Modern Analytical Equipment Research Articles

Study of matrix interference in the determination of selenium and tellurium in ICP-AES in metallurgical materials

The content of selenium and tellurium used in steels and alloys as alloying additives is strictly regulated by the current state standards. The methods of analysis used in state standards are often lengthy and laborious and do not provide their simultaneous determination. Development of alternative methods for the determination of selenium and tellurium in metallurgical materials using modern analytical equipment is an urgent goal. The method of atomic emission spectrometry with inductively coupled plasma (ICP-AES) is widely used in analysis of metallurgical materials. However, the components of the sample base can significantly affect the results of ICP-AES analysis. We present the results of theoretical and experimental study of the effect of the components of the base of samples of metallurgical materials (iron, nickel, chromium, molybdenum, cobalt, copper, tungsten) on the spectral analytical lines of selenium and tellurium. Thermodynamic modeling was used for theoretical prediction of the processes occurring during atomization of the analyzed solutions in argon plasma. It is shown that matrix non-spectral noise on the selenium line is attributed to chromium (at chromium concentrations above 50 mg/dm3), whereas the matrix non-spectral noise on the tellurium line is not observed. It is also shown experimentally that the spectral lines of selenium and tellurium are not free from spectral overlaps attributed to macrocomponents (iron, nickel, chromium, molybdenum, cobalt, copper and tungsten). To reduce the limits of detection and improve the reliability of ICP-AES determination of selenium and tellurium, it is necessary to separate them from the components of the sample base.

ИЗУЧЕНИЕ СВОЙСТВ АЛЮМОСИЛИКАТНЫХ МИКРОСФЕР И ОЦЕНКА КОЭФФИЦИЕНТА ПРОНИЦАЕМОСТИ СТЕНОК ПО ГЕЛИЮ И ВОДОРОДУ

In this work, basic properties of aluminum silicate microspheres are studied using modern analytical equipment. Comparative experiments to assess the permeability coefficients of the glass walls for helium and hydrogen have been carried out, the kinetic parameters of the process have been determined.

ОПРЕДЕЛЕНИЕ УДЕЛЬНОЙ ПОВЕРХНОСТИ ПОРОШКОВ ЦИРКОНИЯ МЕТОДОМ НИЗКОТЕМПЕРАТУРНОЙ АДСОРБЦИИ АЗОТА

The work is devoted to determination of the specific surface of fine-dispersed zirconium powders of different producers by low-temperature nitrogen adsorption method using modern analytical equipment. Sodium-reduced zirconium powders of two different productions, as well as coarse electrolytic zirconium powder after its grinding by hydride technology, were researched in the present work. Consequently the values of the specific surface of the studied zirconium powders by the BET method were obtained, and features of such measurements by “Sorbtometr-M002” evaluator for the specified materials were noted.

A comprehensive review of thermogravimetric analysis in lignocellulosic and algal biomass gasification

Global concern about energy security, climate change, and increasing wastes have propelled the utilization of waste-to-energy technologies. Gasification is a robust thermochemical process that can handle a diverse range of biomass feedstocks and residues with various physicochemical properties while producing several value-added bioproducts and bioenergy. Meanwhile, the use of thermogravimetric analysis to determine the sample mass loss rate under a high-temperature gasification environment is a promising way to understand the chemical reactions, reactivities, and kinetic parameters of the thermochemical processes. This review focuses on the benefits of utilizing thermogravimetry for the biomass gasification process, with particular attention paid to the determination of kinetic parameters such as the pre-exponential coefficient and activation energies, resulting from model-fitting and model-free approaches. Relevant gasification parameters such as onset temperatures, residence times, and other important findings are also reported. Future trends are opined to be leaned towards the more extensive blending of biomass feedstocks with either coal, wastes, or other types of biomass, and applying artificial intelligence to improve data processing, prediction, and optimization of gasifier designs. This study also underlines integration with other modern analytical equipment to better characterize product evolution.

Phytochemical characteristics and the study of acute toxicity of extracts from fruit Рrunus domestica

The increased demand for modern phytopreparations is dictated by their wide application in the complex treatment of various diseases, the presence of low toxicity and the pharmacoeconomic component. Phytochemical analysis of medicinal plants reveals not only potential therapeutic effects, but also assumes their toxicological properties. In this context, the Prunus domestica, widely spread on the territory of our country and well known for its medicinal properties and applications in folk medicine, has attracted our attention.
 The aim of the work was to investigate the phytochemical composition of extracts obtained from fruit Prunus domestica and to study their toxic properties.
 Phytochemical analysis of the extracts obtained from fruits Prunus domestica was carried out according to the original method of extracting biologically active compounds, using instrumental research methods using modern laboratory analytical equipment.
 Studies of the safety of four extracts from Prunus domestica (liquid EC-1, EC-2 and dry CEPC, CEV) with the calculation of median lethal doses were carried out on mice and rats with the single intragastric and intraperitoneal routes of administration according to the method of T. V. Pastushenko. The degree of toxicity was determined according to the classification of K. K. Sidorov.
 Phytochemical study of extracts from fruit Prunus domestica provided information on the presence in their chemical composition of flavonoids, the sum of phenolic compounds, anthocyanins, neutral sugars, amino acids, organic and hydroxycinnamic acids. A higher content of the sum of phenolic compounds in the aqueous (ЕС-1) and alcoholic extracts (ЕС-2) as well as the presence of neutral sugars as products of hydrolysis of homopolysaccharides (СEV extract) and heteropolysaccharides (CEPC extract).
 Experimental studies proved that EC-1, EC-2, CEPC and SEV extracts had low toxicity beyond 15 000 mg/kg when administered orally and 3 000 mg/kg when administered intraperitoneally. The LD50 of the studied extracts of mice and rats after intraperitoneal injection was determined, which was more than 3 000 mg/kg.
 The chemical composition of biologically active compounds of extracts from the fruit Prunus domestica, which provides promising directions for further study of their pharmacological properties, has been investigated.
 Analysis of experimental data on acute toxicity of the studied extracts showed that they belong to the IV class of toxicity “relatively harmless substances", according to K. K. Sidorov classification. The LD50 of extracts from the fruit Prunus domestica for oral administration could not be determined, and the LD50 of the studied extracts for mice and rats after intraperitoneal administration was more than 3 000 mg/kg.

Морфологические, структурные и оптические свойства микропорошков диоксида титана

The work is devoted to a comprehensive experimental study of the morphology, structure and optical properties of titanium dioxide micropowders with several of modern analytical equipment. The method for obtaining photoluminescence (PL) and Raman scattering (RS) for titanium dioxide micropowders in microresonator cuvette (photon traps) was described. The powders consisting of close-packed particles in the shape of spherical particles of specified sizes (29-63 μm) were studied. In the photon traps, a certain mode is implemented, which is associated of trapping of the exciting radiation inside of device. It is shown that, at room temperature, intense photoluminescence in titanium dioxide micropowders (2.91 eV) was observed in excitation by the second optical harmonic (λ exc = 255.3 nm) of a copper vapor laser. It has been established that in micropowders of titanium dioxide micropowders in photon traps, is possible to observe the phenomenon of combination opalescence, which leads to the sharp (5–6 orders) increasing in the RS intensity in an ultradispersed medium. The high conversion efficiency of the exciting radiation into the RS signal is explained by the large value of the total path that the exciting radiation photon travels in the dispersed medium in the photon trap. It was found that an insignificant amount of silicon and aluminum impurities is present in titanium dioxide micropowders that not affect to formation of the photoluminescence band in the region of 2.91 eV. The developed method for recording PL and RS opens up wide possibilities for recording weak signals of secondary radiation that is important for inorganic and organic substances, as well as for creating small-sized laser analyzers of chemical compounds which is necessary for solving many practical problems.

P‐6.5: Cu Erosion of Via Hole within GOA Unit of Super‐large and Ultra‐HD TFT‐LCD of 120Hz Frame Rate

Cu erosion of via hole within GOA unit of super‐large and ultra‐HD TFT‐LCD of 120Hz frame rate is an important issue and may cause some line failures. Reliability tests of panel about temperature and humidity are used to accelerate occurrences of the relative failures (Y‐Line). Effects of some critical factors including ITO thickness, tray life and sealant coverage are analyzed for optimal combination of mass production parameters. Furthermore, mechanisms of the Y‐Line failure are dissected by some modern analytical equipment. Deep via hole broken is found to be primary cause of Y‐Line failure of 75inch 4K 120Hz panel in Green127 pattern. The broken is caused by erosion of gate Cu in the via hole. There is initial Cu erosion at chamfer consisting of GI‐Cu‐ITO, caused by photoresist stripping after via hole etch, leading to open the ITO used to connect gate Cu (below GI) and data line (above GI). The ITO open provides possibility for H2O to passing through, and greatly weakens its shielding ability. A channel for H2O diffusion resulting in Cu erosion after “8585” and “THO” tests can be speculated to be interfaces consisting of Sealant‐PVX and Sealant‐ITO.

The Mobile Complex of Chemical Control as the Basis of Technical Equipment of the Mobile Diagnostic Group of the 33 Central Scientific Research Test Institute of the Ministry of Defenсe of the Russian Federation

The special mobile diagnostic group (MDG) is formed in the Federal State Budgetary Establishment «33 Central Scientific Research Test Institute» of the Ministry of Defenсe of the Russian Federation (hereinafter referred to as the institute) to perform tasks related to the radiation and chemical (RCh) control of different objects, to ensure RCh safety and security of mass events, as well as to perform special tasks of RCh examination of samples of all kinds. The purpose of the work is to consider the design, capabilities and organization of the mobile complex of chemical control (MCCC), which is the basis of the technical equipment of the MDG. The complex is created on the basis of Ford-Transit off-road vehicle with the equipment for the MDG and a container installed on a two-axle platform, where the equipment for the MDG is located. The complex is equipped with modern analytical equipment, means of communications, navigation, information processing and automatic meteorological observation, with the life support kit, autonomous power and water supply systems, exhaust ventilation, heating and air conditioning systems. The technical characteristics of the MCCC are as follows: crew – 8 people; preparation time – no more than 60 minutes; time for the preliminary identification of substances detected by the mobile group (from the moment of arrival) – no more than 60 minutes; the lower limit of detection of toxic chemicals in environmental objects – at the maximum concentration limit; time of confirming identification of detected toxic chemicals (from the moment of delivery of samples) – no more than 180 minutes; cruising range – up to 700 km. The methodological apparatus is also developed, that ensures the functioning of the MCCC crew during the performance of wide range of tasks of the MDG. Subsequently, this methodological apparatus has been repeatedly expanded and refined based on the results of the complex's participation in ensuring the RCh security of various mass events. The algorithm of carrying out special chemical control by technical means of the MCCC complex is presented in the article. The complex is capable of detecting both low-hazard and emergency concentrations of practically all known toxic chemicals in various samples, and identifying these substances in environmental objects.

FORUM «TERRITORY OF NDT» 2020

A brief analytical review of the events of the VII International Industrial Forum “NDT Territory. Non-Destructive testing. Tests. Diagnostics” and the “XXII Аll-Russian Scientific and Technical Conference on Non-Destructive Control and Technical Diagnostics” held simultaneously with it. All events were held at the Expocenter Central Exhibition Complex in Moscow. The exhibition of instruments and tools of NK and TD was accompanied by a business program. Within the framework of the forum, round tables were held on topical issues of non-destructive testing and technical diagnostics. The exhibition was attended by more than 57 companies, and information support was provided by a number of news agencies, including the “Spectrum Publishing House” and “RIA Standards and Quality” (“World of Measurement” magazine). In addition to equipment for non-destructive testing and technical diagnostics, modern test equipment, testing and analytical equipment begins to appear on the stands of exhibitors. This year there was a focus on hightech solutions for engineering, metallurgy, oil and gas and other industries. The final of the competition for NK specialists and the award ceremony took place. For the first time, the “Salon of Innovations and Startups 2020” was organized at this Forum, in which representatives of 20 organizations took part. The forum demonstrated a high technical level of non-destructive testing, their metrological support, as well as certification and standardization.

Current state and development trends of domestic medical device market for in vitro diagnostics in the segment of diagnostic reagents and their kits.

The problem of import substitution in the Russian medical device market for in vitro diagnostics (MDivd) has not been solved, despite a number of measures taken by the government of the Russian Federation since 2011. The reasons hampering this process are the lack of modern analytical equipment of domestic production and deficiencies of the current regulatory system for MDivd circulation in the market. It is proposed the transition from licensing system of MDivd registration to notification system as a radical measure to solve the problem of import substitution.

Preface

These Conference Proceedings contain the selected papers of the X All Russian petrographic conference with international participation “Petrology of magmatic and metamorphic complexes” which was held from 27 to 30 November 2018 in Tomsk. The conference was organized by the Faculty of Geology and Geography of the National Research Tomsk State University. Issues of petrology of different geodynamic complexes of the lithosphere were considered. All their diversity is united by a common paradigm of the Earth evolution as a result of magmatic activity, metamorphism and formation of sedimentary basins.The Program Committee included the members of the Russian Academy of Sciences N.L. Dobretsov, V.A. Koroteev, M.I. Kuzmin, V.V. Reverdatto, V.V. Yarmolyuk, corresponding members of the Russian Academy of Sciences D.P. Gladkochub, G.V. Polyakov, E.V. Sklyarov, Professor of the Carleton University (Canada) R.E. Ernst, Professor of the University of Salamanca G. Gutierrez-Alonso, Professor of the University of Wyoming K. Chamberlain and other famous scientists.The presented materials combine the results of a structural and compositional study of volcanic, plutonic and metasedimentary complexes of Eurasia. This forum became a convenient platform for wider exchange of scientific information between specialists from higher education institutions, academic institutions and companies. Section for young researchers with the aim of developing their scientific and creative potential in the field of modern petrology was foreseen by the conference program.The conference was supported by Russian Foundation for Basic Research and the Government of the Russian Federation (grants No. 18-05-20112, 14.Y26.31.0012) and sponsorship by the famous Russian private companies «TESCAN» (St. Petersburg), «LABTEST» (Moscow) and «Reolgrade service” (Novosibirsk), specializing in the supply of modern analytical equipment and standard samples for physic-chemical research.We are grateful to all participants of the meeting for the fruitful work and active support of the forum.Organizing Committee

REGISTRATION DOCUMENTATION AND AMENDMENTS TO IT AS AN ELEMENT OF A QUALITY MANAGEMENT SYSTEM IN PRODUCTION OF ANTI-RABIES IMMUNOGLOBULIN (REVIEW)

Introduction. Documentation is an integral part of the quality management system, a key element of production and quality control of medicines. A necessary condition for the Rules of good manufacturing practice and guaranteed production of quality products is compliance with the requirements set out in the documents of the registration dossier for the drug. During the life cycle of a drug, post-registration changes in the dossier may be required. Text. This work is an analytical review of changes in the documents of the registration dossier for the drug «Immunoglobulin antirabic from horse blood serum liquid», solution for injections, reflecting the improvement of biotechnology of drug production and methods of its control in the post – registration period. The first post-registration changes in the regulatory documentation were administrative in nature and did not require examination of samples of the drug. The next group of changes in the documents of the registration dossier was due to the expansion of production, reconstruction of technological sites and the introduction of innovative technologies in order to comply with the requirements of GMP, as well as improving the consumer properties of the drug. The last group of changes concerned the revision of methods of quality control of finished products associated with the introduction of modern analytical equipment, expanding the list of standards and bringing into compliance with the requirements of the state Pharmacopoeia XIII edition. Conclusion. The timely introduction of changes into documents of the registration dossier allows you to optimize the procedure for the conduct of internal and external control of rabies immunoglobulin, as well as to avoid violations related to the actualization of the technological documentation. The analysis of changes in the documents of the registration dossier for the drug «Immunoglobulin antirabic from horse blood serum liquid», solution for injections, reflecting the improvement of biotechnology of drug production and methods of its control in the post-registration period. Timely changes in the documents of the registration dossier allow to optimize the procedure of internal and external quality control of anti-rabies immunoglobulin, as well as to avoid violations associated with the updating of technological documentation.

DETERMINATION OF VEGETABLE FATS IN FOOD PRODUCTS

Tightening control over the quality and safety of food products leads to an expansion of the list of standardized indicators and the regulatory framework of research methods. Despite the lack of established standards and requirements for fatty acid composition (FAC) of meat products and the content of vegetable fats in it, methods have been developed for determining FAC and vegetable fats. The presented approaches to sample preparation make it possible to extract analytes from a sample as quickly and efficiently as possible, and the capabilities of modern analytical equipment make it possible to determine even trace amounts. The lower limit of determination of vegetable fats is 1.0 mg / kg. Ionization by electron impact, in which the molecule of the analyte breaks down into characteristic daughter ions, as well as the use of a library of mass spectra exclude obtaining false or falsepositive results.

SPECIFICITY OF ENGINEERING-ECOLOGICAL SURVEYS IN SMALL TIDAL ESTUARIES OF THE WESTERN SECTOR OF THE RUSSIAN ARCTIC

Field investigations of recent years carried out in the tidal estuaries of the western sector of the Russian Arctic zone using modern hydrometric and analytical equipment made it possible to identify a number of regularities. Analysis of these patterns makes it possible to optimize the complex of engineering and ecological surveys conducted in tidal estuaries. The estuaries of small rivers flowing into the tidal seas of the Arctic Ocean have a very specific hydrological and hydro-chemical regime, characterized by a pronounced short-period variability of many parameters due to both tidal forces and solar radiation. Semidiurnal, diurnal and semi-monthly (spring-neap) cycles are reflected in the specific functioning of aquatic ecosystems. Field-studies of small estuaries of the White and Barents Seas show that the intra-season variability of hydrological and hydro-chemical indicators, formed under the influence of three main factors — tides, solar radiation and synoptic processes, is comparable to their seasonal fluctuations or even surpasses it. Tidal semidiurnal, diurnal and semi-monthly cycles are most clearly expressed in changes in water level, currents, salinity and concentration of soluble conservative impurities, with a significant difference between their river and marine background values. In the fluctuations of the suspended matter and insoluble substances concentration, the dominance of the over-harmonic with a period of 3–4 hours and synoptic disturbances with a period of 6–10 days can be observed. To estimate the short-period variability of the parameters under study, the most optimal variant of engineering-ecological surveys is the 14-day series of observations with different discreteness for the hydrological and hydro-chemical parameters of the water masses in the estuary. Under organizational, technical and financial constraints, it may be permissible to perform two series of daily observations with a discreteness of 1–2 hours during spring and neap tides, separated by a weekly interval. In exceptional cases in the hard-to-reach Arctic regions, 3-time observations can be performed during only the spring tidal cycle: high water, half-tide and low water.

Considerations for veterinary practitioners involved in feed-related toxicology cases

The objective of this paper is to identify key considerations for production animal veterinarians involved in legal cases regarding feed-related errors. Veterinarians are trained in the science of management and production, but are often ill-prepared for advising clients on potential litigation that may result when large monetary losses are incurred. The availability of modern analytical equipment and technology can provide practitioners with more information to understand the interactions of toxins with production medicine. This information may further elucidate the source of potential losses. The following considerations were derived from experiences at the Iowa State University Veterinary Diagnostic Laboratory when involved in several legal cases. Since it is likely that production veterinarians will be involved in a legal case at some point in their career, this paper is intended to help practitioners to be better prepared for cases involving feed-related toxicology cases.

Prospects for the use of security air flow to prevent ion-molecule reactions in the ionization and drift zone in classical IMS

The effective transfer of sample problem is relevant in modern analytical equipment. The paper considered a problem in detection trace concentrations of explosives by Ion Mobility Spectrometry (IMS). The investigation deals with sample adsorption on the walls of transport tubes, the ion drift chamber and the chamber of the ion source in ion mobility spectrometer. The sample losses on inlet channel surface and diffusion through penetrable gas channels are comparable with the quantity of sample itself at the sensitivity level of 10-14 g / cm3. The trinitrotoluene (TNT) sorption in different channel materials depending on their sorption properties is analyzed. A new approach preventing sorption of the substance on the chamber walls by security airflow is presented. The study includes gas flow simulation and experiments of protective gas flow setup.

Unipolar hip prosthesis with nanocomposite ceramic coated femoral head

Hip arthroplasty in elderly patients is the most progressive method of medical treatment. The method provides rapid recovery and reha­bilitation of musculoskeletal systems at an earlier period. The aim of the present study was to analyze the structural and mechanical properties of unipolar prosthesis head surfaces made of titanium and stainless steel and coated by oxide and oxynitride nanocom­posite for hemiarthroplastic hip replacement as well as clinical approbation of prostheses «BES-T Manufacturing» (Ukraine), for possibility of applying this technology in traumatology. The struc­ture of Al2O3 (MS) and AlN/ Al2O3 (MS) magnetron sputtered films was investigated by means of XPS and XRD methods. The surface topography and roughness was estimated by profilometer Hommel T-2000 measurements and by AFM method. ElvaX spectrometer is modern analytical equipment for high-line non-destructive el­emental analysis. The analysis of the results of treatment patient’s with fractures of the femoral neck under observation period from 12 months to 3 years was presented. The unipolar hip replacement operations were made in urban trauma hospital during the period from 2012 to 2014. The age of patients was in the range from 72 to 86 years. All patients had a history of intra-articular fractures of the femoral neck. The joint femoral head surfaces with nano­composite oxide and oxinitride coatings demonstrate improved biocompatibility due to wettability increasing and fluid friction characteristics advancing. The deep understanding of the tribology of artificial joints is essential for reducing wear and corrosion of modern prostheses. Deposition of ceramic coatings on a surface of metal artificial joint’s head is an effective way to advance the functional characteristics of unipolar and bipolar prosthesis for joint arthroplasty.

The Thermo Techno Modern Analytical Equipment for Research and Industrial Laboratories

The Thermo Techno Modern Analytical Equipment for Research and Industrial Laboratories

Современное аналитическое оборудование компании «Термо Техно ЛЛС» для научных исследований и промышленных лабораторий

Современное аналитическое оборудование компании «Термо Техно ЛЛС» для научных исследований и промышленных лабораторий

The Precambrian history of the origin and evolution of the Solar System and Earth. Part 1

The paper provides a review of early stages of development the Solar System and the geological history of Earth with reference to the latest data on the origin of the Solar System and the formation of the first continental rocks and results of studies of zircon, the oldest mineral so far dated on Earth. The formation of the Solar System from a gas-and-dust nebula is estimated to have begun 4.568 billion years ago. Ice was formed 1.5 million years later; it concentrated at the periphery of the system and served as the material for the largest planets, Jupiter and Saturn. In the central areas of the system, asteroids with diameters of about 10 km were formed. Their small bodies were composed of the basic material of the solar nebula, as evidenced by carbonaceous chondrite, CI, which composition is similar to the composition of the Sun, with the exception of hydrogen, helium, and volatile components that served as the main material for peripheral planets of the Solar System. Due to collision and partial merger of such small bodies, the formation of embryos of the terrestrial planets was initiated. Gravity made such embryos to cluster into larger bodies. After 7 million years, large asteroids and planet Mars were formed. It took 11 million years to form Planet Earth with a mass of 63 %, and 30 million years to form 93 % of its mass. Almost from the beginning of the formation of the Earth, short-lived radionuclides, 26Al and 60Fe, caused warming up of the small planetary bodies which led to the formation of their cores. During the initial stages, small magma reservoirs were formed, and molten iron particles gathered in the centres of the planetary bodies. As suggested by the ratio of 182W/184W, the major part of the core was formed within 20 million years, while its full mass accumulated completely within the next 50 million years. In 30–40 million years after the creation of the Solar System, the Earth collided with a cosmic body which mass was close to the mass of Mars, and it was the beginning of the formation of its satellite, Moon. When the Earth – Moon system was subject to the major meteorite bombardment 4.5–4.1 billion years ago, zircons formed due to impact activity on the Moon, and on Earth it caused major eruption of basaltic magma, the differentiation of which led to the formation of acid magmas in small amounts which caused the formation of zircons, the only remnants of the first continental rocks of Earth. Later on, meteorite bombardment continued and contributed to the burial of the first continental acid and basic rocks in the mantle, wherein such rocks eventually became part of the mantle which became the progenitor of granite-greenstone rock associations. Grey gneisses contain traces of the first continental formations of Earth as evidenced by ancient zircons that are ubiquitous in the crust of Earth. The above is confirmed by results of detailed studies of regional zircons with the use of modern analytical equipment providing for high accuracy of local analyses.