Two approaches to improving the resolution of electron-probe x-ray spectral microanalysis of the nano-particle composition are considered. The first approach is based on the use of low (less than 5 keV) energy of the probe electrons and characteristic radiation of the detected elements as analytical x-ray lines of L- and M-series. The second approach is based on the use of a part of the analytical signal attributed only to excitation by probe electrons. The lateral and longitudinal resolution thus attained are about 2 nm and 20 - 60 nm, respectively, the minimum detectable mass of the substance corresponds to 10-30 atoms of the elements to be determined.

New data on determination of rare-earth elements (La, Ce, Nd, Eu, Sm, Gd, Yb), Y and Sc in geological samples with an increased lanthanide content are presented. The results are obtained using arc atomic emission spectrometry using a multichannel spectrum analyzer capable of recording atom and ion radiation on photodiode crystals. The accuracy of REE content determination is assessed by comparison with ICP-MS (inductively coupled plasma mass spectrometry) data. Correctness of the results obtained for yttrium and scandium is confirmed by consistency with the characteristics adopted in the International Program for Professional Testing of Geoanalytical Laboratories GeoPT. The study is carried out on scientific equipment of the Center for Isotope-Geochemical Studies of the Institute for Geochemistry, Siberian Branch, Russian Academy of Sciences.

Gas chromatography-mass spectrometry is used to study the impurity composition of germane, isotopically enriched with germanium⁷²Ge to 99.953 %at. For the chromatographic separation of impurities, we used quartz gas-adsorption capillary columns GS-GasPro 60 m х 0.32 mm with modified silica gel, CarbonPlot 25 m х 0.32 mm х 0.25 pm with a carbon sorbent and 25 m х 0.26 mm х 0.25 pm with polytrimethylsilylpropyne. Identification of the impurities was carried out by comparing their mass spectra with the mass spectra of NIST database, using literature data on the retention time and mass spectra of germanium-containing substances. The impurities of permanent gases, xenon, krypton, nitrous oxide, carbon dioxide, silane, hydrocarbons C₁ - C₈, aromatic, chlorinated and fluorinated hydrocarbons, homologues of germane, methylgermane, chlorogermane, carbon disulfide, carbonyl sulfide, 1,4-dioxane, difluorodimethylsilane are identified in different fractions of⁷²GeH₄ obtained during rectification. Impurities of xenon, krypton, carbon disulfide carbon oxides, 1,4-dioxane and difluorodimethylsilane have been identified in germanium for the first time. The impurities of carbon disulfide, krypton and xenon exhibit shifted isotopic composition while the impurities of methylgermane, homologues of germane and chlorogermane, as well as the main component are isotopically enriched. Quantitative determination of the impurities is carried out in the mode of selected ion monitoring (SIM) using the mass numbers with the maximum signal-to-noise ratio. The impurity concentrations are determined by absolute calibration of peak areas using self-prepared and certified calibration mixtures. In the absence of reference samples, the impurity concentrations are determined from the dependence of the coefficients of detection sensitivity on the value of the total ionization cross section. Detection limits calculated by tripling value of the standard deviation of a signal in the “blank” experiment range within 1 x 10⁵ - 5 x 10⁸ % mol.

We developed a method ofchlorine ionometric determination using solid state membrane chloride-selective electrode in the samples of solid mineral fuels: gas coal and semi-coke. The accuracy of the method is evaluated. Correctness of the determination is confirmed by variation of weighted amount. The results obtained by ionometric determination of chlorine are compared with the rated values of chlorine content in solid mineral fuels.

Polymer resins of three classes (cyanate ester, epoxy and diphthalonitrile) are used to compare polymerization indices determined for different stages of cure using IR-spectroscopy and differential scanning calorimetry (DSC). The value of the cure degree (CD) determined by DSC is shown to be higher than that obtained by IR-spectroscopy, the difference in some cases exceeding 25%. The error of determination for different resins essentially depends on the method thus used up to complete invalidity and nonapplicability of DSC to CD determination for phthalonitrile resin. The fundamental methodological difference between polymerization indices determined by IR-spectroscopy and DSC is shown. IR spectroscopy (and other spectroscopic methods) provides information about the degree of component conversion and none about the possibility of further continuation of the reaction, whereas DSC method characterizes the cure process without a possibility of direct evaluation of the component conversion. Despite the identical definition those indices are not interchangeable but supplementary. We recommend to determine CD indices by different methods for complete and correct description of polymer resin condition.

Assignment of the aircraft service life is based on the determination of the physical and mechanical characteristics of materials. Testing of the materials with allowance for fail-safe concept should be carried out under simultaneous exposure of the samples to mechanical loads and external impacts. To increase the accuracy of experiments we propose to use acoustic emission for nondestructive testing of the samples.

Improvement of nanotechnological methods of treating optical components and optielectronic devices provides application of innovation coatings based on oriented carbon nanotubes (CNT) for surface modification. The modified surface of safety glass and optical elements of spectral devices prevent the impact of low-voltage spark on the optical elements, thus increasing their lifetime and improving the quality of the device operation. We present a new method of coating optical elements of the devices aimed at protection and improvement of the transmittance of the optical system. A laser method and experimental scheme of simultaneous application of nanocoatings to 6 pieces of the spectrometers are presented. An example of the experimental scheme with a built-in metallic mesh which provides optimal conditions of laser treatment is considered. Data on the change in the transmittance spectrum of the nanostructured CNT specimen valid for emission spectrometers with a working wavelength ranging from 175 to 400 nm illustrate an increase in the transmittance spectrum attributed to CNT-induced surface modification. It is important that indicated spectrum range is characteristic for the internal elements of optical emission spectrometers.

Four well-known methods for constructing phase diagrams of three-component systems are considered (two methods of Roseboom parallels, the Gibbs perpendicular method and a universal vector method that allows constructing phase diagrams with an optional number of components). A new method for constructing phase diagrams of ternary systems, i.e., method of diagonals is based on the statement that the triangle diagonals divide the sides in the same proportions in which the components are present in the composition, so that the point of their intersection can be considered a figurative point of the composition. The method exhibits clear advantages in rapidity, useability and handling compared to the known methods regarding both construction of the phase diagrams and determination of the compositions attributed to corresponding figurative points of the system.

White wines of four wine-growing regions of the Krasnodar Territory were studied using the ISP-AES method. We have analyzed concentrations of 19 elements in 153 samples of white wines of Chardonnay, Riesling, and Muscat. Statistical analysis of the result demonstrated that despite complex technological cycle of wine production (soil - grapes - juice - wine) the microelement composition provides information about the grape variety and region of origin. Probabilistic statistical models are constructed to identify the grape variety and the region of growing proceeding from the concentration of a certain set of trace elements contained in the wine. The proposed models are based on the assumption that the soil origin is an important factor affecting the microelement composition of the wine.

The problems of estimating the minimum allowable values of the extended uncertainty of measurements are considered for typical methods of calibrating passive instruments (measures) and measuring devices. Recommendations regarding the necessity of indicating the minimum allowable values of the extended uncertainty of measurements upon calibration are specified for calibration laboratories which present data on their calibration and measurement capabilities. The results obtained can be used by the personnel of calibration laboratories.

Dependence of the residual resource on the amount of micropores formed in conditions of prolonged aging of cast steel 15Kh1M1FL under stress conditions and high degree of damage with micropores is determined. Two series of cylindrical specimens are also tested for long-term strength: circumferentially notched and smooth specimens. The resource factor K_t is determined for operation conditions [stress (50 - 80 MPa) and temperatures (520 - 560°C)] by comparison of the calculated durability of the notched specimens of other series with a lower depth of the notches than that in tested specimens and durability of the smooth specimens. Using the results of studying pore formation we revealed a quantitative correlation between the impact of the microdamage severity on the lifetime and relative damage of the section of a circumferentially notched cylindrical specimen. Temperature and stress dependence of K_ô in the working range of loading conditions is studied for notched specimens. The type of damage at which further operation should be terminated is determined. It is found that the same stage of damage of steel 15Kh1M1FL must be simulated by a deeper notch than that in steel 12Kh1MF.

A technique for determination of the wear resistance of the surface layers of rubbing frictional pair is presented. The layers were obtained by different methods of hardening, including coatings applied by the plasma bake on procedures both in conditions of the steady-state friction and upon of acceleration or deceleration of the frictional pair. The method is based on determination of the wear and antifriction properties of cylindrical disc-type specimens, one of them is the reference one, and the other is hardened under conditions of rolling and sliding friction at a normal temperature. The error of measuring the friction coefficient is 0.5%. To increase the wear resistance of the machine parts, a large number of methods aimed at strengthening the material are used: thermal hardening, surface-plastic deformation, alloying of the workpiece material, additional machining, depositing of special, wear-resistant coatings on the surface of the part upon manufacturing or reconditioning. Experimental studies of the wear resistance of the coatings recovered by plasma selective baking demonstrated that the developed technique is advantageous for high accuracy and can be successfully used for evaluation of the quality of coatings.

Review and analysis of the data regarding the study of friction in rolling bearings revealed that the experimental equipment and traditional testing procedures thus used cannot guarantee strictly controlled conditions of testing. The developed design of the friction machine and method of testing provide a precise ranking of radial bearings and liquids by the value of the friction coefficient. Experimental dependences of the friction coefficients in single-row radial ball bearings on the rotation frequency of the inner ring are determined. It is shown that a high-quality bearing can be used as a tribotesting device in solving the continuum problems (contact, elastohydrodynamics, microhydrodynamics, rheology, etc.).