 375
Abstract

Hexagonal ferrites of M-type (in particular, BaFe12O19) are magnetic materials with functional characteristics affected both by chemical composition and technology of their synthesis. We present the results of studying the magnetic and structural properties of BaFe12 – xCuxO19 hexaferrites (x = 0, 0.1, 0.2, 0.3, 0.4) obtained by hydrothermal synthesis with partial substitution of copper for iron. The composition of the synthesized samples was analyzed using X-ray diffraction, and the magnetic characteristics were measured using a vibration magnetometer. It has been revealed that the coercivity of the ferrite powders depends non-monotonically on the copper concentration and reaches the maximum (5629 Oe) and minimum (4698 Oe) values at x = 0 and x = 0.2. The presence of copper reduces the coercive force, but at the same time the values remain rather high compared to the results of similar studies. The saturation magnetization of the obtained ferrites gradually decreases (from 65.88 to 60.75 A · m2/kg at x = 0 and x = 0.4, respectively) with increasing. The distribution of Cu over ferrite sublattices was studied using Mössbauer spectroscopy. It is shown that in the hexaferrite structure, copper ions preferentially occupy 12k and 4f1 sites. Hence, a decrease in the saturation magnetization with increasing x is most likely attributed to the presence of side non-magnetic phases observed on X-ray diffraction patterns. It is also revealed that during synthesis, copper participates in the formation of low-melting phases on the surface of hexaferrite grains which promotes agglomeration of the particles. Thus, the resulting powders can potentially be sintered at lower temperatures and, therefore, without a significant increase in the size of crystallites. Herewith, the coercivity retains its original high values. The results obtained can be used in developing ferrite permanent magnets with improved characteristics.

48-53 145
Abstract

The strength of the working surfaces of gears depends on the mechanical properties of the material and the quality of parts. We present the results of studying the strength of materials and working surfaces of a gear mechanism due to structural changes attributed to chemical and thermal treatment. The surface strength of the gears of gas turbine engines was studied. Nitrocementation and ion nitriding were used for chemical and thermal treatment of the contacting surfaces of steel samples under study (20Kh3MVF-Sh, 16Kh3NVFMB-Sh, 18Kh2H4MA, and 12Kh2H4A). Changes in the microhardness of the component layers (diffusion, transition and basic) of the toothed crown were analyzed. Metallographic analysis of the structure of materials was carried out to describe the factors determining the surface strength of working surfaces. Systematized data on the change in the microhardness of materials obtained experimentally in conditions of mass production are presented. Presented experimental results on changes in the mechanical properties of materials are based on data on the microhardness and structural state of the surface layers of the working profiles of gears. A comparative assessment of the surface strength of the studied samples during contact interaction was performed. The dependence of the surface strength on the multifactorial volumetric structure and structure formation of the material in the process of operation is determined. It is shown that the method of surface saturation forms the structure of a material with different mechanical properties accompanied with the formation of a transition zone having characteristic distinctive values of the hardness. The results obtained can be used in the design of gears, taking into account changes in the mechanical properties and structure of materials to ensure the necessary operational requirements.

TESTING OF STRUCTURE AND PARAMETERS. MECHANICAL TESTING METHODS

54-62 110
Abstract

It is noted that under real operating conditions of technical systems the so-called non-stationary loading in which external loadings increase or decrease arbitrarily is realized most often. At the same time final ratios between strains and stresses are of practical interest to engineering calculations. It is shown that for simple cyclic loadings the state equations in final ratios which are based on the theory of small elastic-plastic strains can be used. In this case the existence of the uniform generalized deformation diagram assuming a final relation between the corresponding components of stresses and strains both for initial and cyclic stages of deformation is essential for the analysis of considered conditions of a non-stationary cyclic loading. The analysis of conditions of achieving limit states at all stages of the life cycle the criteria base and the system of the computation equations become more complicated and more saturated by the factors taken into account and among them first external and internal impacts of natural, technogenic, anthropogenous origin, load from these impacts, and the reactions of installations to such impacts and loads as well. At the same time a set of criteria defining a limit state is presented in the form of a functional dependence characterizing a set of force and deformation parameters of the state of technical system on the one hand, and, on the other hand, a complex of criterion characteristics of constructional materials taking into account their change during operation. The most important step of determining conditions for achievement of the limit state causing fracture is establishing the critical parts that determine risks of emergency and catastrophic situations in which processes of local and main fractures are initiated. In this case transition of the operated installation from design area to the area of initiation of refusals, accidents and disasters occurs when the parameters of damage, defectiveness and risk reach their critical values.

63-74 245
Abstract

In the era of digital transformation, most devices are equipped with a variety of sensors, which provide information to be used in developing intelligent models for predicting the fatigue life. The development of digital models of real objects for fatigue life estimation faces the lack of algorithms for performing such an estimation. The problem arises in the adaptive and automatic analysis of signals from real sensors installed on the object and their subsequent processing to estimate the fatigue life of the object. We propose a new method for assessing the fatigue life of structures based on application of the adaptive method of variational mode decomposition to signals gained from sensors, including non-stationary ones. Variational mode decomposition involves decomposition of an initial complex random process into simpler random processes (modes) that are stationary and narrowband. An original method of summarizing damage resulted from the action of the modes obtained as a result of the decomposition is used. The developed method can be used as an algorithmic support for the generation of digital doubles of the residual lifetimes of natural products. The proposed method is compared with the «rainflow» method in the time domain. Different realizations of random stationary and non-stationary signals with different bandwidths are compared numerically. In addition, the traditional frequency methods of Dirlik and Benasciutti have been compared with the «rainflow» method. The analysis showed good results for the proposed method, i.e., the error was smaller compared to traditional frequency methods, especially for non-stationary processes.

75-84 170
Abstract

Cavitation wear is a pervasive phenomenon on water transport. The parts of ship propulsion system as well as the water-cooled surface of cylinder liners of high-speed ship diesels are subjected to cavitation attack. Bright chromium deposits are used to protect the water-cooled surface of liners. Nevertheless, the effect of cracks appearing in the electrolytic chrome coating upon depositing on the cavitation resistance of coating is still an open relevant problem. The goal of the study is to analyze the kinetics and mechanism of the destruction of the bright chrome electrolytic deposit under cavitation attack. The cavitation resistance of chrome electrolytic coatings after grinding and after polishing was studied. The chrome electrolytic coatings were obtained on the plates (90 × 30 × 7 mm in size) made of cast iron SCh21. The chrome was deposited on one side (90 × 30 mm) of the plate placed vertically by flow anodic jet chrome plating in standard electrolyte (kg/m3): chrome anhydride — 250; sulfuric acid — 2.5; trivalent chrome — no more than 5; trivalent iron ions — no more than 10. The electrolyte was prepared using distilled water of a single distillation. The parameters of depositing: electrolyte temperature is 50°C; the current density amounts to 60 A/dm2. Four samples cut from the same plate were used. The coatings on the first two samples were ground using the abrasive paper number 320. The coatings on the second pair of samples were first ground successively on the abrasive paper of different grit: 320, 500, 800, 1000, and 1200, and then polished on the cloth with GOI paste. The cavitation wear tests were carried out on a magnetostrictive vibratory rig in fresh water, the frequency and amplitude of the rig horn vibration was equal to 22 kHz and 28 μm, respectively. The spacing between the chrome-plated sample surface and the horn butt was 0.5 mm. The wear of the samples was evaluated by periodical weighing during testing. The wear of the ground samples turned to be significantly higher, than that of polished samples. The photographs of the surface after different duration of the cavitation attack show that the initial cracks formed on the coating during chrome plating are the centers of cavitation destruction. To reduce the negative impact of initial cracks on the cavitation resistance of the bright chrome electrolytic coatings deposited on the water-cooled surface of the cylinder liners of diesels it is shown expedient to include polishing in the technological process of depositing chrome coatings.



ISSN 1028-6861 (Print)
ISSN 2588-0187 (Online)