Multi-Spectroscopic Characterization of MgO/Nylon (6/6) Polymer: Evaluating the Potential of LIBS and Statistical Methods

Abstract

The potential of using laser-induced breakdown spectroscopy (LIBS) in combination with various other spectroscopic and statistical methods was assessed for characterizing pure and MgO-doped nylon (6/6) organic polymer samples. The pure samples, obtained through a polycondensation chemical technique, were artificially doped with MgO prior to analysis for comparative purposes. These artificially doped samples served as crucial reference materials for comparative analysis and reference purposes. The LIBS studies were performed under local thermodynamic equilibrium (LTE) and optically thin plasma conditions. To assess the structural crystallinity of the nylon (6/6) polymer samples, X-ray diffraction (XRD) analysis, and Fourier transform infrared (FTIR) spectroscopy were employed to detect functional groups such as N-H, C-H, and C-N in the adsorbent polyamide nylon sample. Additionally, diffuse reflectance spectroscopy (DRS) analysis was conducted to investigate the effects of doping and temperature on the band gap and material reflectance across different sample temperatures. Chemical compositional analysis was performed using X-ray photoelectron spectroscopy (XPS) with the carbon C1s peak at 248.8 eV serving as a reference for spectrum calibration, along with energy-dispersive X-ray (EDX) analysis, which demonstrated good agreement between the techniques. To validate the different methodologies, the results obtained from CF-LIBS and EDX were compared with those from the standard inductively coupled plasma mass spectrometry (ICP-MS) technique. Finally, for classification analysis, principal component analysis (PCA) was applied to the LIBS spectral data at different sample temperatures (25 °C, 125 °C, 225 °C, and 325 °C). The analyses demonstrated that the combination of LIBS with PCA, along with other methods, presents a robust technique for polymer characterization.

Keywords

• polymer
• PCA
• laser-induced breakdown spectroscopy
• EDX
• XPS
• FTIR