Pub Date : 2024-05-23DOI: 10.26896/1028-6861-2024-90-5-20-26
T. Chervonnaya, T. N. Musorina, Z. Temerdashev, V. N. Bekhterev, I. Korpakova
A method for determining polychlorinated biphenyls (PCBs) in water using the method of concentrating analytes through extractive freezing-out under the effect of a centrifugal forces (EFC) has been developed. A mathematical model for analyte extraction using a three-factor Box-Behnken design demonstrated that the content of acetonitrile in the extraction mixture is a significant factor, whereas the degree of PCBs chlorination and the concentration of analytes are insignificant parameters. Analysis of the surface area of the model allowed the determination of the optimal range of the acetonitrile concentration, which fell between 14 and 21%. A 15% content of acetonitrile in the extraction mixture provided maximum extraction efficiency for 7 different PCBs (>92%) across a wide range of analyte concentrations (1.0 – 5000 ng/liter). The relative standard deviations in the repeatability and reproducibility range from 4.2 to 6.8% and 5.3 to 8.1%, respectively, the accuracy of analyte determination being 10 – 15%. Petroleum hydrocarbons were not extracted into the acetonitrile extract and did not interfere with the determination of PCBs, which provided longer operation of the detector without any loss in the sensitivity. Co-extraction of polycyclic aromatic hydrocarbons and chlorinated pesticides did not affect the extraction of PCBs from water (95 – 100%) and did not touch on the metrological indicators of the determination procedure.
{"title":"GC-MS determination of polychlorinated biphenyls in water using extractive freezing-out of analytes","authors":"T. Chervonnaya, T. N. Musorina, Z. Temerdashev, V. N. Bekhterev, I. Korpakova","doi":"10.26896/1028-6861-2024-90-5-20-26","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-5-20-26","url":null,"abstract":"A method for determining polychlorinated biphenyls (PCBs) in water using the method of concentrating analytes through extractive freezing-out under the effect of a centrifugal forces (EFC) has been developed. A mathematical model for analyte extraction using a three-factor Box-Behnken design demonstrated that the content of acetonitrile in the extraction mixture is a significant factor, whereas the degree of PCBs chlorination and the concentration of analytes are insignificant parameters. Analysis of the surface area of the model allowed the determination of the optimal range of the acetonitrile concentration, which fell between 14 and 21%. A 15% content of acetonitrile in the extraction mixture provided maximum extraction efficiency for 7 different PCBs (>92%) across a wide range of analyte concentrations (1.0 – 5000 ng/liter). The relative standard deviations in the repeatability and reproducibility range from 4.2 to 6.8% and 5.3 to 8.1%, respectively, the accuracy of analyte determination being 10 – 15%. Petroleum hydrocarbons were not extracted into the acetonitrile extract and did not interfere with the determination of PCBs, which provided longer operation of the detector without any loss in the sensitivity. Co-extraction of polycyclic aromatic hydrocarbons and chlorinated pesticides did not affect the extraction of PCBs from water (95 – 100%) and did not touch on the metrological indicators of the determination procedure.","PeriodicalId":13559,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-05-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141105705","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-05-22DOI: 10.26896/1028-6861-2024-90-5-5-11
A. Belozerova, A. Mayorova, M. N. Bardina
Direct determination of the content of selenium and tellurium impurities in metallurgical materials by the method of inductively coupled plasma atomic emission spectroscopy (ICP-AES) is difficult due to spectral and non-spectral interference from macrocomponents present in the materials under study. The separation of micro-(Se, Te) and macro-components (Fe, W, Mo, Cr, Cu, Ni, Co) through preliminary precipitation is the goal of the study. The use of barium acetate and sodium fluoride as precipitants are shown to provide an effective separation of Se and Te from Fe, W, Mo, and Cr (the content in the analyzed solution is less than 0.1 wt.% of the original) and partial separation from Cu, Ni, and Co (the content in the analyzed solution from 25 to 55 wt.% of the original). Optimal conditions for the deposition of macrocomponents (Fe, W, Mo, Cr) and inhibition of the process of coprecipitation of selenium and tellurium on sediments of macrocomponents for their subsequent ICP-AES determination were determined. The optimal pH for the precipitation of macrocomponents equals 1. The optimal mass of precipitants (barium acetate and sodium fluoride) is 10 and 3 g, respectively. To inhibit the process of coprecipitation of selenium and tellurium on sediments of macrocomponents, it is proposed to use hydrofluoric acid. The optimal volume of hydrofluoric and hydrochloric acids for inhibiting the process of coprecipitation of analytes on sediments of macrocomponents was determined (3 and 6 cm3, respectively). The developed procedure for separating micro-Se, Te from macro-components was tested on standard samples of alloyed steels using the «spike» method. The technique is characterized by satisfactory accuracy and reproducibility, the limit of determination of analytes after separation of macrocomponents is 10–3 wt.%.
由于所研究材料中存在的宏观成分在光谱和非光谱方面的干扰，采用电感耦合等离子体原子发射光谱法（ICP-AES）直接测定冶金材料中的硒和碲杂质含量非常困难。本研究的目标是通过初步沉淀分离微量成分（Se、Te）和宏观成分（Fe、W、Mo、Cr、Cu、Ni、Co）。研究表明，使用醋酸钡和氟化钠作为沉淀剂可有效地将 Se 和 Te 与 Fe、W、Mo 和 Cr 分离（分析溶液中的含量小于原始含量的 0.1%），并将部分 Se 和 Te 与 Cu、Ni 和 Co 分离（分析溶液中的含量为原始含量的 25 至 55%）。确定了大分子成分（铁、钨、钼、铬）沉淀的最佳条件，以及抑制硒和碲在大分子成分沉淀物上共沉淀的过程，以便随后进行 ICP-AES 测定。大分子沉淀的最佳 pH 值等于 1。沉淀剂（醋酸钡和氟化钠）的最佳质量分别为 10 克和 3 克。为抑制硒和碲在大分子沉积物上的共沉淀过程，建议使用氢氟酸。确定了氢氟酸和盐酸抑制大分子沉积物上分析物共沉淀过程的最佳体积（分别为 3 和 6 立方厘米）。使用 "尖峰 "法在合金钢标准样品上测试了所开发的从宏观成分中分离微量硒、碲的程序。该技术具有令人满意的准确性和可重复性，分离宏观成分后分析物的测定极限为 10-3 wt.%。
{"title":"A technique for depositing iron, tungsten, molybdenum, and chrome in the determination of selenium and tellurium in alloy steel by ICP-AES method","authors":"A. Belozerova, A. Mayorova, M. N. Bardina","doi":"10.26896/1028-6861-2024-90-5-5-11","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-5-5-11","url":null,"abstract":"Direct determination of the content of selenium and tellurium impurities in metallurgical materials by the method of inductively coupled plasma atomic emission spectroscopy (ICP-AES) is difficult due to spectral and non-spectral interference from macrocomponents present in the materials under study. The separation of micro-(Se, Te) and macro-components (Fe, W, Mo, Cr, Cu, Ni, Co) through preliminary precipitation is the goal of the study. The use of barium acetate and sodium fluoride as precipitants are shown to provide an effective separation of Se and Te from Fe, W, Mo, and Cr (the content in the analyzed solution is less than 0.1 wt.% of the original) and partial separation from Cu, Ni, and Co (the content in the analyzed solution from 25 to 55 wt.% of the original). Optimal conditions for the deposition of macrocomponents (Fe, W, Mo, Cr) and inhibition of the process of coprecipitation of selenium and tellurium on sediments of macrocomponents for their subsequent ICP-AES determination were determined. The optimal pH for the precipitation of macrocomponents equals 1. The optimal mass of precipitants (barium acetate and sodium fluoride) is 10 and 3 g, respectively. To inhibit the process of coprecipitation of selenium and tellurium on sediments of macrocomponents, it is proposed to use hydrofluoric acid. The optimal volume of hydrofluoric and hydrochloric acids for inhibiting the process of coprecipitation of analytes on sediments of macrocomponents was determined (3 and 6 cm3, respectively). The developed procedure for separating micro-Se, Te from macro-components was tested on standard samples of alloyed steels using the «spike» method. The technique is characterized by satisfactory accuracy and reproducibility, the limit of determination of analytes after separation of macrocomponents is 10–3 wt.%.","PeriodicalId":13559,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141108535","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-05-22DOI: 10.26896/1028-6861-2024-90-5-12-19
A. A. Arkhipenko, G. E. Marina, V. B. Baranovskaia, M. A. Ryumin
A two-stage technique for X-ray fluorescence analysis of ceramic samples of composition Y3–xYbxNbO7 (where x = 0 – 3) has been developed. At the first stage, using the method of fundamental parameters (FPM), a rapid semi-quantitative analysis of ceramic samples and products of intermediate synthesis was carried out to determine their preliminary composition. At the second stage, the quantitative composition of the samples was determined using the constructed calibration dependencies. To construct calibration dependencies a series of reference samples containing 3.16 – 56.55% Y, 8.78 – 71.0% Yb, and 12.83 – 19.70% Nb was synthesized using a method similar to that used for preparation of the ceramic samples under study. Analytical lines of elements free from spectral overlaps and XRF conditions (current and voltage of an X-ray tube, exposure time, method of taking into account the background near the analytical line) were selected. The relative standard deviation of the results of Y, Yb, and Nb determination in ceramic samples did not exceed 0.66%, the relative error was no more than 1.63%. The results obtained were compared with the calculated content of analytes in the samples of stoichiometric composition and with the results of ICP-AES analysis of real ceramic samples. The developed technique provides determination of the main components of ceramic samples and can be used for analytical control of synthesis of rare earth paraniobates.
{"title":"X-Ray fluorescence analysis of paraniobate based ceramics of composition Y3–xYbxNbO7","authors":"A. A. Arkhipenko, G. E. Marina, V. B. Baranovskaia, M. A. Ryumin","doi":"10.26896/1028-6861-2024-90-5-12-19","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-5-12-19","url":null,"abstract":"A two-stage technique for X-ray fluorescence analysis of ceramic samples of composition Y3–xYbxNbO7 (where x = 0 – 3) has been developed. At the first stage, using the method of fundamental parameters (FPM), a rapid semi-quantitative analysis of ceramic samples and products of intermediate synthesis was carried out to determine their preliminary composition. At the second stage, the quantitative composition of the samples was determined using the constructed calibration dependencies. To construct calibration dependencies a series of reference samples containing 3.16 – 56.55% Y, 8.78 – 71.0% Yb, and 12.83 – 19.70% Nb was synthesized using a method similar to that used for preparation of the ceramic samples under study. Analytical lines of elements free from spectral overlaps and XRF conditions (current and voltage of an X-ray tube, exposure time, method of taking into account the background near the analytical line) were selected. The relative standard deviation of the results of Y, Yb, and Nb determination in ceramic samples did not exceed 0.66%, the relative error was no more than 1.63%. The results obtained were compared with the calculated content of analytes in the samples of stoichiometric composition and with the results of ICP-AES analysis of real ceramic samples. The developed technique provides determination of the main components of ceramic samples and can be used for analytical control of synthesis of rare earth paraniobates.","PeriodicalId":13559,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141111622","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-04-22DOI: 10.26896/1028-6861-2024-90-4-66-74
A. A. Khlybov, D. Ryabov, A. A. Solovyov
{"title":"Application of the magnetic method to control the deformed state of ER308LSI steel samples obtained by additive growing","authors":"A. A. Khlybov, D. Ryabov, A. A. Solovyov","doi":"10.26896/1028-6861-2024-90-4-66-74","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-4-66-74","url":null,"abstract":"","PeriodicalId":13559,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140676681","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-04-22DOI: 10.26896/1028-6861-2024-90-4-75-82
A. Sterlin, E. A. Surkov, I. S. Ivanushkin
{"title":"Method for extending the frequency range of sound generators for strength acoustic tests","authors":"A. Sterlin, E. A. Surkov, I. S. Ivanushkin","doi":"10.26896/1028-6861-2024-90-4-75-82","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-4-75-82","url":null,"abstract":"","PeriodicalId":13559,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140673123","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-04-21DOI: 10.26896/1028-6861-2024-90-4-40-45
A. A. Galkin, Yu.S. Mordovina, M. Anosov, D. Shatagin
{"title":"Study of the mechanical properties and the microstructure of welded joints made of structural high-strength steels S690QL of Russian and foreign origin","authors":"A. A. Galkin, Yu.S. Mordovina, M. Anosov, D. Shatagin","doi":"10.26896/1028-6861-2024-90-4-40-45","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-4-40-45","url":null,"abstract":"","PeriodicalId":13559,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-04-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140678122","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-04-21DOI: 10.26896/1028-6861-2024-90-4-31-39
R. K. Vagapov, O. G. Mikhalkina
{"title":"Research of precipitations in assessing the causes of corrosion at gas facilities","authors":"R. K. Vagapov, O. G. Mikhalkina","doi":"10.26896/1028-6861-2024-90-4-31-39","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-4-31-39","url":null,"abstract":"","PeriodicalId":13559,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-04-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140677979","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-04-21DOI: 10.26896/1028-6861-2024-90-4-53-65
A. V. Nechaeva, V. Polyanskiy, A. Polyanskiy, V. V. Shalagaev, Yu. A. Yakovlev
{"title":"Root cause analysis of the brittle fracture of pipes of boiler heating surfaces after long-term operation","authors":"A. V. Nechaeva, V. Polyanskiy, A. Polyanskiy, V. V. Shalagaev, Yu. A. Yakovlev","doi":"10.26896/1028-6861-2024-90-4-53-65","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-4-53-65","url":null,"abstract":"","PeriodicalId":13559,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-04-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140678655","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-04-21DOI: 10.26896/1028-6861-2024-90-4-46-52
A. S. Dmitriev, A. D. Kuleshov, N. N. Potrakhov, Y. Potrakhov, K. K. Guk
{"title":"High-voltage power supply for x-ray control of the structure of materials","authors":"A. S. Dmitriev, A. D. Kuleshov, N. N. Potrakhov, Y. Potrakhov, K. K. Guk","doi":"10.26896/1028-6861-2024-90-4-46-52","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-4-46-52","url":null,"abstract":"","PeriodicalId":13559,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-04-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140678810","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-04-20DOI: 10.26896/1028-6861-2024-90-4-5-11
E. G. Kulapina, R. K. Mursalov, O. I. Kulapina
{"title":"The effect of magnetic nanoparticles and cetylpyridinium chloride on the electroanalytical properties of planar sensors sensitive to cefuroxime and cefotaxime","authors":"E. G. Kulapina, R. K. Mursalov, O. I. Kulapina","doi":"10.26896/1028-6861-2024-90-4-5-11","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-4-5-11","url":null,"abstract":"","PeriodicalId":13559,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-04-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140679850","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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