Analysis of biomarkers in wastewater is increasingly seen as an important tool for valuation of health, nutrition and use of various substances by humans. Some biomarkers are used for population estimates, since the actual values of population size in cities can differ significantly from official counts, which inevitably leads to errors in assessing the impact of various factors to people calculated per capita. 5-hydroxyindole-3-acetic acid (5-HIAA) is the main metabolite of serotonin, which is excreted by urine and can be used as a biomarker for population estimates. The determination of this metabolite is more preferred than the detection of serotonin itself in terms of correctness of the results. A technique of extraction and subsequent quantitative determination of 5-HIAA in wastewater by high-performance liquid chromatography in combination with tandem mass spectrometric detection was developed. Poroshell Hilic column was used as a stationary phase which has an alternative selectivity compared to traditional C18 columns. Developed procedure is characterized by low detection limits (0.2 μg/liter) and good selectivity. The conditions for liquid-liquid extraction of 5-HIAA from wastewater were selected. This technique provides reliable estimation of the concentration of 5-HIAA in wastewater.

A methodical approach to reduction of the limit of uranium and thorium detection in antique lead is proposed. The approach includes separation of the elements in the extraction system based on tetraphenylmethylene diphosphine dioxide and their subsequent ICP-MS determination. The influence of phase contact time, medium acidity, concentration of the extractant on the extraction of uranium and thorium from nitric acid solutions was studied under conditions of batch extraction. It is shown that the matrix element (lead) is not recovered in the considered extraction system. We specified and optimized conditions for concentration of uranium and thorium and their elution with an aqueous solution of etidronic acid using countercurrent chromatography. The content of uranium and thorium in the sample of antique lead raised from the ocean floor are less than 10^–10 % wt.

A method of aluminum, hafnium, iron, yttrium, calcium, magnesium, and titanium determination in yttria-stabilized zirconia (YSZ) by inductively coupled plasma atomic emission spectrometry (ICP-AES) is described. Conditions for the decomposition of two modifications of the analyzed material — unburned and subjected to stabilizing firing — were studied. It was found that the unburnt zirconia dissolves well in sulfuric acid, and the conversion to the solution of the burnt sample is possible only with fusion with potassium pyrosulfate or potassium bifluoride, but using of these reagents leads to high values of the control experiment correction for trace impurities (at the level of tenths and hundredths of a percent). In this connection, we studied the possibility of acid dissolution of a burnt sample under microwave decomposition, varying the qualitative and quantitative composition of the acid mixture, the reaction temperature, the time to reach and to maintain the required temperature. It was found that the decomposition in the mixture of hydrofluoric and sulfuric acids (2:1) in the microwave system with stepwise heating of the reaction mixture ensures quantitative dissolution of the burnt sample and sufficiently low values of the control experiment correction for microimpurities. The analytical lines were chosen taking into account their relative intensity, possible spectral overlaps, and the matrix effect in the analysis of model solutions containing 1.3 mg/cm³ Zr, 0.2 mg/cm³ Y and from 0.2 to 20 mg/cm³ impurities. As a result, the following analytical lines were chosen: Al II 167.079 nm and Al I 308.215 nm; Ca II 184.006 nm and 393.366 nm; Fe II 238.204 nm; Mg II 279.553 nm, Ti II 334.941 nm, Y II 371.030 nm and Hf II 232.247 nm. The developed method for the analysis of yttria-stabilized zirconia (YSZ) by the ICP-AES allows simultaneously determining aluminum, iron, magnesium and titanium in the range of 0.01 – 1.0%, calcium — 0.02 – 1.0%, hafnium — 0.1 – 5.0% and yttrium — 2.0 – 15% with a % rel. (Y). The correctness of the method is confirmed by the standard addition technique.

A unified technique of AES determination of the impurities in platinum-rhodium alloys is presented. A distinctive feature of the technique is the possibility for analysis of the alloys of the grades not determined by GOSTs, which are widely used in industry. Almost no standard samples (their development is a long and expensive process) are available for such alloys. The technique provides determination of the impurities in platinum-rhodium alloys with rhodium contents of 0.1% – 35 % wt. without using an adequate standard sample for each particular alloy. The unified technique of AES determination of silver, gold, copper, iron, nickel, lead, palladium, antimony, tin, zinc and other in platinum-rhodium alloys (containing up to 36% of rhodium) is thus developed. Certified standard samples were used to plot the calibration curves. The accuracy indices of the developed unified technique are not inferior to those of the procedures developed earlier for platinum and platinum – rhodium alloys.

Current state and prospects of computerization of laboratories are considered. An exponential growth in the speed and storage space of computers, as well as their cheapening obey «Moore’s law». The use of computers in laboratories has become commonplace, the corresponding programs are being improved and become more accessible. Programmers have ceased to think about computer speed and memory savings. Operations are executed instantly, and laboratory information gained throughout many years can be saved on a common hard disk. In addition to general-purpose programs such as Word or Excel a number of the software of special duty are developed and widely used: LIMS (Laboratory Information Management System) and special computer programs. Each LIMS is a consistent program. The laboratory may use several special programs, each of them being focused on a certain type of activity («computerization by blocks»). Those types of programs are used most often because of their simplicity, convenience and low cost. QControl and DControl programs are most common inRussia. All kinds of programs become more and more accessible. Computerization also touches the metrological aspects of the laboratory activity. Correctly written program provides using modern approaches (including complex statistical calculations, Shewhart charts, etc.) almost without special staff training. By entering the results of measurements into the computer and pressing the desired key, the lab technician performs data processing (including calibration and acceptance testing) and control of the stability of measurements, and, if desired, validation and verification of the procedure. In the foreseeable future, computerization will cover almost all laboratories, with specialized programs and simple LIMSs prevailing. The widespread introduction of metrological and other innovations will occur through their incorporation into computer programs.

A method of automated diagnostics of critical lined equipment is improved using a neural network to recognize the thermograms and classify the burnout zones. The proposed method provides an increase in the reliability and promptness in determination of the lining burnout zones and their qualitative assessment. The information signs used for analysis and recognition of the lining burnout zones on a thermogram image are considered. The results of using neural networks with different configurations to minimize the error of classifying the levels of the burnout and determining the optimal number of the learning epochs are presented. The developed automated system for technical diagnostics of critical lined equipment, including the software for analysis and recognition of the thermograms, was evaluated and implemented at the enterprises of metallurgical production. Comparative analysis of the results obtained using the developed automated system and traditional system of diagnostics demonstrated the advantages of the developed method.

Modern requirements to the quality of materials entail the necessity of refining methods for their control and developing various procedures for analysis of the state of the surface with the goal of having defect-free structures for high-precision instruments and devices. Gas-discharge visualization of the defects at atmospheric pressure consists in obtaining bright plasma formations in the vicinity of the surface with a defect against the background of a weak glow of the air plasma in electromagnetic fields of high strength. The potentialities of plasma technologies regarding testing the surfaces of solid materials for various kinds of defects using a self-sustained dielectric barrier discharge (DBD) at atmospheric pressure are considered. The developed rapid technique provides quick rejection of defective materials or samples prior to their technological use. A set of diagnostic tools and auxiliary equipment has been developed to visualize the mechanical defects of different origin and evaluate the quality of raw materials. A number of important issues are considered when controlling the quality of high-grade surfaces, transparent and opaque materials, including metal surfaces. The special attention is paid to the search for defects in the structural elements of industrial equipment and determination of the degree of moisture of fibrous structures, for example, woven materials.

We present the results of studying the structure and structural transformations in the surface layer of glassy carbon (GC) samples after thermal treatment in a temperature range of 1500 – 3000°Cin an inert atmosphere. Heat treatment leads to structural transformations that change the ratio of hybridization of carbon atoms, impurity content, and porosity. IR-Fourier spectroscopy study of the samples using IR-Infinity SHIMADZU with a standard diffuse reflection attachment revealed sp-, sp²-, and sp³-hybridized carbon atoms present in GC samples, and adsorbed hydroxyl, carbonyl groups and hydrogen atoms in aromatic and aliphatic carbon structures. Change in the content of those structures with an increase in the temperature of heat treatment of the samples is analyzed. Electron microscopy carried out on the JEOL JSM-6490LV device revealed the presence of microporosity, layered structural fragments that differ from the GC structure inside the pores. The obtained results compared with the results of X-ray diffraction analysis of the samples match the available data regarding the structure and structural transformations in GC.

Problematic issues of the current state and prospects of development of the standard, unified and special laboratory, bench and full-scale tests are considered to substantiate complex characteristics of the durability, survivability, cold resistance, reliability and safety of the elements of pipeline transport of oil and oil products are considered. These tests are linked to the stages of the pipeline life and improvement of the basic and verification methods of calculation and experimental determination of the criterial characteristics of the pipe steels, pipes and main pipelines with allowance for domestic and foreign experience. In the field of standard tests for static stretching, the experimentally obtained characteristics of the basic mechanical properties (yield strength and strength, elastic moduli) are included in the basic calculations of the static strength of newly designed and functioning pipelines. Standard tests for hardness and toughness are used to control the quality of pipe steels. The results of standard tensile tests are used to provide additional computational information regarding the estimates of ductility and degree of steel hardening upon elastoplastic deformation to get reliable verification estimates of the static strength. Unified laboratory tests are intended to refine determination of the pipeline strength taking into account the effects of 3D character of the stress state, absolute sizes of the pipeline cross section, deformation rate, anisotropy, cold resistance, corrosion and existence of welded connections. Assessment of the crack resistance of the pipe steel and pipes by criteria of linear and nonlinear fracture mechanics with allowance for technological and operational defects takes a special place in laboratory and bench tests. An emphasis is made on the domestic experience gained in the Russian system of testing the main pipelines for transportation of oil and oil products.

One of the little-studied problems of modern mechanics and the physics of fracture is the branching of the crack, which is observed in materials of a different nature. For his research, an analysis of the criteria and mechanisms for crack branching. The investigations of crack branching in polymers and steel, fractographic investigation of the fracture surface are considered; criteria for crack branching as a dynamic stress intensity factor, crack speed. It is established that the crack at branching in brittle plastics reaches the limiting propagation speed V* = 500 – 800 m/sec. Tensile tests of flat samples from polymethylmethacrylate (PMMA) at temperatures of +20 and –60°C were carried out, with measurement of crack speed by the method of rupture of conducting strips. A measuring device based on a precision converter of signals of resistance thermometers and thermocouples «TERCON», connected to a computer, was created. Measured crack speed for rectilinear crack propagation in the mirror, matte, and feather zones of fracture surface of the PMMA; with single branching of the crack; with multiple branching of cracks with parallel movement of the front of several cracks. A hypothesis is proposed for the physical mechanism of fracture branching.

A method for measuring the torque upon loading of the substance by the method of P. U. Bridgman is presented. The method provides a strong axial compression of the substance between two punches. At the same time, the compressed substance is additionally exposed to an external action resulted from rotation of one plunger relative to another. The pressure in such experiments can reach 5 GPa or more. The punches are made of hardened steel or hard alloy. The proposed device is a simple and holistic mechanism. It consists of a universal shell, shell, two punches, converter modules, a hollow cylinder and an elastic thin disc. The device is mounted on a unit of complex loading which has a plunger of rotation and axial displacement. The punches are fixed in the shells. The working diameter of the punches and, correspondingly, of the test sample, depending on the experimental conditions, ranges from 5 to15 mm. In special cases the diameter can be more than15 mm. The torque of loaded sample in this device is measured by transducing modules. To increase the sensitivity, the transducing modules are placed beyond the universal shell and are located far from the supporting surfaces of the device. The original design of the transducing module ensures the independence of the force point from the rotation of the punch in the plane perpendicular to the force axis. This feature of the transducing module provides deformation of tensometric resistors under the impact of elastic compression only from the force resulted from the punch rotation. The guaranteed elimination of undesirable interferences allows a qualitative measuring of the torque. The proposed device provides high sensitivity under extreme conditions and desired quality of torque measurements.