Development of a Test Method for the Estimation of SBR-BR Blend Ratio in Tyre Tread Formulation and Validating It through Robust Statistical Tools

Tirthankar Bhandary, H. Satpathi, Aratrika Banerjee, Koushik Pal, Abhijit Pal, B. K. Samui, S. Dasgupta, R. Mukhopadhyay
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Abstract

Blends of synthetic rubbers are widely used by rubber product manufacturing industries depending on the end use and product application. The estimation of individual rubber in blends is an important aspect to characterise the correctness of the mixing process. In tyre industry, Styrene butadiene rubber/Polybutadiene rubber (SBR/BR) blend is commonly used to achieve different performance properties, particularly for passenger car tyre. Out of the different quantitative analysis techniques to characterise the blend, one of the widely used techniques Gas Chromatography-Mass Spectrometry (GC-MS) has been used to develop and later validate a method to quantify the SBR/BR blend ratio. Through this GC-MS technique detection capability is measured, with a minimum limit of detection (LOD) of 5.17% and a limit of quantification (LOQ) of 15.67% Styrene butadiene rubber (SBR) in an SBR-BR vulcanizate. It is observed that the bias percentage is highest in case of a lower SBR content sample, i.e. 11.1% while in the case of other sets, it is varying from (–)1.4% to (+)1.5%. During the recovery study, it is observed that with increasing SBR content, recovery is also improving. All requirements for a successful method validation: Accuracy, precision, selectivity, detection capability, calibration range and robustness have been carried out in this entire work.
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轮胎胎面配方中SBR-BR混合比估算测试方法的开发,并通过稳健统计工具进行验证
根据最终用途和产品应用的不同,合成橡胶的共混物在橡胶制品制造业中得到了广泛的应用。共混物中单个橡胶的估计是表征混炼过程正确性的一个重要方面。在轮胎工业中,常用丁苯橡胶/聚丁二烯橡胶(SBR/BR)共混物来获得不同的性能,特别是乘用车轮胎。在表征混合物的不同定量分析技术中,广泛使用的技术之一气相色谱-质谱(GC-MS)已被用于开发和验证一种量化SBR/BR混合比的方法。通过该GC-MS技术测定了SBR- br硫化胶中丁苯橡胶(SBR)的最小检测限(LOQ)为5.17%,定量限(LOQ)为15.67%。可以观察到,在SBR含量较低的样本中,偏差百分比最高,为11.1%,而在其他集合中,偏差百分比在(-)1.4%到(+)1.5%之间变化。在采收率研究中,观察到随着SBR含量的增加,采收率也在提高。成功验证方法的所有要求:准确性、精密度、选择性、检测能力、校准范围和鲁棒性在整个工作中都得到了满足。
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