Determination of the diethylene glycol content, isophthalic acid content, intrinsic viscosity (ASTM D4603), and the acid number (AN) of polyethylene terephthalate (PET) is a lengthy and challenging process due to the sample’s limited solubility and the need to use different analytical methods.
This application note demonstrates that the DS2500 Solid Analyzer operating in the visible and near-infrared spectral region (Vis-NIR) provides a cost-efficient and fast solution for a simultaneous determination of the diethylene glycol content, isophthalic acid content, intrinsic viscosity, and the acid number in PET. Vis-NIR spectroscopy allows for the analysis of PET in less than one minute without sample preparation or using any chemical reagents.
PET pellets were measured with a DS2500 Solid Analyzer in reflection mode over the full wavelength range (400–2500 nm). A rotating DS2500 Large Sample Cup was employed to overcome the distribution of varied particle sizes and chemical components. This allowed automated measurements at different sample locations for a reproducible spectrum acquisition. As displayed in Figure 1, samples were measured without any preparation step. The Metrohm software package Vision Air Complete was used for all data acquisition and prediction model development.
Equipment | Metrohm number |
---|---|
DS2500 Solid Analyzer | 2.922.0010 |
DS2500 Large Sample Cup | 6.7402.050 |
Vision Air 2.0 Complete | 6.6072.208 |
The obtained Vis-NIR spectra (Figure 2) were used to create prediction models for quantification of the diethylene glycol, isophthalic acid, intrinsic viscosity, and acid number. The quality of the prediction models was evaluated using correlation diagrams, which display the correlation between Vis-NIR prediction and primary method values. The respective figures of merit (FOM) display the expected precision of a prediction during routine analysis.
Result diethylene glycol content
Figures of merit | Value |
---|---|
R2 | 0.931 |
Standard error of calibration | 0.052% |
Standard error of cross-validation | 0.066% |
Result isophthalic acid content
Figures of merit | Value |
---|---|
R2 | 0.995 |
Standard error of calibration | 0.059% |
Standard error of cross-validation | 0.085% |
Result intrinsic viscosity
Figures of merit | Value |
---|---|
R2 | 0.873 |
Standard error of calibration | 0.0236 |
Standard error of cross-validation | 0.0238 |
Result acid value
Figures of merit | Value |
---|---|
R2 | 0.991 |
Standard error of calibration | 0.093 |
Standard error of cross-validation | 0.143 |
This study demonstrates the feasibility of NIR spectroscopy for the analysis of key quality parameters of PET. In comparison to wet chemical methods (Table 6), the time to result is a major advantage of NIR spectroscopy, since all parameters are determined in a single measurement in under a minute.
Parameter | Method | Time to result |
---|---|---|
Diethylene glycol | Extraction + analysis HPLC-MS | ∼45 min (preparation) + ∼40 min (HPLC) |
Isophthalic acid | Dissolve + HPLC | ∼45 min (preparation) + ∼40 min (HPLC) |
Intrinsic viscosity | Dissolve + viscometry | ∼90 min (preparation) + ∼1 min (viscometry) |
Acid Number | Dissolve + titration | ∼90 min (preparation) + ∼10 min (titration) |