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Identification and quantification of additives in bituminous binders based on FTIR spectroscopy and multivariate analysis methods
Materials and Structures ( IF 3.4 ) Pub Date : 2021-08-06 , DOI: 10.1617/s11527-021-01763-1
Sandra Weigel 1 , Christoph Recknagel 1 , Dietmar A. Stephan 1 , Michael Gehrke 2
Affiliation  

Bitumen is a crucial building material in road construction, which is exposed to continuously higher stresses due to higher traffic loads and changing climatic conditions. Therefore, various additives are increasingly being added to the bitumen complicating the characterisation of the bituminous binder, especially concerning the reuse of reclaimed asphalt. Therefore, this work aimed to demonstrate that the combination of Fourier transform infrared (FTIR) spectroscopy with attenuated total reflexion (ATR) technique and multivariate evaluation is a very well-suited method to reliable identify and quantify additives in bituminous binders. For this purpose, various unmodified and modified binders, directly and extracted from laboratory and reclaimed asphalts, were investigated with FTIR-ATR spectroscopy. The determined spectra, pre-processed by standard normal variate (SNV) transformation and the determination of the 1st derivation, were evaluated using factor analysis (FA), linear discriminant analysis (LDA) and partial least square regression (PLSR). With this multivariate evaluation, first, a significant model with a very high hit rate of over 90% was developed allowing for the identification of styrene-butadiene copolymers (SBC), ethylene-copolymer bitumen (ECB) and different waxes (e.g. amide and Fischer-Tropsch wax) even if the additives do not show any additional peaks or the samples are multi-modified. Second, a quantification of the content is possible for SBC, ECB, and amide wax with a mean error of RMSE ≤ 0.4 wt% and a coefficient of determination of R2 > 90%. Based on these results, FTIR identification and quantification of additives in bituminous binders is a very promising method with a great potential.



中文翻译:

基于 FTIR 光谱和多元分析方法的沥青结合料中添加剂的鉴定和定量

沥青是道路建设中的重要建筑材料,由于较高的交通负荷和不断变化的气候条件,沥青会承受持续较高的压力。因此,越来越多地将各种添加剂添加到沥青中,使沥青粘合剂的表征复杂化,尤其是关于再生沥青的再利用。因此,这项工作旨在证明傅里叶变换红外 (FTIR) 光谱与衰减全反射 (ATR) 技术和多变量评估的结合是一种非常适合可靠识别和量化沥青粘合剂中添加剂的方法。为此,使用 FTIR-ATR 光谱研究了直接从实验室和再生沥青中提取的各种未改性和改性粘合剂。确定的光谱,通过标准正态变量 (SNV) 变换预处理和确定一阶导数,使用因子分析 (FA)、线性判别分析 (LDA) 和偏最小二乘回归 (PLSR) 进行评估。通过这种多变量评估,首先,开发了一个具有超过 90% 的极高命中率的重要模型,允许识别苯乙烯-丁二烯共聚物 (SBC)、乙烯-共聚物沥青 (ECB) 和不同的蜡(例如酰胺和 Fischer -Tropsch 蜡),即使添加剂没有显示任何额外的峰或样品经过多次改性。其次,可以对 SBC、ECB 和酰胺蜡的含量进行量化,平均误差为 RMSE ≤ 0.4 wt%,测定系数为 使用因子分析 (FA)、线性判别分析 (LDA) 和偏最小二乘回归 (PLSR) 进行评估。通过这种多变量评估,首先,开发了一个具有超过 90% 的极高命中率的重要模型,允许识别苯乙烯-丁二烯共聚物 (SBC)、乙烯-共聚物沥青 (ECB) 和不同的蜡(例如酰胺和 Fischer -Tropsch 蜡),即使添加剂没有显示任何额外的峰或样品经过多次改性。其次,可以对 SBC、ECB 和酰胺蜡的含量进行量化,平均误差为 RMSE ≤ 0.4 wt%,测定系数为 使用因子分析 (FA)、线性判别分析 (LDA) 和偏最小二乘回归 (PLSR) 进行评估。通过这种多变量评估,首先,开发了一个具有超过 90% 的极高命中率的重要模型,允许识别苯乙烯-丁二烯共聚物 (SBC)、乙烯-共聚物沥青 (ECB) 和不同的蜡(例如酰胺和 Fischer -Tropsch 蜡),即使添加剂没有显示任何额外的峰或样品经过多次改性。其次,可以对 SBC、ECB 和酰胺蜡的含量进行量化,平均误差为 RMSE ≤ 0.4 wt%,测定系数为 开发了一个具有超过 90% 的极高命中率的重要模型,可以识别苯乙烯-丁二烯共聚物 (SBC)、乙烯-共聚物沥青 (ECB) 和不同的蜡(例如酰胺和费托蜡),即使添加剂没有显示任何额外的峰或样品被多次修改。其次,可以对 SBC、ECB 和酰胺蜡的含量进行量化,平均误差为 RMSE ≤ 0.4 wt%,测定系数为 开发了一个具有超过 90% 的极高命中率的重要模型,可以识别苯乙烯-丁二烯共聚物 (SBC)、乙烯-共聚物沥青 (ECB) 和不同的蜡(例如酰胺和费托蜡),即使添加剂没有显示任何额外的峰或样品被多次修改。其次,可以对 SBC、ECB 和酰胺蜡的含量进行量化,平均误差为 RMSE ≤ 0.4 wt%,测定系数为R 2  > 90%。基于这些结果,沥青结合料中添加剂的 FTIR 识别和定量是一种非常有前途的方法,具有很大的潜力。

更新日期:2021-08-10
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