Quantitative ¹H-NMR spectroscopy as an efficient method for identification and quantification of PVC, ABS and PA microparticles

Abstract

This work presents a new, size-independent, fast, mass based MP-analysis of PVC, ABS and PA 6.6 using quantitative 1H-NMR spectroscopy.

Applicable and cost‐efficient microplastic analysis by quantitative 1H‐NMR spectroscopy using benchtop NMR and NoD methods

“…DCM shows only one NMR signal with a chemical shift between 5.3 ppm (in CDCl 3 ) and 5.8 ppm (in DMSO-d 6 ). [24] Therefore, we did not expect interfering signal overlay for MP particles of the following polymer types: PET in CHCl 3 /TFA 4:1, PS in CHCl 3 , PVC in DMSO (for more information, see Peez et al [12,14] ).…”

“…Table 1 gives true values in mg/ml with the error as weighing error, calculated values with the error as CI, and the corresponding accuracy in % and precision in % of quantitative MP analysis using DCM as an IS for the NoD method, whereas LODs and LOQs are presented in Table 2 and compared to results of the D method obtained by already published methods. [12,14] Concentrations are calculated from calibration curves that link known concentrations from a dilution series of the respective polymer material with values of the integrals of signal intensities in NMR spectra. Accuracy is between 94.3% and 111% for all three polymer types, and thus there is no significant difference to the D experiments (94.1%-110%).…”

“…[6,11] On this basis, we have successfully introduced quantitative 1 H-NMR (qNMR) spectroscopy as a new mass-based MP quantification method. [12][13][14] The high accuracy and low error proneness of qNMR in the identification and quantification of MP particles (low-density polyethylene [LDPE], polyethylene terephthalate [PET], polystyrene [PS], polyvinylchloride [PVC], acrylonitrilebutadiene-styrene [ABS], and polyamide 6.6 [PA]), as our preliminary work has shown, clearly raise the question of further developing this method into a routinely applicable analytical technique. [12,14] This approach seems to be promising due to short measurement times (<5 min per measurement) and the method being largely insensitive to environmental matrix effects.…”

“…[12][13][14] The high accuracy and low error proneness of qNMR in the identification and quantification of MP particles (low-density polyethylene [LDPE], polyethylene terephthalate [PET], polystyrene [PS], polyvinylchloride [PVC], acrylonitrilebutadiene-styrene [ABS], and polyamide 6.6 [PA]), as our preliminary work has shown, clearly raise the question of further developing this method into a routinely applicable analytical technique. [12,14] This approach seems to be promising due to short measurement times (<5 min per measurement) and the method being largely insensitive to environmental matrix effects. [13,14] Nevertheless, with regard to the potential application of qNMR methods as a routine analytical technique, cost-efficiency still is a major problem.…”

“…[12,14] This approach seems to be promising due to short measurement times (<5 min per measurement) and the method being largely insensitive to environmental matrix effects. [13,14] Nevertheless, with regard to the potential application of qNMR methods as a routine analytical technique, cost-efficiency still is a major problem. This was already addressed in the before-mentioned review article by Primpke et al, who mentioned the costs for deuterated solvents as well as the high purchase and operating costs for high-field NMR devices (300-1,000 MHz) as a potential problem.…”