Although mounting evidence suggests the ubiquity of microplastic in aquatic ecosystems worldwide, our knowledge of its distribution in remote environments such as Polar Regions and the deep sea is scarce. Here, we analyzed nine sediment samples taken at the HAUSGARTEN observatory in the Arctic at 2340-5570 m depth. Density separation by MicroPlastic Sediment Separator and treatment with Fenton's reagent enabled analysis via Attenuated Total Reflection FTIR and μFTIR spectroscopy. Our analyses indicate the wide spread of high numbers of microplastics (42-6595 microplastics kg). The northernmost stations harbored the highest quantities, indicating sea ice as a possible transport vehicle. A positive correlation between microplastic abundance and chlorophyll a content suggests vertical export via incorporation in sinking (ice-) algal aggregates. Overall, 18 different polymers were detected. Chlorinated polyethylene accounted for the largest proportion (38%), followed by polyamide (22%) and polypropylene (16%). Almost 80% of the microplastics were ≤25 μm. The microplastic quantities are among the highest recorded from benthic sediments. This corroborates the deep sea as a major sink for microplastics and the presence of accumulation areas in this remote part of the world, fed by plastics transported to the North via the Thermohaline Circulation.

Environmental context. Microplastics are of increasing environmental concern following reports that they occur worldwide from the arctic to the deep sea. However, a reliable methodology that facilitates an automated measurement of abundance and identity of microplastics is still lacking. We present an analytical protocol that applies focal plane array detector-based infrared imaging of microplastics enriched on membrane filters applicable to investigations of microplastic pollution of the environment.Abstract. The pollution of the environment with microplastics (plastic pieces ,5 mm) is a problem of increasing concern. However, although this has been generally recognised by scientists and authorities, the analysis of microplastics is often done by visual inspection alone with potentially high error rates, especially for smaller particles. Methods that allow for a fast and reliable analysis of microplastics enriched on filters are lacking. Our study is the first to fill this gap by using focal plane array detector-based micro-Fourier-transform infrared imaging for analysis of microplastics from environmental samples. As a result of our iteratively optimised analytical approach (concerning filter material, measuring mode, measurement parameters and identification protocol), we were able to successfully measure the whole surface (>10-mm diameter) of filters with microplastics from marine plankton and sediment samples. The measurement with a high lateral resolution allowed for the detection of particles down to a size of 20 mm in only a fractional part of time needed for chemical mapping. The integration of three band regions facilitated the pre-selection of potential microplastics of the ten most important polymers. Subsequent to the imaging the review of the infrared spectra of the pre-selected potential microplastics was necessary for a verification of plastic polymer origin. The approach we present here is highly suitable to be implemented as a standard procedure for the analysis of small microplastics from environmental samples. However, a further automatisation with respect to measurement and subsequent particle identification would facilitate the even faster and fully automated analysis of microplastic samples.

We present an automated approach to reduce the time demand currently needed for data analyses. We have developed a novel analysis pipeline, followed by image analysis with Python and Simple ITK image processing modules.

The identification of microplastics becomes increasingly challenging with decreasing particle size and increasing sample heterogeneity. The analysis of microplastic samples by Fourier transform infrared (FTIR) spectroscopy is a versatile, bias-free tool to succeed at this task. In this study, we provide an adaptable reference database, which can be applied to single-particle identification as well as methods like chemical imaging based on FTIR microscopy. The large datasets generated by chemical imaging can be further investigated by automated analysis, which does, however, require a carefully designed database. The novel database design is based on the hierarchical cluster analysis of reference spectra in the spectral range from 3600 to 1250 cm−1. The hereby generated database entries were optimized for the automated analysis software with defined reference datasets. The design was further tested for its customizability with additional entries. The final reference database was extensively tested on reference datasets and environmental samples. Data quality by means of correct particle identification and depiction significantly increased compared to that of previous databases, proving the applicability of the concept and highlighting the importance of this work. Our novel database provides a reference point for data comparison with future and previous microplastic studies that are based on different databases. Graphical abstractᅟ Electronic supplementary materialThe online version of this article (10.1007/s00216-018-1156-x) contains supplementary material, which is available to authorized users.

Microplastics (MPs, <5 mm) have been reported as emerging environmental contaminants, but reliable data are still lacking. We compared the two most promising techniques for MP analysis, namely, Raman and Fourier transform infrared (FTIR) spectroscopy, by analyzing MPs extracted from North Sea surface waters. Microplastics >500 μm were visually sorted and manually analyzed by μ-Raman and attenuated total reflection (ATR)-FTIR spectroscopy. Microplastics ≤500 μm were concentrated on gold-coated filters and analyzed by automated single-particle exploration coupled to μ-Raman (ASPEx-μ-Raman) and FTIR imaging (reflection mode). The number of identified MPs >500 μm was slightly higher for μ-Raman (+23%) than ATR-FTIR analysis. Concerning MPs ≤500 μm, ASPEx-μ-Raman quantified two-times higher MP numbers but required a four-times higher analysis time compared to FTIR imaging. Because ASPEx-μ-Raman revealed far higher MP concentrations (38–2621 particles m–3) compared to the results of previous water studies (0–559 particles m–3), the environmental concentration of MPs ≤500 μm may have been underestimated until now. This may be attributed to the exceptional increase in concentration with decreasing MP size found in this work. Our results demonstrate the need for further research to enable time-efficient routine application of ASPEx-μ-Raman for reliable MP counting down to 1 μm.

Micro-Fourier transform infrared (micro-FTIR) spectroscopy and Raman spectroscopy enable the reliable identification and quantification of microplastics (MPs) in the lower micron range. Since concentrations of MPs in the environment are usually low, the large sample volumes required for these techniques lead to an excess of coenriched organic or inorganic materials. While inorganic materials can be separated from MPs using density separation, the organic fraction impedes the ability to conduct reliable analyses. Hence, the purification of MPs from organic materials is crucial prior to conducting an identification via spectroscopic techniques. Strong acidic or alkaline treatments bear the danger of degrading sensitive synthetic polymers. We suggest an alternative method, which uses a series of technical grade enzymes for purifying MPs in environmental samples. A basic enzymatic purification protocol (BEPP) proved to be efficient while reducing 98.3 ± 0.1% of the sample matrix in surface water samples. After showing a high recovery rate (84.5 ± 3.3%), the BEPP was successfully applied to environmental samples from the North Sea where numbers of MPs range from 0.05 to 4.42 items m. Experiences with different environmental sample matrices were considered in an improved and universally applicable version of the BEPP, which is suitable for focal plane array detector (FPA)-based micro-FTIR analyses of water, wastewater, sediment, biota, and food samples.

Recent studies have shown that despite its remoteness, the Arctic region harbors some of the highest microplastic (MP) concentrations worldwide. Here, we present the results of a sampling campaign to assess the vertical distribution of MP particles (>11 μm) at five stations of the HAUSGARTEN observatory. Water column samples were taken with large volume pumps by filtering 218−561 L of seawater at two to four depth strata (near-surface, ∼300 m, ∼1000 m, and above seafloor), and sediment samples were taken with a multiple corer. MP concentrations in the water column ranged between 0 and 1287 N m −3 and in the sediment from 239 to 13 331 N kg −1 . Fourier transform infrared spectroscopy (FTIR) imaging with automated data analysis showed that polyamide (39%) and ethylenepropylene-diene rubber (23%) were the most abundant polymers within the water samples and polyethylene-chlorinated (31%) in sediments. MPs ≤ 25 μm accounted for more than half of the synthetic particles in every sample. The largest MP particle recorded was in the 200 μm size class. The concentrations of fibers were not reported, as fiber detection by FTIR imaging was not available at the time of analyses. Two-and three-dimensional simulations of particle transport trajectories suggest different pathways for certain polymer types. A positive correlation between MP size composition and particulate organic carbon indicates interactions with biological processes in the water column.

Microplastic pollution within the marine environment is of pressing concern globally. Accordingly, spatial monitoring of microplastic concentrations, composition and size distribution may help to identify sources and entry pathways, and hence allow initiating focused mitigation. Spatial distribution patterns of microplastics were investigated in two compartments of the southern North Sea by collecting sublittoral sediment and surface water samples from 24 stations. Large microplastics (500−5000 µm) were detected visually and identified using attenuated total reflection (ATR) Fourier transform infrared (FTIR) spectroscopy. The remaining sample was digested enzymatically, concentrated onto filters and analyzed for small microplastics (11−500 µm) using Focal Plane Array (FPA) FTIR imaging. Microplastics were detected in all samples with concentrations ranging between 2.8-1188.8 particles kg-1 for sediments and 0.1-245.4 particles m-3 for surface waters. On average 98% of microplastics were <100 µm in sediments and 86% in surface waters. The most prevalent polymer types in both compartments were polypropylene, acrylates/polyurethane/varnish, and polyamide. However, polymer composition differed significantly between sediment and surface water samples as well as between the Frisian Islands and the English Channel sites. These results show that microplastics are not evenly distributed, in neither location nor size, which is illuminating regarding the development of monitoring protocols.