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Industrial laboratory. Diagnostics of materials

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Vol 82, No 10 (2016)

SUBSTANCES ANALYSIS

5-16 717
Abstract
High performance liquid chromatography-mass spectrometry with ionization at atmospheric pressure is one of the most sensitive and selective methods, though, being an analytical technique, it is also greatly subjected to matrix-related effects. Suppression of analyte ionization by matrix components (IS) is one of the least understood and most unpredictable manifestation of the matrix effects in HPLC-MS analysis. As IS can greatly affect the main characteristics of the method - the detection and quantification limits, precision, and reproducibility - evaluation of the contribution and allowance for IS appeared rather important upon development and validation of the methods of analysis. Considerations on the origin and mechanisms of ionization suppression and brief review regarding the major approaches to identification, minimization, and accounting of IS effect in measurements are presented.
17-21 474
Abstract
The trace element concentrations in four oils from different fields of the Russian Federation (Arlanskoe, Labaganskoe, Priobskoe, Romashkinskoe) are determined using ICP-MS. Sample preparation is carried out using two procedures: microwave decomposition of oils (in determination of Be, Na, Mg, Al, S, Ca, Ti, V, Cr, Co, Ni, Cu, Zn, Ga, Se, Rb, Sr, Zr, Mo, Cs, Ba, W, Re, U) and extraction concentration with rotating coiled columns (RCC) (in determination of Nb, Ru, Rh, Ag, Cd, Sb, Te, Hf, Ir, Pt, Tl and rare earth elements in oils. The use of RCC provides concentration of trace elements in oil and thus significantly improve the detection limits of ICP-MS.
22-25 310
Abstract
Combination of Data Mining algorithms (clustering and regression tasks) proposed for determination of a limited number of analytes in the samples of complex chemical composition with an unknown matrix provides elimination of the impact of host environment components on the intensity of analytical lines of the element to be determined. The developedprocedure is tested in XRFAdetermination ofS, Fe, Cu, Zn, and As in the samples of flotation concentrate obtained upon processing of polymetallic ores and V and Fe in synthetic film samples close in their physicochemical properties to welding aerosols accumulated on a filter. The error of analysis decreased by a factor of 1.5 - 5 compared to classical Lucas - Tooth regression equation. The developed procedure significantly shortens time of analysis on an x-ray sequential spectrometer.
26-28 465
Abstract
The technique of spectrophotometric determination of molybdenum in ferrous and non-ferrous alloys based on the reaction of Mo interaction with bromopyrogallol red with cationic SAS (cetylpyridinium chloride) present is developed. Molybdenum determination in a highly acidic solution does not require strict adherence of pH balance and excludes errors attributed to small changes in the acidity of the environment. The technique is highly selective and does not require additional operations to eliminate the interfering effect of associated components, including the presence of tungsten element-analogue. The technique is rapid and the available as for reagents and equipment thus used. The convergence and accuracy of the results are rather high.

STRUCTURE AND PROPERTIES INVESTIGATION PHYSICAL METHODS OF INVESTIGATION AND MONITORING

29-32 576
Abstract
The size of the radiation source focal spot affects the image quality upon x-ray control of the objects. Prolonged use of x-ray tubes changes the size of the focal spot. Thus, both domestic and foreign regulatory documents contain requirements regarding a recurrent control of the focal spot of the radiation source which is rather time-consuming operation. Usually, the spot image obtained on a high contrast radiographic film is measured with a measuring magnifier or comparator. The method is inaccurate, since it suggests manual scanning ofthe image with a given step. Apossi bility of measuring the spot size using analysis of a digital radiographic image of the spot on a monitor of the digital radiographic unit and method of calculating adjustment factors are demonstrated.
33-36 314
Abstract
Thermoactivation current spectroscopy is used to study crazing of polyethylene terephthalate fibers upon their orientation stretching. It is found that each stage offiber crazing is characterized by specific temperature ranges of extrema location in the spectra of thermally stimulated currents, and crazing is accompanied by the competing processes of redistribution and relaxation of the electret charge. Thus, thermoactivation current spectroscopy can be used to assess microdeformation changes in the structure of polymer dielectrics.
37-38 327
Abstract
The use of a capillary viscometer with a measuring needle as working medium providing accurate viscosity measurements of small volume of low transparent liquids is discussed. Operating principle of the viscometer is described. A working formula of the viscometer is derived proceeding from Stokes equation. Presented results of water viscosity measurements in a range of 25 - 70°C match the referenced data. Pressure distribution over the perimeter of the perpendicular section of working medium (cylindrical needle) is analyzed as a function of the needle shift from central position on a capillary axis. Self-focusing mechanism of the measurement system is demonstrated.
39-43 835
Abstract
Thermal simulation of temperature fields is used to increase the accuracy of determining dielectric permeability of materials in high temperature waveguide resonator with allowance for the impact of inhomogeneous temperature distribution. Experimental results of measuring the temperature dependence of the dielectric constant e(T) of solid samples of silicon dioxide (up to 1668 °C) at microwave frequencies are presented. The value of e(T ) is shown to range within ±2% of the initial value throughout the whole temperature interval.

EXCHANGE OF EXPERIENCE

MECHANICAL TESTING METHODS

47-55 849
Abstract
We present an ultrasonic technique for determination of the physical and mechanical properties of polymer composite materials (PCM) using a complex parameter including the value of the ultrasonic pulse velocity in the plane of the article and frequency value of the main spectral component of the ultrasonic pulse got through the article back and forth. We also propose to assess the degree of accumulation of the microdamages to PCM by their mechanical characteristics (e.g. tensile interlaminar shear and compression strength), determined by nondestructive method. A degree of microdamage accumulation in polymer composite materials can be assessed using their mechanical characteristics (e.g., strength upon interlaminar shear and strength upon compression) determined by a non-destructive method. We also consider a fundamentally new informative diagnostic parameter characterizing the decay of ultrasonic waves in materials: frequency of the main component of the spectrum of ultrasonic pulse passed through the article in forward and backward directions. It is shown that for destruction diagnostics of the material it is advisable to excite a longitudinal wave and a wave similar to a zero-order symmetrical wave.
56-61 535
Abstract
Mechanical tests for stretch ing are carried out on ring specimens (2 mm heigh on 4 -mm cylindrical posts). Processing of the resulted machine stress-strain diagrams in coordinates of displacement of the active capture of the testing machine - force provides determination of the value of the conditional yield strength of the material with a 1.1 % tolerance for the residual deformation.
62-65 306
Abstract
A universal device for tribotechnical tests of materials and coatings is presented. An example of its practical realization in a prototype is given. Methods of calibration of the measuring systems of the device are described. Ratios for estimation of the average contact pressure and friction distance are determined for a number of renewable joints used in the device in tests for wear and friction. Testing of the prototype showed a reasonable accuracy of the constituent measurement systems, versatility and economic efficiency of the device
66-70 601
Abstract
A problem of experimental determination of the physical and mechanical characteristics of aramid torsion bars (D = 0.046 mm) is considered. An emphasis is made on the choice of test procedure for tensile testing of such materials. In Russia tensile tests of aramid yarns are performed according to standard GOST 6611.2-73 “Textile threads. Methods for determination of breaking load and elongation upon rupture.” However, this standard has been developed before the onset of aramid yarns production in Russia. Current international standards used for tensile testing of aramid yarns are analized. Standard ASTM D7269/D7269M-11 is selected as the most suitable. The main principles of standards ASTM and GOST are considered and analyzed.
71-77 366
Abstract
We developed an alternative to summation score method for assessing the results of expert evaluations. The method is based on representation of the objects to be examined in the form of points of multidimensional space in a coordinate system with axes corresponding to experts estimations, the dimension of the space being equal to the number of experts. A distance to the object with the best possible estimations (according to the rule: the smaller the distance, the preferable object) is used as a criterion for final evaluation of the objects with a possibility of their further ranking according to the degree of preferences. For example, expert estimations of tasting wine demonstrated that the developed method is more representative and mathematically justified compared to traditional aggregation of points.
78-81 411
Abstract
The activity and developmental landmarks of the Central Fire Assay Laboratory (CFAL) of the Analytical center of LLC “R&D and manufacturing company “Regis” (Blagoveshchensk) are presented. The laboratory was honored with the “Silver mole” award in 2012 and in December 2014 celebrated the tenth anniversary of the lab foundation. Over the past decennial period an ordinary assay lab turned into a multifunctional center focused on comprehensive analytical support to geological exploration, mining, geology and geochemistry, mineralogy, civil-engineering survey, and environmental monitoring. Despite a large scope of analytical work and remoteness from the center of the country, CFAL provides methodological assistance for industrial laboratories of the relating group of companies. Stages of the development, structure and guidelines of lab activities as well as the quality management system are considered. An emphasis is made on the development of the methodology of quantitative chemical analysis (QCA) and availability of standard samples, hiring and training of the assay lab personnel.


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