Using attenuated total reflection (ATR) Fourier transform infrared (FTIR) spectroscopy for direct quantitative analysis is highly desirable for many sample systems due to advantages such as rapid spectra collection and being completely non-destructive. However, for many complex sample matrices the feasibility of direct quantitative analysis using ATR-FTIR is uncertain. The commonly used Beer-Lambert law may not be applicable for many systems in general, besides sample related complexities such as inhomogeneity, variable optical properties, or heavily overlapping absorption bands. In this study, we consider fully formulated vulcanized rubber with carbon black or silica as the primary filler as our system of interest. We developed a method to simultaneously quantify the concentration of three different antidegradents of similar chemical structure directly on rubber samples using ATR-FTIR spectra. Results show that absorbance follows the Beer-Lambert law well for the range of antidegradent concentrations considered. Despite this, a direct application of the Beer-Lambert law to deconvolute overlapping peaks between antidegradents proved insufficient. Through the application of partial least squares (PLS) multivariate analysis, remarkable prediction accuracy of within about 0.15 wt% error for all three antidegradents was achieved for both types of rubber formulations, even with high levels of carbon black. These results show the value this method has for quantitative analysis of additives in rubber. Our investigation highlights the potential usefulness of FTIR spectroscopy in general for rapid quantitative analysis directly on samples of interest without any prior chemical separation.
Keywords: ATR-FTIR Spectroscopy; Chemometrics; Classical Least Squares; Partial Least Squares; Rubber.
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