Feasibility of using quantitative 1H-NMR spectroscopy and ultra-microbalances for investigation of a PET microplastic reference material

Here, we report on the feasibility of using quantitative NMR and ultra-microbalances for additional measurements of the mass of poly-ethylene terephthalate (PET) particles in a reference material (RM). The microplastic (MP) PET particles were immobilised in solid NaCl following freeze-drying of a 1-ml NaCl suspension. The particles ranged from 30 to about 200 µm (Feret). In a 3-day process, more than 500 such units of PET particles in the NaCl carrier were prepared and later used in a large-scale inter-laboratory comparison. The homogeneity of PET in the salt carrier over these 500 units had previously been evaluated with respect to the mass of PET using an ultra-microbalance. In addition to the original results obtained by weighing, two independent results of quantitative H-NMR have been obtained for further investigation of this reference material together with one additional set of weighing data. The NMR data were used for confirmation of the weighed amount of PET (as weighing is non-specific for PET). Average masses of 0.293 ± 0.04 mg and 0.286 ± 0.03 mg of PET were obtained using two different ultra-microbalances (14% RSD for n = 14 and 9% RSD for n = 4, respectively). The corresponding H-NMR data was 0.300 ± 0.02 mg of PET (6.7% RSD for n = 5) and 0.345 ± 0.04 mg of PET (12.5% RSD for n = 14), respectively. The average mass of PET obtained by H-NMR measurements was in agreement with the weighed amounts within their standard deviations. A mean value of 0.306 mg PET with an expanded uncertainty of 0.058 mg (± 19% relative) was calculated, and it is traceable to the SI system of measurements. Measurement of PET by quantitative H-NMR spectroscopy is also reported for a water sample. The PET contained in one RM sample was transferred to 1 L of water to mimic a drinking water sample for microplastics.