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Industrial laboratory. Diagnostics of materials

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Vol 84, No 10 (2018)
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SUBSTANCES ANALYSIS

5-11 770
Abstract
An ever-growing scientific interest in the development of effective methods for transformation of various cellulosic resources into fermentable sugars necessitates development of a universal procedure for determination of the reactivity of cellulosic substrates towards enzymatic hydrolysis. The practical significance consists in maximum accessibility of the procedure for the labs of pilot-production enterprises engaged in testing and scaling up the biotech processes. The developed procedure fully complies with modern requirements and relies on measuring the concentration of reducing sugars (spectrophotometry and HPLC) in the enzymatic hydrolyzates obtained from pre-prepared substrates, the biocatalysis being run by a cocktail composed of available CelluLuxe-A and BrewZyme-BGX. On top of that, the procedure implies gravimetric analysis of the solid residues after hydrolysis of substrates. Cellulosic biomasses can usually be fermented for control without any pretreatment, however, commercial celluloses can be used as well. The use of the developed procedure is shown to provide prompt and high-quality assessment of the reactivity of a series of chosen substrates to enzymatic hydrolysis. In contrast to the methods of enzymatic hydrolysis discussed in literature for evaluation of the enzyme efficiency, the developed procedure allows arranging of chosen cellulosic raw materials in a descending order of their reactivity to hydrolysis using the same multi-enzyme cocktail and, moreover can demonstrate dependence of the reactivity of substrates on the pretreatment method. The results can be presented as a dependence of the concentration (yield) of reducing sugars on the duration of enzymatic hydrolysis of the substrate, and also in the form of the calculated hydrolysis rates, final yields of reducing sugars including pentoses, content of glucose component of reducing substances and decrease in mass. The procedure was repeatedly tested on a wide range of cellulosic substrates and provided reliable results regarding evaluation of their reactivity and forecasting of the scale-up results of enzymatic hydrolysis, including that in aqueous medium when preparing nutrient broths for microbiological synthesis.
12-19 722
Abstract
The procedures of gold determination in microelectronic waste using flame atomic absorption spectroscopy (FAAS) and gravimetric analysis are developed. The developed methods are used for gold determination in the waste of gold etching (KI + I2) solution, technological mixture formed after cleaning vacuum deposition unit with aqua-regia solution as well as in a gold-containing powder obtained after reprocessing of liquid wastes. Optimum conditions for preparation and analysis of liquid and solid wastes having complex and variable matrix composition are specified. The FAAS methods of analysis provide determination of wastes in a wide range of gold concentration: in the solution for gold etching within the concentration range from 0.02 to 40 g/dm3, in the liquid phase of the technological mixture — from 0.1 to 30 g/dm3, in the solid phase of the technological mixture and in the gold-containing powder — from 3 to 80 wt. % with the relative error no more than ±5%. The gravimetric methods provide gold determination in the liquid phase of the technological mixture after gold reduction with hydrazine hedrochloride within the range of gold concentration from 0.5 to 500.0 g/dm3 with the relative error no more than ±1.3%. It is shown that the developed methods of analysis demonstrate good convergence of the results of analysis. The methods of analysis are certified by the Metrological Department of the enterprise and can be in a support technology of microelectronics production.
20-22 570
Abstract
Most of the errors in determining the trace contents of the elements are attributed to contamination at the stages of sample preparation and preparation of calibration solutions. One of the main sources of contamination is the laboratory air containing detectable impurities in the form of dust and aerosols. Reagents, dishes, dispensers and chemist himself may also act as sources of pollution. Background contents of the elements in a laboratory can be rather significant and lead to serious accidental and systematic errors, especially for wide-spread elements: Al, Si, Ca, Mg, Na, Fe, Zn, Cu, P, etc. A new development of the ANALIT company «Clean workplace» intended for sample preparation for trace spectral analysis is designed to solve the aforementioned problems.

PHYSICAL METHODS OF RESEARCH AND MONITORING

23-28 484
Abstract
Destruction of bodies is accompanied by formation of both large and microscopic fragments. Numerous experiments on the rupture of different samples show that those fragments carry a positive electric charge. his phenomenon is of interest from the viewpoint of its potential application to contactless diagnostics of the early stage of destruction of the elements in various technical devices. However, the lack of understanding the nature of this phenomenon restricts the possibility of its practical applications. Experimental studies were carried out using an apparatus that allowed direct measurements of the total charge of the microparticles formed upon sample rupture and determination of their size and quantity. The results of rupture tests of duralumin and electrical steel showed that the size of microparticles is several tens of microns, the particle charge per particle is on the order of 10–14 C, and their amount can be estimated as the ratio of the cross-sectional area of the sample at the point of discontinuity to the square of the microparticle size. A model of charge formation on the microparticles is developed proceeding from the experimental data and current concept of the electron gas in metals. The model makes it possible to determine the charge of the microparticle using data on the particle size and mechanical and electrical properties of the material. Model estimates of the total charge of particles show order-of-magnitude agreement with the experimental data.
29-34 534
Abstract
A contactless microwave method and corresponding information-measuring system (IMS) for determination of thermal and physical characteristics thermal and physical characteristics (TPH) of building materials and products are considered. The method provides microwave heating of the samples by exposing the surface of the sample to electromagnetic field of the microwave range through a circular area, as well as temperature control of the environment and in the center of the circle. A microprocessor-based IMS system developed for practical implementation of the proposed method provides determination of the thermal and physical characteristics of the objects under study with high accuracy. A possibility of on-line automatic control of all operations of the thermophysical experiment, as well as the control of heat losses to the environment from the surface of the circular spot subjected?? to microwave heating and the timely correction of those losses to improve the accuracy of the final results is a distinctive feature of the system. Analysis of the calculated and experimental data showed that the elimination of the impact of the contact thermal resistance arising between the surfaces of the sample and the heating element on the determination of the desired thermal characteristics increases the accuracy of the method by 6— 8 %. The developed method allows more accurate determination of the thermal characteristics compared to other known techniques and can be used in practice of general thermal measurements and thermal engineering for construction.
35-40 723
Abstract
The results of studying single-crystal turbine blades with a promising scheme of cooling, cast from a heat-resistant ZhS32 alloy using ceramic rods with high-temperature sintering additives and additional impregnation with a varnish solution are presented. The program of crystallizing blades with a single-crystal structure is improved on a VIP-NK installation. A comparison of the operation modes of the updated program and serial technology is presented. A pilot batch of blade castings is obtained under production conditions of a machine-building enterprise with an output suitable in single-crystal structure of about 94%. Blade castings are studied using X-ray diffraction, X-ray and ultrasound methods. Quantitative metallographic analysis is carried out on an optical complex to determine spacing between axes of the first order dendrites (λ1) of the alloy and the volume fraction of the micropores in the cross section of the pen and casting lock. The results of scanning electron microscopy study of macro-and microstructure of the blade castings with a promising cooling scheme showed that the structure is typical for ZhS32alloy in the cast state and is well formed in the elements of the inner cavity of monocrystalline blades.

MATERIALS MECHANICS: STRENGTH, DURABILITY, SAFETY

41-52 832
Abstract
The stages and results of fundamental and applied research regarding the problems of strength, resource, survivability and technogenic safety carried out at the A. A. Blagonravov Mechanical Engineering Research Institute of the Russian Academy of Sciences throughout a 80-year history are considered. Equations of state and criterion expressions regarding static and dynamic loading, high-cycle and a low-cycle fatigue resistance, high-temperature and low-temperature static and cyclic strength, stress-strain states analysis upon elastic and elastoplastic strain, problems of linear and nonlinear fracture mechanics are derived. The last decades have been marked by the development of basic research on the mechanics of catastrophes, survivability and man-made safety of machines and structures, including the results of complex developments in all the listed areas of strength and resource. The results of studying strength, resource and survivability are the basic components for the mechanics of catastrophes and risks in the technogenic sphere, as well as the new principles and technologies for technogenic objects ensuring their safe operation and prevention on a reasonable scientific basis emergency and catastrophic situations and°r minimize possible damages attributed to them. Diagnostics of the current parameters of the material state and determination of the characteristics of stress-strain states in the most loaded zones of the analyzed technical system is thus a tool for ensuring safe operation conditions. The solution to the problem of assessing the strength and resource in such conditions includes creation of generalized mathematical and physical models of complicated technological, operation and emergency processes in technical systems to analyze conditions of their transition from normal state to emergency or catastrophic states. It is shown that as the analyzed structure passes through admissible to limiting states thus causing the occurrence of failures and subsequent emergency and catastrophic situations, it is necessary to introduce into the regulatory calculations of such states an additional set of defining equations and their parameters characterizing these limiting states. Those calculations are based on the systems of criterion equations, including the parameters of risk, safety and security of the technosphere objects.
53-58 672
Abstract
Change of acoustic emission parameters is observed upon a single static loading of a flat metal specimen with the brittle strain-sensitive coating deposited on the surface. The activity of acoustic emission signals (their energy, number, and frequency) was recorded as the time of tensile loading increased. It is shown that upon further loading to the ultimate strength in the region of small elastic and elastoplastic deformations comparable to the yield stress deformations, the dislocation mechanism of deformation is attributed to the processes occurring at nano and micro levels with the corresponding frequencies of acoustic emission signals. The development of local deformations at micro- and meso-levels should be accompanied by a different signal structure when microdefects occur, with larger amplitudes and lower frequencies. Presumably, this occurs during formation of mesobreaks at the grain boundaries and in zones of large dislocation clusters. In this case the number of high energy signals should decrease at simultaneous decrease of acoustic frequencies. When tensile tests are performed on relatively coarse-grained steels of high strength and low ductility, then sound effects can be recorded even by human ear. In addition to the traditional analysis of these parameters, acoustic emission spectra have been constructed for given loading intervals. With the use of new integral parameters of those spectra, the gen- eral patterns of changes in the spectra from the region of higher to lower frequencies with increasing number of signals are shown. This fact indicates to oncoming of dangerous damaged state as the stresses increase in the coated aluminum sample. The generalized parameters of spectrum changes are presented. This provides a possibility to study the indicated features of elastic and elastoplastic deformation using spectral methods and new integral diagnostic parameters.
59-66 598
Abstract
A methodical approach to the estimation of the localization zone and geometric parameters of a delamination defect in layered composite materials is presented on the basis of mathematical processing of the experimental results of deformation measurements obtained with a grid of fiber-optic sensors. The results of methodological developments related to the determination of the optimal topology of the grid of sensors to ensure the detection of defects of a given size with the necessary accuracy and determination of their parameters are presented. We present methods for computational analysis and simulation of the strain-stress state in the defect zone, based on the algorithm used for modeling the problems of strain-stress analysis in the defect zone using 2D finite elements, instead of 3D ones, thus allowing the use a model of lower dimensionality and retain all the features of the stress-strain state. The results of methodological developments related to the determination of the defect parameters from the results of strain measurements using the methodology of solving the inverse problem, based on solving the problem of minimizing the discrepancy between the vector of deformation response and the vector of initial parameters are presented. The technique is implemented as a software consisting of a series of macros for ANSYS and programs for MATLAB. The results of cyclic testing of a sample from a multilayer CM with a delamination type of defect are presented. Estimation of the increment in the defect size upon loading is performed by mathematical processing of data recorded by fiber-optic strain sensors glued on one of the sample surfaces, based on the solution of the inverse problem. Comparison of the results of calculations of geometric parameters of the defects with the measurement data obtained by the method of ultrasonic flaw detection showed good agreement between them.

COMPLIANCE VERIFICATION. LABORATORY ACCREDITATION

67-78 1323
Abstract
Despite the fact that the global market for medicinal plants amounts to hundreds of billions of dollars, there is almost no government control over the quality of such pharmaceuticals in most countries of the world. This is partly attributed to the complex composition of plant materials: traditional analytical methodology is based on the use of standard reference samples for each analyte. In this case, preparations based on medicinal plants may contain tens and hundreds of physiologically active components. Isolation of those compounds in a pure form in practice is carried out using preparative chromatography, which leads to their high cost. Moreover, varying of the chemical composition of the medicinal plants depending on the geographical origin of the raw materials interfere with prescribing strict ranges of permissible contents for all physiologically active components. Combination of the above factors limits the possibilities of using traditional approaches to analysis, requiring strict standardization, the list of compounds for each type of plant, levels of contents and the availability of the reference materials and standards of comparison. This led to the study of the possibility of introducing various mathematical approaches as an auxiliary methodology. Unlike traditional methodologies, machine learning approaches are based on the correct collection of the data samples. Such a sample should contain groups of the samples that correspond to the states of the object which the developed algorithm must distinguish: authentic/fake, pure/containing impurities, effective/not containing a certain level of active components, etc. This review is devoted to consideration of the application of machine learning technique to the problems of chemical analysis and production control of raw materials of medicinal plants and preparations on their base for the last 15 years.


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