{"title":"利用差示扫描量热法确定保护性油漆涂层固化程度的测试结果的重复性和再现性估算","authors":"M. M. Melnikov, Y. V. Prykina, Y. Z. Vagapova","doi":"10.26896/1028-6861-2024-90-3-39-44","DOIUrl":null,"url":null,"abstract":"The degree of curing of protective paint-and-varnish coatings for oil country tubular goods is a parameter characterizing the completeness of their polymerization, and allows drawing a conclusion about the final physicomechanical properties and the possibility of using the material under specific conditions. This parameter is considered decisive in conducting acceptance tests and incoming quality control of pipe products with plated protective epoxy coatings despite a low accuracy of the obtained results and the impact of various instrumental factors and methodological approaches. The authors have developed a methodology for determining the curing degree of coatings based on the procedures given in regulatory documents (CSA Z245.20 Series-18, GOST R ISO 21809-2), taking into account the analysis of factors affecting the results of determining the curing degree carried out in the previous work. According to the conducted studies, the rates of heating and cooling during the measurement process, the temperature test program (in particular, the presence and duration of isothermal exposures before heating cycles), and curve processing methods were corrected and selected in the proposed methodology. The aim of this work is the analysis of the precision of the developed method for determining the curing degree of protective coatings to confirm the high accuracy of the obtained values under observing the prescribed procedure. The analysis was carried out by statistical processing of the results obtained in comparative tests performed in four testing laboratories, and included calculation of the repeatability of the results by their standard deviation, reproducibility and assessment of the acceptability of these parameters. The developed procedure for determining the curing degree of protective coatings, from sampling to processing of DSC curves, showed good precision, which indicates the reproducibility and repeatability of the proposed method. The developed method can be used as a unified sequence for determining the curing degree of paints and varnishes used as protective coatings in different laboratories.","PeriodicalId":504498,"journal":{"name":"Industrial laboratory. 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引用次数: 0
摘要
石油国家管状产品保护性油漆和清漆涂层的固化程度是表征其聚合完全性的一个参数,可以对最终的物理机械性能和在特定条件下使用材料的可能性得出结论。尽管获得的结果准确性不高,而且受到各种仪器因素和方法的影响,但这一参数被认为是对带有电镀环氧保护涂层的管材产品进行验收测试和进货质量控制的决定性因素。作者根据规范性文件(CSA Z245.20 Series-18、GOST R ISO 21809-2)中给出的程序,并考虑到之前工作中对影响固化度测定结果的因素进行的分析,制定了一种测定涂层固化度的方法。根据所进行的研究,对测量过程中的加热和冷却速率、温度测试程序(特别是加热循环前等温暴露的存在和持续时间)以及曲线处理方法进行了修正,并在建议的方法中进行了选择。这项工作的目的是分析所开发的保护涂层固化度测定方法的精度,以确认在遵守规定程序的情况下获得的数值具有很高的准确性。分析是通过统计处理在四个测试实验室进行的对比测试所获得的结果来进行的,包括通过标准偏差计算结果的可重复性、可重复性和评估这些参数的可接受性。从取样到处理 DSC 曲线,所开发的确定保护涂层固化程度的程序显示出良好的精确性,这表明所建议的方法具有重现性和可重复性。所开发的方法可作为不同实验室测定用作保护涂层的油漆和清漆固化度的统一程序。
Estimation of the repeatability and reproducibility of test results in determining the degree of cure of protective paint coatings using differential scanning calorimetry
The degree of curing of protective paint-and-varnish coatings for oil country tubular goods is a parameter characterizing the completeness of their polymerization, and allows drawing a conclusion about the final physicomechanical properties and the possibility of using the material under specific conditions. This parameter is considered decisive in conducting acceptance tests and incoming quality control of pipe products with plated protective epoxy coatings despite a low accuracy of the obtained results and the impact of various instrumental factors and methodological approaches. The authors have developed a methodology for determining the curing degree of coatings based on the procedures given in regulatory documents (CSA Z245.20 Series-18, GOST R ISO 21809-2), taking into account the analysis of factors affecting the results of determining the curing degree carried out in the previous work. According to the conducted studies, the rates of heating and cooling during the measurement process, the temperature test program (in particular, the presence and duration of isothermal exposures before heating cycles), and curve processing methods were corrected and selected in the proposed methodology. The aim of this work is the analysis of the precision of the developed method for determining the curing degree of protective coatings to confirm the high accuracy of the obtained values under observing the prescribed procedure. The analysis was carried out by statistical processing of the results obtained in comparative tests performed in four testing laboratories, and included calculation of the repeatability of the results by their standard deviation, reproducibility and assessment of the acceptability of these parameters. The developed procedure for determining the curing degree of protective coatings, from sampling to processing of DSC curves, showed good precision, which indicates the reproducibility and repeatability of the proposed method. The developed method can be used as a unified sequence for determining the curing degree of paints and varnishes used as protective coatings in different laboratories.