A reliable method to determine airborne microplastics using quantum cascade laser infrared spectrometry.

The number of studies dealing with airborne microplastics (MPs) is increasing but sampling and sample treatment are not standardized, yet. Here, a fast and reliable method to characterize MPs is presented. It involves the study of two passive sampling devices to collect atmospheric bulk deposition (wet and dry deposition) and three digestion methods (two alkaline-oxidative and an oxidative) to treat the samples. The alkaline-oxidative method based on KOH and NaClO was selected for a mild organic matrix digestion. In addition, some operational parameters of a high-throughput quantum cascade laser-based infrared device (LDIR) were optimized: an effective automatic tiered approach to differentiate fibres from particles (>90 % success in validation) and a criterion to establish positive matches when comparing an unknown spectrum against the spectral database (proposed match index > 0.85). The procedural analytical recoveries were very good for particles (82-90 %) and slightly lower for fibres (62-73 %). Finally, the amount and type of MPs deposited at a sub-urban area NW Spain were evaluated. Most common polymers were Polyethylene (PE), Polypropylene (PP) and Polyethylene terephthalate (PET). The deposition rates ranged 98-1220 MP/m2/day, ca. 1.7 % of the total collected particles. More than 50 % of the total MPs deposited were in the 20-50 µm size range, whereas fibres were mostly in the 50-500 µm size range.

Supervised classification combined with genetic algorithm variable selection for a fast identification of polymeric microdebris using infrared reflectance.

Pollution caused by plastics and, in particular, microplastics has become a source of environmental concern for Society. Their ubiquity, with millions of tons of plastic debris spilled in both land and sea, requires efficient technological improvements in the ways residues are collected, handled, characterized and recycled. For reliable decision-making, dependable chemical information is essential to assess both the nature of the plastics found in the environment and their fate. In this work an efficient method to identify the polymeric composition of microplastic fragments is proposed. It combines infrared reflectance spectra and chemometric methods. A breakthrough result is that the models include polymers weathered under both dry (shoreline) and submerged (in sea water) conditions and, hence, they are very promising as a starting point for eventual practical applications. In addition, no spectral processing is required after the initial measurement. SYNOPSIS: This approach to identify microplastics in aquatic environments combines infrared measurements and multivariate data analysis to fight against (micro)plastic pollution.

Weathering-independent differentiation of microplastic polymers by reflectance IR spectrometry and pattern recognition.

The presence and effects of microplastics in the environment is being continuously studied, so the need for a reliable approach to ascertain the polymer/s constituting them has increased. To characterize them, infrared (IR) spectrometry is commonly applied, either reflectance or attenuated total reflectance (ATR). A common problem when considering field samples is their weathering and biofouling, which modify their spectra. Hence, relying on spectral matching between the unknown spectrum and spectral databases is largely defective. In this paper, the use of IR spectra combined with pattern recognition techniques (principal components analysis, classification and regression trees and support vector classification) is explored first time to identify a collection of typical polymers regardless of their ageing. Results show that it is possible to identify them using a reduced suite of spectral wavenumbers with coherent chemical meaning. The models were validated using two datasets containing artificially weathered polymers and field samples.

Monitorization of polyamide microplastics weathering using attenuated total reflectance and microreflectance infrared spectrometry.

The EU goal to reduce marine plastic litter by ca. 30% by 2020 stressed the need to deploy analytical methods to ascertain the polymeric nature of a residue. Furthermore, as plastics age under natural conditions and usual databases do not include their weathered spectra, (micro)plastics in environmental samples may be unidentified. In this paper, polyamide (nylon) microplastics weathering was monitored because of its ubiquity in household commodities, clothes, fishery items and industry, whose residues end up frequently in the environment. Infrared spectra (ATR and microreflectance) and Scanning Electron Microscopy (SEM) images were collected periodically while exposing nylon to controlled weathering. It was seen that ATR was more sensitive than microreflectance to monitor the structural evolution of polyamide and that the spectra and the surface of weathered microplastics showed remarkable differences with the pristine material, which stresses the need for considering its evolution when identifying microplastics in environmental studies. The evolution of six band ratios related to the chemical evolution of this polymer are presented. SEM images revealed the formation of secondary microplastics at the most advanced weathering stages of polyamide.

Standardization of the minimum information for publication of infrared-related data when microplastics are characterized.

Infrared spectrometry (IR) became a workhorse to characterize microplastics (MPs) worldwide. However, reports on the experimental conditions to measure them decreased alarmingly. As complete, relevant information on the instrumental setup determining IR spectra is crucial for scientific reproducibility, ca. 50% of the papers that reported FTIR to measure MPs were evaluated and it was found that most studies cannot be replicated due to missing experimental details. To ameliorate this, the most critical parameters influencing IR spectra are depicted, their impact when matching a spectrum against databases exemplified, and, following efforts from other scientific fields, a minimum information for publication of IR-related data on MPs characterization (MIPIR-MP) is proposed, along with a brief, simple paragraph to resume the most critical information to be reported. This can be used to improve the worrying figures that point out to a reproducibility crisis in the field, as disclosed by the survey.