МЕТОДИКА ОПРЕДЕЛЕНИЯ ИЗОТОПНЫХ ОТНОШЕНИЙ Cu И Zn МЕТОДОМ МК ИСП-МС С ИСПОЛЬЗОВАНИЕМ СМОЛЫ AG MP-1

The isotopic composition of copper is of great interest for researchers in various fields of science, geochemistry and hydrology in particular, wherein the consideration is being given to the variations in the isotopic composition of the Earth's crust, extraterrestrial matter, and water basins, as well as to the origin and transfer of matter. Zn isotopes appear to be promising for identifying the sources and pathways of the environmental pollution. The aim of this study involves the refinement and validation of the zinc and copper isotopic ratio determination methodology covering the whole process from sample digestion to MC ICP-MS measurements. For this reason, as well as to assess the suitability of the methodology for the analysis of environmental samples, Zn and Cu isotopic analysis of the BHVO-2, BCR-2 and AGV2 USGS certified reference materials has been performed. The method for determination of Cu and Zn stable isotope ratios by multi-collector inductively coupled plasma mass spectrometry in environmental samples is developed. The application of the AG MP1 resin with optimized layer parameters (resin bed height 3.5 cm, diameter 1 cm) provides the highpurity Cu and Zn fractions. The method is characterized by high throughput and adequate analytical figures of merit when using the standardsample bracketing technique for mass bias correction. The procedural blanks related to chemical dissolution and ion exchange procedures are lower than 1 and 3 ng for Cu and Zn, respectively, assuring no blank effect on the isotopic composition of samples. The accuracy and precision obtained for Cu and Zn isotope measurements in the BHVO2, BCR2 and AGV2 geological certified reference materials demonstrate good agreement with the reference values published. © 2022 Institute of the Earth's Crust. All rights reserved.ААААА181180530900458; Ministry of Education and Science of the Russian Federation, Minobrnauka: 075-15-2021-680; Russian Science Foundation, RSF: 18-77-10024The work of Okuneva T.G. is supported by the Russian Science Foundation (project 18-77-10024), the rest authors are supported by the state assignment of the IGG UB RAS ААААА181180530900458. Isotopic analyses are performed at the "Geoanalitik" Shared Research Facilities of the IGG UB RAS. The reequipment and comprehensive development of the "Geoanalitik" Shared Research Facilities of the IGG UB RAS is financially supported by the grant of the Ministry of Science and Higher Education of the Russian Federation (Agreement 075-15-2021-680).authors are supported by the state assignment of the IGG UB RAS ААААА 猃?猃猃稃爃眃甃爃笃爃爃瘃?稁 Isotopic analyses are performed at the 㘀Geoanalitik ? Shared Research Facilities of the IGG UB RAS. The reequipment and comprehensive development of the 㘀Geoanalitik 㘀 Shared Research Facilities of the IGG UB RAS is 퀀inancially supported by the grant of the Ministry of Science and Higher Education of the Russian Federation (Agreement 075-15-2021-680).FUNDING: The work of Okuneva T.G. is supported by the Russian Science Foundation (project 18-77-10024), the res

THE METHOD FOR Cu AND Zn ISOTOPE RATIO DETERMINATION BY MC ICP-MS USING THE AG MP-1 RESIN

The isotopic composition of copper is of great interest for researchers in various fields of science, geochemistry and hydrology in particular, wherein the consideration is being given to the variations in the isotopic composition of the Earth’s crust, extraterrestrial matter, and water basins, as well as to the origin and transfer of matter. Zn isotopes appear to be promising for identifying the sources and pathways of the environmental pollution. The aim of this study involves the refinement and validation of the zinc and copper isotopic ratio determination methodology covering the whole process from sample digestion to MC ICP-MS measurements. For this reason, as well as to assess the suitability of the methodology for the analysis of environmental samples, Zn and Cu isotopic analysis of the BHVO-2, BCR-2 and AGV-2 USGS certified reference materials has been performed. The method for determination of Cu and Zn stable isotope ratios by multi-collector inductively coupled plasma mass spectrometry in environmental samples is developed. The application of the AG MP-1 resin with optimized layer parameters (resin bed height 3.5 cm, diameter 1 cm) provides the high-purity Cu and Zn fractions. The method is characterized by high throughput and adequate analytical figures of merit when using the standard-sample bracketing technique for mass bias correction. The procedural blanks related to chemical dissolution and ion exchange procedures are lower than 1 and 3 ng for Cu and Zn, respectively, assuring no blank effect on the isotopic composition of samples. The accuracy and precision obtained for Cu and Zn isotope measurements in the BHVO-2, BCR-2 and AGV-2 geological certified reference materials demonstrate good agreement with the reference values published

The first experience of combined treatment of patients with diabetic macular edema and complicated cataract

Diabetic cataracts in combination with diabetic macular edema (DME) is a leading cause of vision loss i n patients with diabetes mellitus.Purpose. To evaluate the efficacy and safety of one-stage combined treatment of patients with diabetes complicated by DME and cat aract.Material and methods. This study involved 16 patients with diabetes of the type 2 (32 eyes). The main group included 16 eyes with complicated cataracts, who underwent the simultaneously performed phacoemulsification of cataract (FEC) with IOL implantation and intravitreal implantation of the «Ozurdex» implant. The second (retrospective control) group included 16 fellow eyes, where a standard FEC with IOL implantation was performed.Results. Six months after the treatment, the main group showed a BCVA stabilization at a level 0.25±0.12 (0.1-0.4). In the  retrospective group, the BCVA decreased and reached a baseline level 0.1±0.05 (0.05-0.2), in 5 patients the BCVA became below the baseline values. In all cases in the main group, a partial resorption of «solid» exudates was observed in the macular area. Edema of the retina decreased by 102-275 microns in comparison with preoperative indicators, the average retinal thickness was 385±58 microns in fovea area. Diffuse macular edema with a deposition of «solid» exudates remained in the retrospective control group, all patients had an increase in the amount of intra-etinal hemorrhages. In 5 patients, not only an increase in the number of «solid» exudates was revealed in the dynamics, but also their spread to the fovea region, in 3 cases the exudation foci acquired the form of hyper-reflective layers. The increase in the edema height occurred in all cases by 74-144 microns, index of average retinal thickness was 598±76 microns. In 7 cases, the dynamics showed an increase in flat subfoveal detachments of the neurosensory retina.Conclusions. The complex effect of the OzurDex drug in the combined treatment of diabetic cataracts in combination with DME reduces a risk of inflammatory complications in the early postoperative period, and also provides a reduction in the height of edema and partial resorption of «solid» exudates

Temperature Evolution of Sodium Nitrite Structure in a Restricted Geometry

The NaNO$_{2}$ nanocomposite ferroelectric material in porous glass was studied by neutron diffraction. For the first time the details of the crystal structure including positions and anisotropic thermal parameters were determined for the solid material, embedded in a porous matrix, in ferro- and paraelectric phases. It is demonstrated that in the ferroelectric phase the structure is consistent with bulk data but above transition temperature the giant growth of amplitudes of thermal vibrations is observed, resulting in the formation of a "premelted state". Such a conclusion is in a good agreement with the results of dielectric measurements published earlier.Comment: 4 pages, 4 figure

ИЗУЧЕНИЕ ПРОЦЕССА СООСАЖДЕНИЯ МЫШЬЯКА И СУРЬМЫ ПРИ ОТДЕЛЕНИИ МАКРОКОЛИЧЕСТВ ЖЕЛЕЗА, ХРОМА В ВИДЕ Na3FeF6, Na3CrF6

Theoretical and experimental studies were carried out for the first time in order to determine the mechanism of co-precipitation of arsenic and antimony during their separation from the macro-quantities of iron and chromium in the form of Na3FeF6 and Na3CrF6 sediments. It was found that the application of Dubinin-Radushkevich adsorption isotherm gives the most accurate description of the process. The average free energy of adsorption for As and Sb is 9.6 and 9.7 kJ/mol respectively. Co-precipitation of analytes in the micropores of precipitates occurred as a result of the chemical (ion-exchange) reaction. The possibility of inhibiting this process by introducing a different amount of complexing agent (hydrofluoric acid) was studied. The addition of HF led to the formation of more coarse crystalline precipitates with lower specific surface area and porosity. For the accurate ICP-AES determination of analytes (As, Sb) the molar ratio of precipitating agent / complexing agent (NaF / HF) ≈ 1 should be strictly observed. According to the developed procedure, state standard samples of steels and nickel-based precision alloys were prepared for ICP-AES determination of As and Sb contents. The difference between the found and certified content of analytes did not exceed the permitted deviations given in the corresponding Russian state standards. The ICP-AES method of simultaneous determination of As and Sb contents after their preliminary separation from the main components is recommended for the analysis of materials with high content of Fe and Cr.Keywords: sorption, co-precipitation, determination of arsenic and antimony, inductively coupled plasma atomic emission spectroscopy (ICP-AES), adsorption isotherms, fluorides, matrix componentsDOI: http://dx.doi.org/10.15826/analitika.2017.21.3.001 A.V. Maiorova1, S.Yu. Melchakov1,2, T.G. Okuneva2 , K.A. Vorontsova1, M.A. Mashkovtsev21Institute of Metallurgy of Ural Branch of Russian Academy of Sciences,101 Amundsena st., Yekaterinburg, 620016, Russian Federation2Ural Federal University, 19 Mira st., Yekaterinburg, 620002, Russian FederationВпервые проведены теоретические и экспериментальные исследования с целью определения механизма соосаждения мышьяка и сурьмы при отделении от макроколичеств железа, хрома в виде Na3FeF6, Na3CrF6. Установлено, что использование изотермы адсорбции Дубинина-Радушкевича приводит к наиболее точному описанию процесса. Средняя свободная энергия адсорбции для As и Sb принимает значения 9.6 и 9.7 кДж/моль соответственно. Соосаждение в микропорах осадков происходит в результате химической (ионообменной) реакции. Изучена возможность ингибирования процесса с помощью введения разного количества комплексообразующего агента – фтороводородной кислоты. Ее использование приводит к получению более крупнокристаллических осадков с меньшей удельной поверхностью и пористостью. Для точного ИСП-АЭС определения аналитов необходимо строгое соблюдение мольного соотношения осадитель/комплексообразующий агент (NaF/HF) ≈ 1. По разработанной процедуре к ИСП-АЭС определению содержания As и Sb были подготовлены ГСО состава стали и сплавов прецизионного типа на никелевой основе. Разница между найденным и аттестованным их содержанием не превышает нормативов, приведенных в соответствующих ГОСТах.  ИСП-АЭС методика одновременного определения содержания As и Sb с предварительным отделением основных компонентов рекомендована для анализа материалов с высоким содержанием Fe и Cr.Ключевые слова: адсорбция, соосаждение, определение мышьяка и сурьмы, атомно-эмиссионная спектрометрия с индуктивно связанной плазмой (ИСП-АЭС), изотермы адсорбции, фториды, матричные компонентыDOI: http://dx.doi.org/10.15826/analitika.2017.21.3.00

Определение фоновых изотопных отношений биодоступного стронция для рудника бронзового века новотемирский

To assess the mobility and provenance of ancient populations, it is necessary to compare their 87Sr/86Sr isotopic ratios with the local bioavailable strontium baseline (background), characteristic of each specific location or potential provenance region of an individual or artifact. Its definition requires a comprehensive approach to the analysis of heterogeneous samples («proxies») characterizing the ecosystem of the archaeological site under study, the identification of the most suitable proxies, as well as the unification and standardization of the sampling and analytic protocols. A pilot study is presented devoted the definition of the local range of bioavailable strontium by the example of the Novotemirskiy Bronze Age mine (Southern Urals). 87Sr/86Sr isotope ratios were determined in surface and underground water, bedrock (serpentinite), clay from the mine wall, and steppe polecat’s bone, as well as in grass and a bivalve shell from the lake. The lowest range of strontium isotope ratios relative to each other is characteristic of surface and groundwater, shell and grass, which allows them to be used to determine the combined baseline of bioavailable strontium. Multi-proxy (surface and underground water, grass and a bivalve shell) local bioavailable strontium baseline for the Novotemirskiy ancient mine (Southern Urals) is 0,7096 ± 0,0003 (2σ, n = 5). © 2021 Russian Academy of Sciences, Institute of Archaeology. All rights reserved.Работа выполнена при финансовой поддержке РНФ, проект No 20-18-00402 «Миграции человеческих коллективов и индивидуальная мобильность в рамках мультидисциплинарного анализа археологической информации (бронзовый век Южного Урала)», в ЮУрГУ (НИУ) (Д. В. Киселева – геохимическая интерпретация, П. С. Анкушева – археологическая документация и аналитика; Т. Г. Окунева, А. В. Касьянова – измерения проб и стандартных образцов; Е. С. Шагалов, М. Н. Анкушев – отбор проб и геологическая характеристика)

OPTIMIZATION OF CONDITIONS OF SEPARATION OF CHROMIUM AND IRON FOR ICP-AES DETERMINATION OF ARSENIC AND ANTIMONY IN STEELS

For the first time is given a new approach to solve the problem of separation of trace analytes (As, Sb) from matrix elements (Fe, Cr) forming steels. Matrix elements provide an interfering effect on the results of arsenic and antimony determination employing the ICPAES analysis. It is found that required deposition conditions of macroamounts (Fe, Cr) should meet the molar ratio NaF/HF close to 1 in aim to inhibit analytes coprecipitation.Работа выполнена при финансовой поддержке РФФИ (грант № 16-33-00317)

Fungal endophthalmitis

The article presents a clinical case of fungal endophthalmitis, the causative agent of which was Paecilomyces lilacinum. Patient M., female, 1947 year of birth was operated on for complicated cataract of the right eye. Two weeks later, she complained of decreased vision. A local anti-inflammatory therapy of the exudative reaction in the anterior chamber was carried out, therefore an improvement was achieved. Two weeks later, the patient again complained of visual impairment. Лечение было продолжено со сменой фунгицидных средств, обладающих большим Systemic and local anti-inflammatory and antibacterial therapy of exudative uveitis with the course of fluconazole for 15 days was carried out. Extended clinical and laboratory studies did not reveal any chronic inflammatory and immune diseases in the female patient. In connection with the further progression of the process, vitrectomy was performed with the removal of IOL and washing of the vitreous cavity with a solution of vancomycin. The achieved stabilization lasted short. There were appeared signs indicating a fungal etiology of the inflammatory process. Taking into account the previous long-term antibiotic therapy, yeast contamination was suggested. Despite the active treatment, there was a further deterioration of the eye. No pathogenic and conditionally pathogenic microflora growth was revealed as a result of seeding. Confocal microscopy revealed a filamentous structure of the mycelium in the thickness of the corneal stroma, which indicated infection with mold, not yeast fungi. Treatment was continued with a change of fungicidal agents with a large spectrum of action, as well as a silicone oil tamponade. The obtained culture was aimed at identification of the species and determination of sensitivity to fungicides in the medical scientific and practical center for tuberculosis control, Moscow. Cultural studies identified pathogenic microflora – Paecilomyces lilacinum, sensitive to ketoconazole. In connection with the spread of infection to the periorbital tissues, with the subsequent probability of systemic damage, an emergency enucleation of the eyeball was decided. This example indicates the need for increased alertness for fungal infection in cases of atypical flow of intraocular inflammation, the search for methods for early detection of the pathogen

ENVIRONMENTAL GEOCHEMISTRY OF HEAVY METALS AND METALLOIDS IN THE WATER-SOLUBLE SOIL FRACTION (ORENBURG REGION)

The study is devoted to the investigation of distribution of heavy metals and metalloids (HMM) in the water-soluble soil fraction of soil samples collected over the territory of the Orenburg Region. HMM are analyzed by ICP-MS, and their environmental-geochemical indices are calculated and discussed.Работа выполнена в ЦКП УрО РАН «Геоаналитик» в рамках темы № 123011800012-9 государственного задания ИГГ УрО РАН