Estimation of the repeatability and reproducibility of test results in determining the degree of cure of protective paint coatings using differential scanning calorimetry

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.