We consider four basic methods used for analysis of recoverable metal-containing raw materials: x-ray fluorescence analysis, atomic absorption spectrometry, atomic emission spectrometry with inductively coupled plasma, and mass spectrometry with inductively coupled plasma. The features of different methods are discussed taking into consideration the specificity of the recoverable raw material and methods of sample preparation harmonized with the method of analysis and sample composition.

The procedures atomic absorption determination of the total content of lead and zinc in biological samples (laboratory rats) are developed with allowance for microwave sample preparation of biological samples and assessment of toxic impact and developmental toxicity of lead and zinc compounds. The total content of lead and zinc range within 0.005 - 2500 and 1 - 300 pg/g, respectively, at the relative standard deviations not exceeding 0.15 (Pb) and 0.07 (Zn).

Voltammetric behavior of T-2 toxin on carbon-containing electrodes and the effect of composition and pH of the base (supporting) electrolyte on the value of the analytical signal ofT-2 toxin are studied. The optimum pH of background electrolyte ranges within 3.5 - 5.5. We evaluated the effect of chemical adsorption on the peak current ofT-2 toxin electroreduction (the share of chemical adsorption is about 70%) and specifies conditions of voltammetric determination of T-2 toxin. The correctness of the results is confirmed in spiking test, the error of determination within a concentration range of 0.05 - 60 mg/dm³ is 15 - 20 %.

A procedure of atomic-emission determination of zinc in polystyrene plastics is presented. Optimal conditions of spectra recording and spectral buffer composition are specified. The use of synthesized calibration specimens imitating a matrix of considered industrial samples provided reduction of the error not of analysis up to 15 % rel.

A technique of ionometric determination of molybdenum (VI) in etching solutions for molybdenum cores and plates used in lighting engineering industry is presented. A liquid electrode with a membrane based on nitrobenzene solution of tetradecyl chloride is used as an indicator electrode. Conditions of analysis are optimized. Multiple excesses (100-fold excesses of Zn²⁺, Mg²⁺, Co²⁺, Mn²⁺, Fe²⁺, Ni²⁺ and 5-fold excesses of Cu²⁺, Fe³⁺) do not interfere with the determination of molybdenum (VI). The interfering effect of ions increased in series: SO₄^2- < - - 2O₇^2- < WO₄^2- < Br^- < NO₃^- < I^-. The relative standard deviation in determination of molybdenum (VI) at a level of 3.0 • 10⁵ mol/liter is not more than 0.05.

The effect of supersonic vibration on the spectrum of dielectric losses is studied for electrical engineering and laser materials with proton conductivity. Simulta neous impact of ultrasonic vibrations, alternating electric field and temperature results in absorption of ultrasonic vibration quanta. The width of the potential barrier pulsates and is reduced by 2 - 3.5% thus making proton tunneling more probable. We propose a non-destructive method of quality control and determination of condition of crystalline materials and adhesive joints of the materials with a proton type of conductivity, the time of analysis being dramatically decreased from 14 - 28 days (according to GOST 12175-90) to one hour.

A mechanism of curve formation in high-resolution x-ray diffractometry is presented. Rule given for calculating the intensity of which is recorded by the detector. Angular positions of peaks attributed to reflection from monochromator, sample and analyzer are determined. Diffraction scattering in a reciprocal space and the principles of construction are considered. A scheme of the two-dimensional intensity distribution near a node of the reciprocal lattice of the crystal is presented along with a detailed description of the adjustment of three - axis diffraction scheme. An emphasis is made on the difference between the zero position of the diffraction pattern, the origin of the reciprocal space and node of the reciprocal lattice. Considered sequence of forming contours of equal intensity of diffuse scattering is used for determination of the morphology of the samples. The pore size and orientation in lead telluride formed upon electrolytic etching are determined. Defect formation in the samples is also evaluated both before and after etching.

Calculation of the distribution function of grain orientations (ODF) from the experimental data is one of the major problems of mathematical texture analysis. Currently, there are a large number of methods and software solutions aimed at the problem of ODF recovering. One of them is ODF approximation by “standard” functions on the rotation group. Normal distributions (ND) on SO (3) are used, inter alia, as “standard” functions. Central normal distributions (CND), characterized by the circular nature of scattering with respect to a given orientation, are calculated most simply. We propose a method of ODF recovery by a set of individual orientations using approximations by normal distribution on SO (3). We present an algorithm for recovering the parameters of normal distribution in the case when orientations are divided into separate clusters: position of the “center”, sharpness and weight. Numerical examples of the recovery procedure are also presented.

EBSD (Electron Backscattered Diffraction) is well-known method for phase analysis of micro-sized objects. EBSD detector is produced as an accessory for a scanning electron microscope. The spatial resolution of EBSD is approximately 30 nm, so this is very attractive method for local phase determination and quantitative texture analysis. Appropriate sample preparation is critical for using of EBSD, but that preparation depends on material of a sample and can be laborious. It was suggested to use an ion column of a FIB/SEM dual platform instrument for EBSD sample preparation. That method is uniform and very straightforward as compared with traditional methods of sample preparation for EBSD. And this is the only way for handling with unique micro-objects because all other methods require doing final polishing of the whole sample surface. The unique micro-object can disappear after such polishing. Also suggested method is the only way if general polishing of a sample is forbidden.

We present a methodology and results of experimental study of the mechanical properties of carbon steels in cold-formed profiles used in frameless buildings. The profiling technology provides two-stage cold bending of steel bars: i)rolling of a straight profile, and ii) rolling of a curved profile using trandverse corrugation of corresponding faces whereby the initial material undergoes two stages of strain hardening. Both straight and curved (arched) profiles are considered. The standard mechanical properties of steel are determined. The results of experimental studies demonstrated that the material of the corner site of the profile gains additional strengthening resulted from transverse corrugation: the mechanical strength of stell increases, whereas the ductility undergoes significant reduction.

A method and results of using pendulum scribing for comparative qualitative rapid assessment of physical and mechanical characteristics of the tool and other materials, as well as operational properties of the tool made from those materials are presented. A correlation between those characteristics and parameters of pendulum scribing trace is demonstrated thus providing simplification and reduction of the quality assessment cost for novel materials to be developed.

A method of qualitative assessing of the parameters of shape memory effect and superelasticity of NiTi alloys based on analysis of the physical and mechanical properties and temperature dependence of the martensite shear stress of titanium nickelide are presented. It is found that the experimental temperature dependencies of the shear stress of martensite provide determination of the level of the mechanical properties, parameters of the shape memory effect, superelasticity, and allocate the intervals of shape recovery under the effect of both temperature and strain. The method also makes possible to reduce time of analysis for titanium nickelide based alloys and get almost complete picture of their deformation behavior upon martensitic transformations.

Development of the Association of analytical centers “Analytics” in its 25-year period in existence in Russia is described: background, main activities, participation in formation of the Russian System of accreditation of analytical laboratories, membership in the International organization for accreditation (ILAC), participation in the development of metrology and analytical control. List of winners of “Silver mole” (the award constituted by the national Association for the best national laboratories) is presented. The results of years of work of the Association for the accreditation of the Russian laboratories and development of metrology of chemical analysis are evaluated along with relevant challenges to address in the forthcoming work.

A device for measuring the dispersion of capillary diameters in multichannel tubes (MCT) used as a source of raw material in production of multicapillary columns is described. Principle of operation consists in correlation between the capillary diameter and time of non-sorbing compound passage through the capillary, i.e., using the parameters of a chromatographic peak of non-sorbing compound run through the MCT (methane). With equal capillary length and pressure difference across the capillaries, the flow rate of a carrier-gas and, hence, of methane sample definitely correlates with the capillary diameter, thus providing determination of the dispersion of the capillary diameters of the MCT from the variance of time of the methane passage through the capillaries. The device is a chromatograph operating at room temperature provided with a system of quick gaseous sample injection, flame-ionization detector, gas unit and recorder. A distinguishing feature of the device design is a possibility of attaching MCT of different length (50 - 1200 mm) and diameter to the sample injector (SI) and detector, due to mobility of SI and quick-detachable fittings of various standard sizes. The characteristics of the device: the accuracy of measurements is about 3%, correction for contribution of the methane peak of exrtacolumn broadening σ² ec = (7.21 ± 0.24) x 10⁴ sec². Examples of measurements performed for different batches of multichannel tubes are presented.