Inorganic Materials最新文献

{"title":"Flame Photometry Determination of Lithium and Calcium in Novel Hydroxyapatite-Based Materials for Osteoplasty","authors":"A. A. Fomina,&nbsp;A. Yu. Demina,&nbsp;N. A. Andreeva,&nbsp;T. N. Penkina,&nbsp;N. V. Petrakova,&nbsp;D. G. Filatova","doi":"10.1134/S002016852470047X","DOIUrl":"10.1134/S002016852470047X","url":null,"abstract":"<p>A technique has been proposed for flame photometry determination of lithium additions and calcium, a major component, in the synthesis of novel hydroxyapatite (HA) based materials in order to find relationships between synthesis conditions, the composition of the material, and its functional properties. Ceramic samples were prepared via coprecipitation with the use of lithium carbonate, followed by calcination at 1300°C. We synthesized materials containing 0.25 to 1 at % lithium. Some of the samples contained 0.25 to 1 at % cerium (Ce(NO₃)₃). Lithium in the HA samples was determined using the standard addition method and appropriate reference solutions. Calcium was determined in separate aliquots after a 50-fold dilution. The results demonstrate that lithium concentrations at a level of 0.1 mg/L in hydroxyapatite solutions can be determined by flame photometry with <i>S</i>_r = 0.1. The material is difficult to dope with lithium via coprecipitation from solution. Moreover, heat treatment in the synthesis process has no effect on its result. We propose codoping of the material with lithium and cerium, which ensures incorporation of at least 0.25 at % Li into the structure of HA. The proposed technique can be employed for lithium and calcium determination with the use of a PFA-378 flame photometer in all steps of synthesis of new HA-based materials.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"60 3","pages":"355 - 358"},"PeriodicalIF":0.9,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143533091","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":"Study of the Distribution of Microelements in Hydrocarbon Groups of Oil","authors":"D. I. Panyukova,&nbsp;K. Ossipov,&nbsp;T. A. Maryutina","doi":"10.1134/S0020168524700432","DOIUrl":"10.1134/S0020168524700432","url":null,"abstract":"<p>Information on the expanded microelement composition of oil from various classes has practical significance and is of interest for both scientific research and the development of technological processes for its refining. From a geochemical perspective, data on the features on the quantitative distribution of microelements in oil provide an opportunity to identify its genetic differences for oil exploration tasks. In the petrochemical industry, the results of analysis of microelement composition allow for assessing the oil composition at the production stage and monitoring the quality of the obtained products at different stages of refining. In this study, the distribution of microelements in hydrocarbon groups (SARA groups) was investigated using two samples of commercial oil of Russian origin differing in physicochemical properties (heavy high-viscosity and bituminous super-viscous). The content of microelements in the oil samples, comprising their maltenes and asphaltenes, as well as in paraffinic–naphthenic hydrocarbons, aromatic hydrocarbons and resins, was determined using inductively coupled plasma mass spectrometry. These components, exept for asphaltenes, were isolated from the maltenes part using liquid adsorption chromatography according to the generally accepted research procedure developed by Joint-Stock Company VNII NP. It was found that most of the detected elements are present in the oil samples at levels more than 1.0, 0.1–1.0, and less than 0.1 μg/g. The concentrations of other elements were below the limits of detection (0.3–9 ng/g). On the basis of the results of analysis, it was established that both oils studied are enriched in microelements and belong to the “vanadium” type. The main trends in the distribution of microelements in hydrocarbon groups indicate their concentration within polar polycondensed structures (resins and asphaltenes).</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"60 3","pages":"279 - 285"},"PeriodicalIF":0.9,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143533092","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":"Application of Piezoelectric Sensors for the Determination of Aspartame in Fluids","authors":"A. Yu. Vybornyi,&nbsp;O. A. Shuvalova,&nbsp;A. N. Zyablov,&nbsp;Cao Nhat Linh","doi":"10.1134/S0020168524700365","DOIUrl":"10.1134/S0020168524700365","url":null,"abstract":"<p>A molecularly imprinted polymer (MIP) with an aspartame imprint is synthesized by noncovalent imprinting which is used to modify the surface of the electrode of a piezoelectric sensor. The values of the selectivity coefficients and imprinting factors of the developed MIP-E951 sensor in relation to target molecules and other sweeteners are calculated to confirm its ability to selectively detect aspartame. The range of determined concentrations is 1–1 × 10^–3 g/L; the detection limit of aspartame is 5 × 10^–4 g/L. When analyzing model solutions, it is found that foreign components usually present in soft drinks do not interfere with the determination of aspartame using the MIP sensor. The obtained results are compared with the data of the reference high performance liquid chromatography method: it is shown that the results of two methods are in a good agreement. The developed MIP sensor can be used for simple and rapid determination of aspartame in soft drinks.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"60 3","pages":"375 - 378"},"PeriodicalIF":0.9,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143533090","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":"Nondestructive Analysis of Fluoroquinolone Drugs by Colorimetric Method Using a Smartphone","authors":"V. G. Amelin,&nbsp;O. E. Emelyanov","doi":"10.1134/S0020168524700328","DOIUrl":"10.1134/S0020168524700328","url":null,"abstract":"<p>A method for nondestructive analysis of pharmaceuticals for the content of fluoroquinolones through diffuse reflection of infrared radiation using a smartphone and a device printed on a 3D printer has been proposed. It has been established that the diffuse reflection of infrared radiation with a wavelength of 850 nm from tablets containing active substances of the fluoroquinolone class can be captured using a smartphone camera. The blister packaging and the tablet coating do not hinder the passage of radiation, as confirmed by comparing the results of colorimetric determination of fluoroquinolones in drug samples both in packaging and without it, as well as on a split tablet. A correlation between the analytical signal and the concentration of the active substance is observed regardless of the variant of investigation. The possibility of using chemometric methods is demonstrated, which allows for reduced time of analysis and visualization of the obtained data. The data array was processed using principal component analysis (PCA), hierarchical cluster analysis (HCA), partial least squares regression (PLS), and the least squares method with the use of PhotoMetrix PRO^® software. Using these algorithms, the identification of drugs by their manufacturer was conducted. Colorimetric signals from tablets of the same manufacturer form distinct clusters on diagrams constructed using the HCA algorithm. Data obtained using PCA indicate the placement of signals from tablets of different manufacturers in separate quadrants, allowing for the identification of the pharmaceutical company and the country of manufacture. For example, the drug Ciprofloxacin with varying concentrations of the active substance produced in Russia is located in quadrants 2 and 4, while products manufactured in India are found in quadrants 1 and 3. The use of chemometric analysis methods for determining active substances is discussed in detail. The relative standard deviation of the analysis results did not exceed 0.07.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"60 3","pages":"270 - 278"},"PeriodicalIF":0.9,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143533093","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":"Improvement of Spark Atomic Emission Spectrometry for Determination of Oxysulfides in Structural Steel","authors":"E. A. Probenkova,&nbsp;E. V. Yakubenko,&nbsp;T. N. Ermolaeva,&nbsp;Yu. N. Orekhova","doi":"10.1134/S0020168524700456","DOIUrl":"10.1134/S0020168524700456","url":null,"abstract":"<p>We have studied conditions of oxysulfide determination in structural steel by spark atomic emission spectrometry (SAES) using an ARL iSpark Model 8860 spectrometer fitted with the Spark-DAT program option for spark diagram processing. In addition, to improve characteristics of calibration curves for determination of Al, Ca, Mn, and sulfur forming nonmetallic inclusions (NMIs), we used structural steel composition standards. The results demonstrate better sensitivity of Al and Ca determination and an increase in correlation coefficients of calibration curves for Mn and sulfur determination. Since no oxysulfide reference standards are available, the percentage of Al₂O₃MnS, Al₂O₃MnSMgO, Al₂O₃MnSCaS, Al₂O₃CaOCaS, Al₂O₃CaOMgOCaS in steel was pre-evaluated in accordance with the ASTM E1245 Standard (method 3) by scanning electron microscopy (SEM) with the use of an energy dispersive electron probe spectrometry (EDS) system. The results indicate that, in SAES determination of oxysulfides in structural steel, it is reasonable to use corrected algorithms for computer processing of the integrated spectrum, in combination with a pseudoformula. A proper algorithm and a pseudoformula for determination of each component were chosen with the use of Student’s <i>t</i>-test statistic by comparing the percentages of NMIs determined by SEM/EDS and SAES. We chose the spark range and analytical signal integration delay time for Al, Ca, Mg, Mn, and sulfur and confirmed the correctness of results of SAES determination of oxysulfides in the range from 500 to 1900 sparks (<i>t</i>_exp = 0.01) at a signal integration delay time of 110 μs (<i>t</i>_exp = 0.23). The technique for SAES determination of the total percentage of oxysulfides was tested in analysis of industrial structural steel samples. The results confirmed that there was no systematic error and that correct determination data were obtained (<i>t</i>_exp &lt; 4.30). The proposed technique for NMI determination allows the analysis time to be reduced from 18 h (SEM/EDS) to 10 min.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"60 3","pages":"259 - 269"},"PeriodicalIF":0.9,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143533173","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":"Validation of a Procedure for Determining Priority Phthalates by Gas Chromatography–Mass Spectrometry at a Trace Level of Concentrations in Surface Water with a Background Pollution Level","authors":"T. A. Grigoryeva,&nbsp;A. G. Gorshkov","doi":"10.1134/S0020168524700377","DOIUrl":"10.1134/S0020168524700377","url":null,"abstract":"<p>A procedure for determining trace concentrations of priority phthalates in surface waters with a background pollution level is validated. Lake Baikal, characterized by a minimal concentration of suspended organic matter, a low degree of mineralization, and a background level of concentrations of organic pollutants, is chosen as a natural model for the study. Four priority phthalates are found in Lake Baikal water: dimethyl phthalate, diethyl phthalate, di-<i>n</i>-butyl phthalate, and di-(2-ethylhexyl) phthalate present in a range of concentrations of 0.01 to 0.66 μg/L. The procedure for the determination of phthalates includes a single liquid–liquid extraction of phthalates (<i>V</i>_sample = 1 L) and a direct analysis of the extracts by gas chromatography–mass spectrometry. Considering the minimum concentration of suspended particles in the water and high sensitivity of mass spectrometry, stages of filtration of samples and concentration of extracts are excluded from the procedure. Deuterated phthalates are used as surrogate internal standards. The laboratory background of phthalates is assessed by conducting a control experiment and multiple extractions. The limits of determination of phthalates are assessed (0.01–0.17 μg/L); the error of determination is 12 to 38%. The procedure was validated during the monitoring of persistent organic substances in the Baikal water for the period of 2015–2023.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"60 3","pages":"379 - 387"},"PeriodicalIF":0.9,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143533086","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 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":"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":"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":"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}