{"title":"Bismuth Determination by Controlled-Potential Coulometry: Developing a Highly Accurate Procedure based on GET 176","authors":"V. M. Zyskin, A. В. Sobina","doi":"10.20915/2077-1177-2023-19-4-129-141","DOIUrl":"https://doi.org/10.20915/2077-1177-2023-19-4-129-141","url":null,"abstract":"In this work, we develop a procedure for reproducing the units of bismuth mass fraction in metallic bismuth and those of bismuth (III) mass concentration in bismuth nitrate solutions by controlled-potential coulometry based on the GET 176-2019 State primary standard of mass (molar, atomic) fraction units and mass (molar) concentration of components in liquid and solid substances and materials based on coulometry. The results obtained can be used when manufacturing certified reference materials (CRMs) for the composition of high-purity bismuth and CRMs for the composition of solutions of bismuth (III) ions directly traceable to GET 176-2019. These CRMs may find application in pharmacological, metallurgical, and nuclear industries.","PeriodicalId":486160,"journal":{"name":"Эталоны. Стандартные образцы","volume":"23 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-09-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135859786","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}
{"title":"A Comparative Analysis of OIML Documents and Russian Rules on the Use of Reference Materials","authors":"N. G. Oganyan, V. I. Dobrovolskiу","doi":"10.20915/2077-1177-2023-19-4-151-159","DOIUrl":"https://doi.org/10.20915/2077-1177-2023-19-4-151-159","url":null,"abstract":"The article analyzes the compliance of Russian legal documents with the Recommendations of the International Organization of Legal Metrology regarding the use of reference materials in the fields covered by the state control and supervision. The problem of ensuring the quality of measurement results is relevant for each laboratory, performing measurements in any fields of activity. In addition to a reliable and proven measurement method, a decisive role in obtaining comparable results is played by reference materials. In order to ensure the traceability of measurements, a reference material must be certified. Certified reference materials are obligatory for the state metrological control and supervision of the quality and safety of food and pharmaceutical products, quality of measurements in clinical laboratories, environmental safety, etc. Considering the important role of reference materials in the process of ensuring the uniformity of measurements in analytical laboratories, this study can contribute to the promotion of ideas for improving the Russian legislative framework in the relevant area.","PeriodicalId":486160,"journal":{"name":"Эталоны. Стандартные образцы","volume":"67 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-09-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135815957","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}
{"title":"Estimation of Uncertainty in Charpy Pendulum Impact Test Using the Reference Material","authors":"Iu. S. Chentsova, V. V. Tolmachev, A. A. Zabelina","doi":"10.20915/2077-1177-2023-19-4-143-150","DOIUrl":"https://doi.org/10.20915/2077-1177-2023-19-4-143-150","url":null,"abstract":"An urgent task for accredited testing laboratories is to estimate the uncertainty of test results. In Charpy pendulum impact test the sources of the main contributions from the measuring instrument to the uncertainty of the result are: the angle of rise and the angle of fall of the pendulum, force exerted by the pendulum, and the distance from the axis of rotation to the center of strike. The aim of the work is to describe the method for estimating the uncertainty of the results of Charpy pendulum impact test based on information about the calibration of the impact testing machine and traceability to the reference material of impact energy (absorbed energy) of steel grade 45 GSO 11934–2022. The uncertainty estimation method is based on the statistical model from ISO 21748–2017. Uncertainty estimation was carried out for a pendulum impact tester TE JBW-300 using GSO 11934–2022 type 11 samples according to GOST 9454–78 with a type V-notch concentrator at room temperature. The study found that the greatest contribution to the uncertainty of test results is made by a systematic error associated with traceability to CRM GSO 11934–2022 and a random component of measurements. Accounting of traceability to the CRM GSO 11934–2022 increases the estimate of the uncertainty of the result, but makes it possible to correctly compare the results of two different laboratories, which is of fundamental importance in arbitration tests.","PeriodicalId":486160,"journal":{"name":"Эталоны. Стандартные образцы","volume":"1 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-09-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135815498","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}
A. S. Sergeeva, A. V. Kasilyunas, E. G. Parfenova, S. V. Medvedevskikh
{"title":"Primary Reference Measurement Procedures in the Food Industry: Usage Experience and Development Prospects","authors":"A. S. Sergeeva, A. V. Kasilyunas, E. G. Parfenova, S. V. Medvedevskikh","doi":"10.20915/2077-1177-2023-19-4-83-98","DOIUrl":"https://doi.org/10.20915/2077-1177-2023-19-4-83-98","url":null,"abstract":"This article reviews the usage experience and development prospects of four state primary reference measurement procedures (SPRMPs) created to provide metrological support of measurements in the food and agricultural industries. The SPRMPS certified in 2016–2019 include those of the mass fraction of fat, ash, and carbohydrates in food products and raw materials; of the mass fraction of crude fat (oil content) in oilseeds and related products. The mass fraction of fat, crude fat, and oil content is measured using the Randall method; the mass fraction of ash is determined by the thermogravimetric method; the mass fraction of carbohydrates (total sugar) is defined by iodometric titration. The considered SPRMPs were used to develop reference materials (RMs) for the composition of dairy and meat, egg powder, starch, baby food, oilseeds, related products, and compound feeds. SPRMPs implementation required extending the range of the manufactured RMs for new product groups. High-precision procedures for measuring the mass fraction of fat in liquid dairy products, fish, pastry, confectionery, and pasta products, as well as the mass fraction of lactose in liquid dairy products were developed and certified to describe the characteristics of dairy, pollock fillets, and wheat crackers composition.","PeriodicalId":486160,"journal":{"name":"Эталоны. Стандартные образцы","volume":"38 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135926151","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}
{"title":"Study of Certified Reference Materials for Temperature and Specific Enthalpy of Phase Transitions of Metals and Metal Salts","authors":"A. M. Nepomiluev, A. P. Shipitsyn, A. E. Tyurnina","doi":"10.20915/2077-1177-2023-19-4-35-50","DOIUrl":"https://doi.org/10.20915/2077-1177-2023-19-4-35-50","url":null,"abstract":"The development of calibration procedures, as well as the certification of readily available reference materials (RMs) and the improvement of their metrological characteristics, are topical issues for thermal analysis methods. In the course of the work, the necessity of conducting a study in order to expand the range of CRMs for temperature and enthalpy of phase transitions is substantiated. The substantiation of the choice of the measurement procedure and starting materials is given. The conditions for conducting experiments are described in detail, and the choice of these conditions is justified. The developed CRMs passed the metrological examination and were included in the Register of approved types of reference materials FIF EUM as a set of certified reference materials for temperature and specific enthalpy of phase transitions (set SOTSF-2) GSO 11890–2022/GSO 11896–2022. The practical significance of the obtained results is as follows: certified reference materials allow expanding the possibility of establishing and monitoring the stability of the calibration characteristics of thermal analysis installations and measuring instruments; certification of measurement procedures (methods) and accuracy control of the measurement results of the phase transition temperature of metals, metal salts, metal oxides, and polymeric materials, organic and inorganic substances.","PeriodicalId":486160,"journal":{"name":"Эталоны. Стандартные образцы","volume":"39 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135926523","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}
E. V. Kulyabina, T. V. Kulyabina, T. V. Grebennikova, V. V. Morozova, V. Yu. Morozov
{"title":"Virus-like Particles: Properties and Characteristics of Reference Materials","authors":"E. V. Kulyabina, T. V. Kulyabina, T. V. Grebennikova, V. V. Morozova, V. Yu. Morozov","doi":"10.20915/2077-1177-2023-19-4-27-34","DOIUrl":"https://doi.org/10.20915/2077-1177-2023-19-4-27-34","url":null,"abstract":"Virus-like particles (VLPs) have long attracted the attention of biologists and metrologists due to their dual nature. Despite their similarity to viruses, VLPs lack a virus DNA or RNA, thereby posing no threat of infection. The development of methods for the creation and standardization of VLPs, as well as for monitoring their characteristics, represents an important problem in the field of biotechnology and molecular biology. In this work, we aim to substantiate the requirements, methods, and instruments used to ensure the traceability of VLP-based certified reference materials (CRMs). The following methods for characterization of biological and physicochemical properties of such CRMs were considered: mass balance; high-performance liquid chromatography-mass spectrometry (HPLC–MS); gas chromatography-mass spectrometry (GC–MS); Karl Fischer coulometric titration; ion chromatography; inductively coupled plasma mass spectrometry; and isotope dilution. It was established that VLP-based CRMs should meet the following requirements: the presence of molecular patterns common to many pathogenic biological agents (PBAs) but absent in the organism; traceability to SI units (Systeme international d’unites, SI); the absence of own genetic material; the presence only of inactivated homogenous strains when used for vaccine delivery. VLP-based CRMs facilitate metrological support in the field of medicine and vaccine production.","PeriodicalId":486160,"journal":{"name":"Эталоны. Стандартные образцы","volume":"28 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135926158","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}
{"title":"Ensuring the Uniformity of Measurements in the Field of Radiation Thermometry on the Basis of a New Definition of the Unit of Temperature","authors":"Iu. A. Sild","doi":"10.20915/2077-1177-2023-19-4-7-15","DOIUrl":"https://doi.org/10.20915/2077-1177-2023-19-4-7-15","url":null,"abstract":"Ensuring the uniformity of measurements (EUM) in the field of temperature measurements, in particular radiation thermometry is one of the main tasks of metrology solved at the state level. The system of metrological support (MS) of radiation thermometry means requires continuous maintenance at the level that meets modern requirements of science, technology, and industry. In order to develop and improve the EUM system in radiation thermometry, a number of measures have been taken in recent years, namely: a new standard base has been developed, including the creation of the State primary standard (SPS) of a temperature unit in the range from 0 °C to 3 200 °C, implementing a new definition of kelvin; a new State verification schedule (SVS) has been developed, which regulates the transfer of the temperature unit to working means from the SPS. To reduce the load on the SPS, decrease the loss of accuracy in the transfer of a unit of thermodynamic temperature and meet the increased requirements for metrological support of measuring instruments, a secondary standard (SS) of a temperature unit was created and studied in accordance with the new definition of kelvin. It included high-temperature blackbody based on fixed points of pure metals and eutectics, a blackbody and comparators that ensure the transfer of a temperature unit in the range from 961.78 °C to 3 200 °C. Based on the results of the research, the created State secondary standard (reference standard) of the temperature unit in the range from 961.78 °C to 3 200 °C was approved by the order of Rosstandart dated November 21, 2022 No. 2931 and fully meets the requirements in accordance with the SVS for temperature MI.","PeriodicalId":486160,"journal":{"name":"Эталоны. Стандартные образцы","volume":"53 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135925442","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}
{"title":"Reference Materials of Absorbed Dose: Expanding Dynamic Range and Improving Measurement Accuracy","authors":"V. P. Tenishev","doi":"10.20915/2077-1177-2023-19-4-63-71","DOIUrl":"https://doi.org/10.20915/2077-1177-2023-19-4-63-71","url":null,"abstract":"Establishment and control of metrological characteristics of measurements of absorbed ionizing radiation doses in the range of 0.01 and 200 kGy by reference materials is an urgent task due to their wide application in various industries. The most convenient means of metrological support for transferring a unit of absorbed dose rate of intense photon, electron, and beta radiation to measuring instruments in radiation technologies are reference materials with established metrological traceability to the International System of Units (SI). In the present study, a method for expanding the dynamic range of measuring the absorbed dose of high-intensity ionizing radiation by radiochromic film dosimetry systems was considered and tested. The accuracy (uncertainty) of dose measurements was estimated depending on the initial optical density of the radiation-sensitive layer of the radiochromic composition. The possibility of expanding the dose characteristics and improving the metrological characteristics of the existing reference materials of absorbed dose (in water) for use as secondary standards (Measures) of the absorbed dose of ionizing radiation reproducing and (or) storing one or more points of the selected measurement scale of the absorbed dose with increased accuracy (uncertainty) of the measured values of the absorbed dose (in water) in an extended dynamic range was shown.","PeriodicalId":486160,"journal":{"name":"Эталоны. Стандартные образцы","volume":"25 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135926156","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}
{"title":"Caffeine Quantification Via High-Precision Coulometric Titration","authors":"A. Yu. Shimolin","doi":"10.20915/2077-1177-2023-19-4-115-127","DOIUrl":"https://doi.org/10.20915/2077-1177-2023-19-4-115-127","url":null,"abstract":"Caffeine has traditionally been used to assess and control the metrological characteristics of liquid chromatographs. In recent years, with increasing requirements for the traceability of measurement results, the use of caffeine as a reagent for verification, calibration, and type approval tests has started to contradict the effective regulations governing measurement uniformity. This study aims to develop and test a procedure of caffeine quantification in caffeine via primary coulometric titration for the metrological support of high-performance liquid chromatography (HPLC) with an accuracy of no more than 1 % abs. In the course of work, a detailed analysis of methods for determining caffeine content in various matrices was carried out; in addition, a procedure for determining caffeine mass fraction in caffeine via coulometric titration was developed and tested. A comparison of the obtained results with caffeine mass fraction measurements performed using HPLC confirmed the commutativity of coulometric titration and HPLC. The developed procedure of caffeine quantification in caffeine via primary coulometric titration employing GET 176 can be used to develop a caffeine composition reference material and to provide metrological traceability of HPLC measurements on its basis to state primary standards reproducing the «mass fraction of components» and to SI units (Systeme international d’unites, SI).","PeriodicalId":486160,"journal":{"name":"Эталоны. Стандартные образцы","volume":"24 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135926150","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}
E. V. Kulyabina, A. E. Shchekotikhin, A. N. Tevyashova, T. V. Kulyabina, V. V. Morozova
{"title":"Reference Materials for the Composition of Antimicrobial Substances","authors":"E. V. Kulyabina, A. E. Shchekotikhin, A. N. Tevyashova, T. V. Kulyabina, V. V. Morozova","doi":"10.20915/2077-1177-2023-19-4-17-26","DOIUrl":"https://doi.org/10.20915/2077-1177-2023-19-4-17-26","url":null,"abstract":"The present study aims to generalize the experience of creating state reference materials (GSOs) of active substances and determine their main characteristics, standardized both in the State Pharmacopoeia of the Russian Federation and in the regulatory documents of the measurement uniformity assurance system. In connection with the violation of supply chains, the acquisition and use of foreign reference active substances became quite problematic or even impossible. As a consequence of the current difficult situation with the insufficient nomenclature of GSOs, the domestic manufacturers and developers faced urgent problems in creating them. The development of antimicrobial reference active substances will solve urgent issues of strengthening the technological sovereignty of Russia, minimize the import dependence of the Russian economy, as well as ensure the targets of the Strategy for Scientific and Technological Development of the Russian Federation to be achieved. The conclusions of the study can be applied in creating GSOs to substitute imported reference materials or surpass their level.","PeriodicalId":486160,"journal":{"name":"Эталоны. Стандартные образцы","volume":"49 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135925445","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}