SUBSTANCES ANALYSIS
A discussion of the prospects for creating a multi-element atomic absorption (AA) spectrometer leads to the conclusion regarding the expediency of using spectral devices of relatively low resolution. Previous studies showed that the spectrometer with instrumental bandwidth 0.12 nm equipped with a CCD detector could provide the absorption measurements within a wavelength range of 200 – 400 nm using low-noise radiation sources, e.g., deuterium or low current xenon lamps. The rate of data acquisition was sufficient for vapour spectra monitoring during the pulse atomisation in graphite furnace atomizer. The loss in sensitivity due to low resolution is compensated by the possibility of direct determination of several elements in a single liquid or powder sample. Feasibility of multi-element simultaneous AA spectrometry depends on the efficiency of atomization technique and technology of data processing. The concurrent problems are discussed by the example of new calculation algorithm and its application to the analysis of multi-element nitrate and halogen containing reference materials. It is shown that linearization of the calibration curves for about 10 – 15 elements, which are not subject to chemical impacts, can be carried out automatically in a concentration range up to 4 – 5 orders of magnitude with 5 – 10 % deviation from the linearity at the ends of the interval. For the elements forming stable molecular compounds further improvement of the atomization technique is required.
An approach to detection of triterpene glycosides in ginseng extracts is developed using high performance liquid chromatography/mass spectrometry (HPLC-MS). Enhanced selectivity compared to commonly used HPLC-UV techniques provides simultaneous registration of chromatographic peaks and determination of 23 major and minor ginsenosides. For this purpose, in addition to the use of highly selective MS detection of adduct ions of sodium ginsenoside molecules and fragmentary sapogenin ions, special conditions of chromatographic separation on a sorbent modified with pentafluorophenyl (PFP) groups were specified. The effect of column temperature and mobile phase composition on the separation selectivity of glycosides was also studied. Though we failed to achieve complete chromatographic separation of the peaks for several compounds (F4 and Rg6, Rk3 and Rh4), their determination appeared possible in case of their joint attendance due to registration of the signals that differ in the value of m/z ratio. For all studied compounds, the linearity ranges and calibration equations along with the metrological characteristics such as the detection limit and reproducibility were determined. The developed approach was tested in standardization of the reference extracts of Asian (P. ginseng) and American (P. quinquefolius) ginseng roots. For some ginsenosides, the content declared by the manufacture did not match the actual content, but for others the concentrations were close to the declared values. Moreover, we managed to expand the range of ginsenosides under control which is rather important for their use in medicine.
MATERIALS MECHANICS: STRENGTH, DURABILITY, SAFETY
The cycle configuration at two-frequency loading regimes depends on the number of parameters including the absolute values of the frequencies and amplitudes of the low-frequency and high-frequency loads added during this mode, the ratio of their frequencies and amplitudes, as well as the phase shift between these harmonic components, the latter having a significant effect only with a small ratio of frequencies. Presence of such two-frequency regimes or service loading conditions for parts of machines and structures schematized by them can significantly reduce their endurance. Using the results of experimental studies of changes in the endurance of a two-frequency loading of specimens of cyclically stable, cyclically softened and cyclically hardened steels under rigid conditions we have shown that decrease in the endurance under the aforementioned conditions depends on the ratio of frequencies and amplitudes of operation low-frequency low-cycle and high-frequency vibration stresses, and, moreover, the higher the level of the ratios of amplitudes and frequencies of those stacked harmonic processes of loading the greater the effect. It is shown that estimation of such a decrease in the endurance compared to a single frequency loading equal in the total stress (strains) amplitudes can be carried out using an exponential expression coupling those endurances through a parameter (reduction factor) containing the ratio of frequencies and amplitudes of operation cyclic loads and characteristic of the material. The reduction is illustrated by a set of calculation-experimental curves on the corresponding diagrams for each of the considered types of materials and compared with the experimental data.
MATHEMATICAL METHODS OF INVESTIGATION
A new known modification for simulation of annealing to search the global extremum of the functions of many variables uses the fact that the function when n → ¥ converges to the δ-function concentrated at the point of global maximum of f(x). The case when the function has many equal extrema is discussed in detail. Problems of this type are often present, particularly in the design of regression experiments. Here we introduce the reader to an extremum search method that is effective in solving a wide range of applied problems, and also illustrate the use of the method in some of the simplest problems of designing the regression experiments. The proposed modification of simulated annealing uses quasi-random search at the intermediate stages. This is not the most rapid, but very reliable method which provide a complete exploring of the function domain. When solving numerical examples, the so-called exact D-optimal designs are constructed, which are very difficult to be obtained by other methods. Although with the increase in the number of variables, the complexity of the method (as well as the complexity of other well-known methods) increases dramatically due to an increase in the order of the determinant, the proposed algorithm is simple, reliable, and easily parallelized. It is known that the gain from using optimal designs in some cases can justify any computational costs of developing those designs. Using the described technique, the reader will be able to construct (even using the laptop capacity) the optimal designs in different areas at moderate values of the parameters (for example, for quadratic regression for s variables in variables for s ≤ 10).
STRUCTURE AND PROPERTIES INVESTIGATION
ISSN 2588-0187 (Online)