Inorganic Materials最新文献

{"title":"Determination of Polychlorinated Biphenyls in Water Using Gas Chromatography–Mass Spectrometry with Extractive Freezing-Out of Analytes","authors":"T. A. Chervonnaya,&nbsp;T. N. Musorina,&nbsp;Z. A. Temerdashev,&nbsp;V. N. Bekhterev,&nbsp;I. G. Korpakova","doi":"10.1134/S0020168524700481","DOIUrl":"10.1134/S0020168524700481","url":null,"abstract":"<p>A method for determining polychlorinated biphenyls (PCBs) in waters using preliminary concentration of analytes through extractive freezing-out under the action of centrifugal forces (EFC) is developed. According to the mathematical model of extraction constructed using the three-factorial Box–Behnken plan, the significant factor is the content of acetonitrile in the extraction mixture, and the insignificant factors are the degree of chlorination of PCBs and the concentration of analytes. Analysis of the surface area of this model allows one to establish the region of optimal values of acetonitrile concentration in the range from 14% to 21%. The acetonitrile content of 15% in the extraction mixture ensures the maximum extraction efficiency of seven different PCBs (&gt;92%) in a wide range of their concentrations (from 1.0 to 5000 ng/L). The relative standard deviations of repeatability and reproducibility of the analysis results are in the range from 4.2 to 6.8% and from 5.3 to 8.1%, respectively, at an error in determining the analytes being 10–15%. Petroleum hydrocarbons are not extracted into the acetonitrile extract and do not interfere with the determination of PCBs, which also ensures longer detector operation without loss of sensitivity. Co-extraction of polyaromatic hydrocarbons and organochlorine pesticides does not affect the extraction of PCBs from waters (95–100%) and does not affect the metrological indicators of the determination method.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"60 3","pages":"342 - 347"},"PeriodicalIF":0.9,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143533176","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Effect of Magnetic Nanoparticles and Cetylpyridinium Chloride on Electroanalytical Properties of Planar Sensors for Cefuroxime and Cefotaxime","authors":"E. G. Kulapina,&nbsp;R. K. Mursalov,&nbsp;O. I. Kulapina","doi":"10.1134/S0020168524700419","DOIUrl":"10.1134/S0020168524700419","url":null,"abstract":"<p>We have developed planar potentiometric sensors for cephalosporin antibiotics: cefuroxime and cefotaxime. Tetradecylammonium associates with silver(I)–cefuroxime (cefotaxime) complexes were used as electrode-active components. The linear range of the electrode function of the unmodified sensors is 10^–5 (10^–4) to 10^–2 mol/L, its slope is 46 ± 6 mV/p<i>C</i>, and the response time of the sensors is 40 s. Fe₃O₄ magnetic nanoparticles and cetylpyridinium chloride (CPCh) have been shown to improve electroanalytical properties of the sensors in cefuroxime and cefotaxime solutions. We have optimized the ratio of the modifiers in carbon-containing ink (Fe₃O₄ : CPCh = 1 : 2.5) and evaluated the principal electroanalytical characteristics of the modified sensors. The addition of a binary mixture of magnetic nanoparticles and cetylpyridinium chloride to carbon-containing ink lowers the detection limit for cefuroxime and cefotaxime to 10^–6 mol/L (10^–7 mol/L), increases the slope (55 ± 3 mV/p<i>C</i>) and linear range (10^–6 to 10^–2 mol/L) of the electrode function, and reduces the response time of the sensors to 26–30 s. Interfacial surfactant adsorption ensures stability of nanoparticle suspensions and enables preconcentration of analyte molecules. Electrostatic and hydrophobic interactions with surfactants increase solubility of organic compounds. We have demonstrated that modified screen-printed sensors can be used for determination of cefuroxime and cefotaxime in medications and model aqueous solutions containing additions of antibiotics.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"60 3","pages":"304 - 310"},"PeriodicalIF":0.9,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143533179","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of S, Ni, and Cu in Copper Nickel Sulfide Ores by Total Reflection X-ray Fluorescence Analysis: Experience of Participation in an Interlaboratory Comparison Program","authors":"A. N. Zhilicheva,&nbsp;G. V. Pashkova,&nbsp;A. V. Karkhova,&nbsp;N. N. Ukhova,&nbsp;V. M. Chubarov","doi":"10.1134/S0020168524700389","DOIUrl":"10.1134/S0020168524700389","url":null,"abstract":"<p>The quality of total reflection X-ray fluorescence (TXRF) analysis data for S, Ni, and Cu in copper nickel sulfide ores has been assessed in the framework of an interlaboratory comparison program, with allowance for requirements that should be met by techniques for determination of the chemical composition of mineral raw materials. Certified techniques for analysis of mineral raw materials by this method are not available, and the results obtained in the interlaboratory comparison program were used to assess and improve TXRF measurement accuracy. Ore samples were prepared in the form of suspensions using wet grinding. The analytical signal used was the intensity ratio of characteristic lines of the elements to be determined and a Ga internal standard. To construct calibration curves, we used reference samples analyzed by certified techniques: Cu and Ni were determined by atomic absorption, and S by gravimetry. The quality of analytical data was assessed using the <i>Z</i>-criterion. The random measurement error did not exceed 5% relative. The relative discrepancies between the TXRF results and interlaboratory comparison test results were within 10%. The described technique can be used for rapid analysis of copper nickel sulfide ore samples.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"60 3","pages":"367 - 374"},"PeriodicalIF":0.9,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143533089","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Precipitation of Iron, Tungsten, Molybdenum, and Chromium for Determination of Selenium and Tellurium in Alloy Steel by Inductively Coupled Plasma Atomic Emission Spectrometry","authors":"A. A. Belozerova,&nbsp;A. V. Mayorova,&nbsp;M. N. Bardina","doi":"10.1134/S0020168524700353","DOIUrl":"10.1134/S0020168524700353","url":null,"abstract":"<p>Selenium and tellurium impurities in metallurgical materials are difficult to determine directly by inductively coupled plasma atomic emission spectrometry (ICP-AES) as a consequence of spectral and nonspectral interferences from their major components. In this paper, we report separation of trace components (Se and Te) and macrocomponents (Fe, W, Mo, Cr, Cu, Ni, and Co) of alloy steel via precipitation. We demonstrate that the use of barium acetate and sodium fluoride as precipitants enables effective separation of selenium and tellurium from iron, tungsten, molybdenum, and chromium (less than 0.1 wt % of the initial concentration in the test solution) and partial separation from copper, nickel, and cobalt (25 to 55 wt % of the initial concentration in the test solution). We have optimized conditions for precipitation of the macrocomponents (iron, tungsten, molybdenum, and chromium) for subsequent ICP-AES determination of impurities: precipitation of the macrocomponents at pH 1; weight of the barium acetate and sodium fluoride precipitants, 10 and 3 g, respectively. We propose that hydrofluoric acid can be used to inhibit coprecipitation of selenium and tellurium on precipitates of macrocomponents. The optimal volumes of hydrofluoric and hydrochloric acids are 3 and 6 cm³, respectively. The procedure we developed for separation of trace components and macrocomponents was tested in analysis of alloy steel reference standards. The results of Se and Te determination by ICP-AES are characterized by satisfactory accuracy and reproducibility. The determination limit for the analytes after separation of the macrocomponents is 10^–3 wt %.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"60 3","pages":"328 - 333"},"PeriodicalIF":0.9,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143533174","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Modification of Block-Porous Systems with Sorption-Active Materials","authors":"I. A. Platonov,&nbsp;E. A. Novikova,&nbsp;A. S. Karsunkina","doi":"10.1134/S0020168524700444","DOIUrl":"10.1134/S0020168524700444","url":null,"abstract":"<p>We have prepared block-porous systems modified with sorption-active materials and differing in major component (AD1 aluminum or Kh20N80 steel) and porosity (0.6 or 0.75). Before applying a layer of a sorption-active material, an adsorption layer was produced on the surface of the block-porous material via chemical oxidation in the case of aluminum and thermal oxidation in the case of steel. BAU activated carbon and Polysorb-1 were used as modifiers and polymethylsiloxane was used as a binding component. Examination of the surface morphology of the systems showed that particles of the sorption-active materials had the most uniform distribution in the case of Polysorb-1 on the steel surface. To compare sorption characteristics of the sorption systems for preconcentration of volatile organic compounds, we evaluated the degree of recovery in preconcentration and desorption using a standard gas mixture containing 0.7 mg/L of hexane. The degrees of recovery ensured by the systems studied are comparable to those in the case of powder sorbents and depend on the weight of the sorption-active material applied. The highest degree of recovery (61%) was reached with the sorption systems having Polysorb-1 and polymethylsiloxane on their surface because both substances exhibit sorption activity for volatile organic compounds. Using the sorption systems five times was shown to cause no decrease in the degree of recovery upon sorption or desorption, suggesting that they can be successfully used repeatedly.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"60 3","pages":"311 - 316"},"PeriodicalIF":0.9,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143533178","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Evaluation of the Degree of Starch Pyrodextrinization Using Binary Digital Image Colorimetry","authors":"S. V. Araslankin,&nbsp;M. V. Shchankin,&nbsp;E. N. Golovina,&nbsp;O. V. Nipruk,&nbsp;A. A. Gubina","doi":"10.1134/S002016852470033X","DOIUrl":"10.1134/S002016852470033X","url":null,"abstract":"<p>Pyrodextrins widely used in industry are obtained using thermal destruction of starch in the absence of a catalyst. The viscosity and solubility of pyrodextrins are determined by the degree of pyrodextrinization of starch, which is usually assessed visually by the color intensity of the reaction products. The article summarizes information on the mechanism of starch pyrodextrinization and examines the effect of temperature and heating time on the color intensity of the resulting dextrins. It is proposed to use binary digital image colorimetry to measure the level of dextrin binarization; on the basis of the obtained values, taking into account a number of assumptions, the degree of starch pyrodextrinization is estimated. Using two-factor analysis of variance, the significance of the effect of temperature and heating time on the degree of starch pyrodextrinization α₀ is established. Using multiple regression, an equation for the dependence of α₀ on these parameters is obtained. A diagram of isothermal pyrodextrinization of starch characterizing the conditions for obtaining dextrins with different degrees of pyrodextrinization is plotted. The results presented in this article can be used to control the process of starch pyrodextrinization.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"60 3","pages":"359 - 366"},"PeriodicalIF":0.9,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143533088","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Monitoring of the Concentration of Volatile Organic Compounds in Beef Meat after Radiation Processing with Accelerated Electrons","authors":"V. S. Ipatova,&nbsp;U. A. Bliznyuk,&nbsp;P. Yu. Borshchegovskaya,&nbsp;T. A. Bolotnik,&nbsp;A. D. Nikitchenko,&nbsp;A. P. Chernyaev,&nbsp;I. A. Rodin","doi":"10.1134/S0020168524700407","DOIUrl":"10.1134/S0020168524700407","url":null,"abstract":"<p>Oxidation of lipids and proteins occurs in food products with a high concentration of fat and water such as chilled meat and fish under the action of ionizing radiation, which leads to the formation of volatile organic compounds (VOCs) in the product and appearance of specific smell and taste. During storage, various biochemical processes occur in processed chilled products which also result in a change in the concentration of VOCs that affect the organoleptic properties of the product. The accumulation of volatile compounds identified in beef samples both immediately after radiation processing and within four days after irradiation is studied by gas chromatography–mass spectrometry to determine the effective dose range for the radiation processing of beef. Monitoring of the concentration of VOCs in samples of chilled beef meat irradiated with accelerated electrons with the energy of 1 MeV in a dose range of 0.25 to 5 kGy reveals explicit dependences of the concentrations of certain alcohols, aldehydes, and alkanes on the absorbed dose and storage time. The proposed mathematical model that describes the dependences of the concentrations of VOCs identified immediately after irradiation in beef samples on the irradiation dose is based on the simultaneous occurrence of two competing processes: decomposition of compounds due to their oxidation and accumulation due to the oxidation of other compounds after exposure to ionizing radiation. It is found on the basis of the results of the study that the effective dose range of radiation processing is 250 to 1000 Gy.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"60 3","pages":"292 - 303"},"PeriodicalIF":0.9,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143533087","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of Strategic Metals in Graphitic Formations by the Methods of Neutron Activation Analysis with a Californium Source","authors":"S. I. Ivannikov,&nbsp;V. V. Ivanov,&nbsp;N. S. Markin,&nbsp;A. V. Ruslan,&nbsp;L. A. Zemskova","doi":"10.1134/S0020168524700390","DOIUrl":"10.1134/S0020168524700390","url":null,"abstract":"<p>The content of a number of strategic metals (Au, Sc, La, Sm, Eu, Dy) was determined by the method of instrumental neutron activation analysis (INAA) at the original device with a radionuclide neutron source based on ²⁵²Cf at a level comparable to their clarks in graphite-bearing rocks of the south of the Russian Far East. The key advantage of INAA in the analysis of difficult to dissolve carbon-containing materials is the non-destructive nature of the method. The proposed methodological approach avoids the complex procedure of sample decomposition, analyte separation and associated problems (dissolution, contamination and losses). Introduction into the activation zone up to 300 cm³ of a carbonaceous sample with at least 87 wt % carbon content was not shown significant influence of the carbon on the INAA results. The detection limits were calculated for analyzed elements. The possibility to determine in natural high-carbon objects the contents of Sc, La, Sm, Eu, Dy at the level below Clark level was confirmed. No significant dependence of INAA results on the density and coarseness of the tested samples was revealed. The results of determination of strategic metals in graphite-bearing metamorphic rocks of the south of the Russian Far East for two different INAA variants (reactor and with ²⁵²Cf radionuclide source) were compared. The comparison shows that our data obtained at the device with the ²⁵²Cf radionuclide source for most of the studied elements well agree with the results obtained earlier at the WWR-M reactor at the St. Petersburg Institute of Nuclear Physics named after B.P. Konstantinov. At the same time, the possibility to irradiate samples with volume of 50–100 cm³ provides high representativeness of the INAA method at ²⁵²Cf activation. It was shown that INAA method with radionuclide source ²⁵²Cf is suitable for effective determination of trace elements content in carbon-containing samples of mineral raw materials.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"60 3","pages":"317 - 327"},"PeriodicalIF":0.9,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143533228","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Some Features of Iron Determination in Dust Emissions from Gas Purification at the Electrometallurgical Plant","authors":"Z. A. Temerdashev,&nbsp;E. G. Ryadno,&nbsp;L. V. Vasileva,&nbsp;A. G. Abakumov,&nbsp;A. M. Vasilev","doi":"10.1134/S0020168524700468","DOIUrl":"10.1134/S0020168524700468","url":null,"abstract":"<p>We have studied specific features of iron determination in dust emissions from gas purification in the electrometallurgical plant by energy dispersive X-ray fluorescence (EDXRF) analysis and inductively coupled plasma atomic emission spectrometry (ICP-AES). Sample preparation conditions have been optimized with allowance for the analytical techniques used. The phase composition of the gas purification dust emissions has been determined by X-ray diffraction: the major phases are zincite, zinc ferrites, halite, and sylvite. Taking into account the X-ray diffraction results, we prepared model mixtures which were then used to construct calibration curves. A technique has been developed for rapid iron determination in gas purification dust emissions by EDXRF. The technique was tested in analysis of real dust emission samples, which were analyzed by ICP-AES as well. We obtained satisfactory agreement between the results of iron determination by EDXRF (Δ = 1.3%) and ICP-AES (Δ = 2.6%).</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"60 3","pages":"348 - 354"},"PeriodicalIF":0.9,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143533166","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"X-ray Fluorescence Analysis of Y3–xYbxNbO7 Paraniobate-Based Ceramics","authors":"A. A. Arkhipenko,&nbsp;G. E. Marina,&nbsp;V. B. Baranovskaia,&nbsp;M. A. Ryumin","doi":"10.1134/S0020168524700341","DOIUrl":"10.1134/S0020168524700341","url":null,"abstract":"<p>A two-stage technique has been developed for X-ray fluorescence (XRF) analysis of Y_3–<i>x</i>Yb_<i>x</i>NbO₇ (<i>x</i> = 0–3) rare-earth paraniobates, suitable for use as thermal barrier coating materials. In the first stage, a preliminary composition of ceramic samples and intermediate synthesis products was determined by rapid semiquantitative analysis using the fundamental parameter method. In the second stage, the quantitative composition of the samples was determined using calibration curves. To obtain the calibration curves, a series of reference samples containing 3.16–56.55 wt % Y, 8.78–71.0 wt % Yb, and 12.83–19.70 wt % Nb were prepared in the same way as the ceramic samples studied. We chose analytical lines free from spectral overlaps and optimized XRF analysis conditions (X-ray tube current and voltage, exposure time, and the way in which the background near analytical lines is taken into account). The relative standard deviation in the results of Y, Yb, and Nb determinations in the ceramic samples did not exceed 0.66% and the relative error was no greater than 1.63%. The results we obtained were compared to calculated percentages of the analytes in stoichiometric samples and to analytical data obtained for the ceramic samples by inductively coupled plasma optical emission spectroscopy. The proposed technique allows major components of ceramic samples to be determined and can be used for analytical monitoring of the rare-earth paraniobate synthesis process.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"60 3","pages":"334 - 341"},"PeriodicalIF":0.9,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143533175","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}