Tirkey 2021

Marine Pollution Bulletin 170 (2021) 112604
Contents lists available at ScienceDirect
Marine Pollution Bulletin

journal homepage: www.elsevier.com/locate/marpolbul
Review
Microplastics: An overview on separation, identification and

characterization of microplastics
Anita Tirkey, Lata Sheo Bachan Upadhyay *
National Institute of Technology Raipur, Department of Biotechnology, Raipur, Chhattisgarh 492010, India
A R T I C L E I N F O A B S T R A C T
Keywords: At present plastic residues has become grave threat to the environment. Microplastics are plastic residues with a
Microplastics size <5 mm, due to their small size it is very difficult to remove them from water bodies, sediments and air with
Digestion available techniques. Nanoplastics are different in size range as nanoplastics are smaller than 1 μm in size. This
Density separation
review is an attempt to gather an insight towards microplastic and its associated point of concerns. The review
SEM
will highlight some of the methods appropriate for microplastics sampling and techniques for its identification in
FTIR
NIR environmental samples. Some of the sampling methods include sieving, filtration, visual sorting, digestion,
Raman spectroscopy density separation. While, identification techniques in practice are SEM-EDS, FTIR, NIR, Raman, NMR spec
qNMR troscopy, etc. Still there is a need and scope for development of more economical and portable techniques in this
direction.
1. Introduction These changes might impact their chemical and physical activities and
have an impact on environments and life forms (Rincon-Rubio et al.,
In the past few decades, microplastics and nanoplastics have 2001; Lambert and Wagner, 2016; Zettler et al., 2013; Rouillon et al.,
emerged as a global challenge due to an increase in worldwide plastic 2016). The presence of microplastics have not only been found in soil,
pollution rate with approximately 51 trillion microplastic particles (UN water, and air sources but also marine organisms, salt, beer, and very
News, n.d.) being reportedly present in the ocean which is affecting the recently in bottled drinking water globally (Desforges et al., 2015;
environment and biota adversely (Nguyen et al., 2019). Microplastics Gasperi et al., 2018; Kosuth et al., 2018; Schymanski et al., 2018).
are solid plastic particles of size ≤5 mm which are insoluble (Bergmann Microplastic on exposure may be accumulated and deposited in human
et al., 2015) in the aqueous environment. There is a broad classification tissue and body parts and can alter the immune system or may cause
of these small size plastic residues based on their size as; (i) large some other clinical complications (Wright and Kelly, 2017).
microplastics of size ranging between 5 mm to 1 mm, (ii) small micro In lower trophic level organisms, microplastics resemble prey
plastics of 1 mm to 1 μm size range, and (iii) nanoplastics of <1 μm size because of their minute size, due to which these organisms get confused
(Crawford and Quinn, 2017). Microplastics are not only of different sizes and they capture it and consume it, (Moore, 2008) making its
but are also of different shapes like microbeads, fibers, fragments, film bioavailability in the food web. For example, microplastics get trans
foam pellets, and filaments to mention some (Hidalgo-Ruz et al., 2012; ferred from algae to zooplanktons then to fish (Cedervall et al., 2012).
Wright et al., 2013). Based on their source of origin microplastics are The resemblance of microplastic residues as prey for zooplankton as a
divided into primary and secondary microplastics (Arthur et al., 2009). feed is due to their color. Generally, microplastics exhibit or appear
Primary microplastics are manufactured intentionally by industries for yellow, white, and tan color in the marine ecosystem and attract the
cosmetics purposes whereas secondary microplastics occur due to zooplanktons by appearing as a feed; via marine food chain finally they
weathering/degradation of plastic residues in the environment by wave become a part of commercially important fishes meant for human con
action, growth of bio-film, solar exposure, mechanical shear, and ther sumption (Shaw and Day, 1994). Once microplastics enter and accu
mal oxidation (Andrady, 2017). Continuous degradation of primary and mulate within the organism's body, they may cause physical harm such
secondary microplastics brings changes in their properties like color, the as internal scratches and blockings (Wright et al., 2013).
morphology of surface, size, crystallinity, and density as shown in Fig. 1. Likewise, Leaching chemicals from plastic additives and monomers
* Corresponding author.
E-mail address: lupadhyay.bt@nitrr.ac.in (L.S.B. Upadhyay).
https://doi.org/10.1016/j.marpolbul.2021.112604
Received 24 March 2021; Received in revised form 2 June 2021; Accepted 4 June 2021
Available online 16 June 2021
0025-326X/© 2021 Elsevier Ltd. All rights reserved.
A. Tirkey and L.S.B. Upadhyay Marine Pollution Bulletin 170 (2021) 112604
have the ability to trigger endocrine disruption and carcinogenesis 2. Sample preparation methods
(Wright et al., 2013). On entering the organism body they are subse
quently introduced as pollution to aquatic biota and later reaches to Being a global problem various studies have been conducted for
aquatic food web (Santana et al., 2017; Bakir et al., 2012). Microplastics sample preparation and identification of microplastics in biological as
are also prone to adsorb other toxins from their nearby environment well as water aliquots, but still there is a lacuna in the available protocol
(Holmes et al., 2012; Hodson et al., 2017; Fries and Zarfl, 2012; Kosuth to detect and characterize microplastics specifically (Rocha-Santos and
et al., 2018; Li et al., 2018) as they have an increased surface to volume Duarte, 2015). In the following sections of the paper, various methods
ratio and minute size. Sorption behavior of microplastics depends on have been demonstrated to process microplastics.
factors such as (i) the rubbery domains (high accessibility and mobility),
small size, large surface area, functional groups, age and polarity of
2.1. Physical method
microplastic residues (Hu et al., 2017; Zhang et al., 2018; Guo et al.,
2012; Luo et al., 2017; Guo et al., 2018), (ii) nature of pollutants i.e.,
Initial processing of microplastics is done either by sieving or visual
organic pollutants polarity, heavy metals and hydrophobicity (Hüffer
sorting after this density separation method is used. Visual sorting and
and Hofmann, 2016; Ziccardi et al., 2016) and (iii) aquatic environment
sieving is the ideal, convenient and inexpensive method for removal of
i.e. salinity, pH and dissolved organic matter (DOM) (Xu et al., 2018;
plant matter, sand gravel and organic matter and separate microplastics.
Crawford and Quinn, 2017). Old microplastics tend to adsorb more
Any type of distortion is not done in this process, as no chemicals are
toxins as compared to unadulterated microplastics (Brennecke et al.,
added. This process is carried out manually with a naked eye and great
2016; Müller et al., 2018; Guo and Wang, 2019). Due to lack of avail
acquisition and patience. In density separation microplastics are
ability of significant evidence, data and reports on the hazardous impact
removed on basis of plastics particle density, whereby the addition of
of microplastic on a human health regime, WHO has yet not listed
salt increases the density, which allows the floatation of lightweight
microplastics and microplastic sorbed with POPs (persistent organic
plastic. NaCl is the most recommended salt for density separation.
compounds) along with microbial pathogens bound microplastics in
drinking water as major distress for humankind (Pete Marsden et al.,
2.1.1. Sieving
2019). Primary objective of this review paper is to estimate various
It is the most basic method for microplastic separation from water
techniques used for sampling, identification and characterization of
samples using sieves of different types and mesh sizes. Materials that are
microplastics in water.
left on the top surface of the sieve on filtration are collected and passed
over particles are discarded. In some cases sieving to separate the
Fig. 1. Degradation of microplastics tend to alter its chemical and physical properties (modified from (Guo and Wang, 2019)).
2
microplastic component from the sample is performed with help of a hydrophobicity (Maes et al., 2017). However the method suffers from
single mesh size sieve while in certain cases 3 to 4 meshes are combined, some limitations, fibers are difficult to stain (Tamminga et al., 2017) and
this helps in size differentiation study. According to reports different low hydrophobic microplastics like Polycarbonate, Polyvinyl chloride,
types of sieve used in various studies are in the pore size range of 5 mm, Polyurethane and Polyethylene terephthalate are weakly fluoresced
1 mm, 335 μm, 330 μm, 80 μm, 0.2 μm (Tiwari et al., 2019; Wagner (Erni-Cassola et al., 2017).
et al., 2017; Jayasiri et al., 2013; Frère et al., 2016; Wang et al., 2017;
Foekema et al., 2013; Dris et al., 2015). 2.1.4. Density separation
This technique is used to segregate microplastic from sediments or
2.1.2. Filtration else from other inorganic substances which were not damaged in the
Filtration is a simple method where solids are separated from the chemical or enzymatic digestion (Stock et al., 2019). Density of plastic
liquid by use of a medium through which only liquid can pass. The pore (0.8–1.6 gcm− 3) is much lower than density of sediment (2.7 gcm− 3),
size of the filter paper determines the size of the solid is separated. this difference could be used to segregate microplastics from sediment.
Filtration is usually done by a funnel, filter membrane and vacuum In saturated salt solution sediment is cautiously mixed after some time
pump system (Crawford and Quinn, 2016). Filter membrane of different supernatant containing microplastics is separated and the remaining
pore sizes: 0.7 μm, 0.22 μm, 5 μm, 10 μm, 11 μm are used (Blair et al., solution is further filtered (Hidalgo-Ruz et al., 2012; Rocha-Santos and
2019; Coppock et al., 2017; Maes et al., 2017; Erni-Cassola et al., 2017; Duarte, 2015). Solutions with >1.4 g cm− 3 density are specified to
Karlsson et al., 2017; Cai et al., 2019). segregate microplastics from sediment. Density of microplastic is influ
Cloth shreds cellulose and synthetic fibers, which act as a potent enced by the concentration of additives, polymer type and by even
contaminant and could pass through the filtering membrane. During the adsorbed substances and organisms (Quinn et al., 2017). In this tech
transfer of the filter from the filtration setup into the petri plates, there nique, saturated salts solution or salt of high concentration is mixed with
could be a loss of microplastics. Nylon filter paper could also be a the sample in an appropriate volumetric ratio thoroughly mixed and left
possible contaminant. Therefore there is a risk of under or over- for density-based separation for a fixed time interval (Löder and Gerdts,
estimation of microplastics during the filtration process (Lares et al., 2015).
2019). In most of the studies NaCl solution(1.2 g/cm3) has been used for
density separation of microplastics from water samples, as it is the most
2.1.3. Visual sorting economical and reliable method recommended by MSFD Technical
Visual identification and separation are an important stage for Subgroup of Marine Litter and NOAA (Masura et al., 2015), however due
microplastic analysis, so that non-microplastic debris from the sample to low density of NaCl, high polymers like polyvinyl chloride and
can be removed easily. Such debris includes naturally occurring bio polyethylene terephthalate cannot be separated employing this method
logical remains, like shell fragments, seaweed, wood and man-made (J. Frias et al., 2018). Lower density polymers like polypropylene or
pollutants, like oil residues, paints and metals. It is done either by polyamide can be easily separated (Imhof et al., 2012). Thus to over
naked eyes or optical microscopy with help of the tweezers as a pre- come this limitation of NaCl other salts of high density (1.8 g/cm3) such
screening technique to reduce the number of particles that needed to as sodium iodide (NaI) has also been tested and used even though being
be analyzed thus minimize the chances of error. However it is difficult to expensive (Stock et al., 2019). Nuelle and co-workers developed a two-
distinguish microplastics from other material and hence it is very time- step density separation method in which, first the sample was fluidized
consuming, and often leads to misidentification (Wang et al., 2017; in NaCl solution which reduced the sample to 80%, then followed by
Hidalgo-Ruz et al., 2012; Tagg et al., 2015; Lusher et al., 2017; Wagner floatation with NaI solution, as the sample quantity has already been
et al., 2017). Sometimes shell fragments are mistaken as microplastics reduced small amount of NaI was required (Nuelle et al., 2014). Table 2
due to its white color, likewise brittle angular PE fragments would be summarizes the characteristics of different salts used in density sepa
mistaken for shell fragments, this shows that visual sorting may lead to ration methodology.
false positives or false negatives results (Wagner et al., 2017). Lithium metatungstate solution was suggested as another commer
There are some attributes that help to identify and separate the cially alternative separator by Masura (Masura et al., 2015) due to its
microplastics listed in Table 1, like structure and form of particle, greater density value (1.62 g cm− 3) in comparison to NaCl. Zinc chloride
hardness or elasticity of particle by using tweezers (Fries et al., 2013). (ZnCl2) is also considered as one of the best density separation salt,
Researchers have demonstrated and used some alternate methods to according to researchers flotation of Polyamide, Polystyrene, Polyvinyl
avoid misidentification like, the hot needle test in which needles are chloride, Polyethylene terephthalate, Polyethylene, and Polypropylene
used to prod the plastic particles (De Witte et al., 2014; Shim et al., is possible with solution of density 1.37 g mL− 1 with maximum recovery
2017). and minimum interference (Maes et al., 2017). Coppock et al. used
Fluorescence staining in which nile red is used to stain microplastics, sediment microplastic isolation (SMI) unit with ZnCl2 with a recovery
is a promising method in visual sorting as it helps in the identification of rate of 95.8% which is considerably high as compared to NaCl and NaI,
microplastics in orange, green or red filter under fluorescence micro and was also reported to be cost effective (Coppock et al., 2017). Quinn
scope (Erni-Cassola et al., 2017). Incubation time is short and it provides et al. found that recovery rate of NaCl and sodium bromide (NaBr) was
a high recovery rate and can be validated in IR spectroscopy, as being a low (<90%) with larger error bars, while recovery rates of both NaI and
solvatochromic dye, the fluorescence emissions depend upon solvent Zinc bromide (ZnBr2) was good (99%) with tight error bars and was able
polarity, thus microplastics can be categorized on the basis of its to segregate denser polymers. In addition, separation using NaCl and
NaBr salts entails thrice washing of the sediment, while NaI and ZnBr2
entails only s single wash which makes NaI and ZnBr2 suitable option for
Table 1 microplastic separation. But then NaI confounds visual sorting as it turns
Criteria for visual sorting of microplastics from samples (Crawford and Quinn, cellulose filters black and ZnBr2 is dangerous to the environment and
2017). costly, by adjusting the density and vigilant filtration, ZnBr2 can be
Categories Description reused (Quinn et al., 2017).
Size Macro(≥25 mm), Meso(<25 mm–5 mm), Micro(<5 mm-1 μm)
A novel method based on Wet Peroxide Oxidation in which 96%
Sources Primary(raw), secondary(fragmented) ethanol is used instead of salts for vegetal rich samples has been
Type fragments, pellets, films, fibers, microbead, foam described, the sample is mixed with ethanol stirred for 3 min at 600 rpm
Color transparent, white, red, orange, black, blue, opaque, gray, brown, and then allowed to settle. 97% of biogenic matter floats and get sepa
green, tan, yellow, pink
rated from microplastics which have been sunk to the bottom.
3
Table 2
Summary of different salts used for density separation method.
Salt Salt Advantages Disadvantages Reference
density
NaCl 1.2 g Cost-effective Polyvinyl chloride and polyethylene (Quinn et al., 2017;
cm3 Easy terephthalate not removed Claessens et al., 2011)
Recovers polystyrene, polyamide, polypropylene, polyvinyl chloride, and Multiple washing for recovery, Time
polyethylene consuming
Followed by FTIR/Raman separation
NaI 1.8 g Easy methodology Costly (Claessens et al., 2013)
cm3 Greater density than NaCl Blackens the cellulose filter, Difficult for
Recovers polystyrene, polyamide and polyvinyl chloride visual sorting
ZnCl2 1.7 g Recovers polyamide, polystyrene, polyvinyl chloride, polyethylene Hazardous and corrosive (Maes et al., 2017)
cm3 terephthalate, polyethylene, and polypropylene
Cheap
Recovery rate is upto 95%
ZnBr2 1.71 g Easy methodology Environmental hazardous, Expensive (Quinn et al., 2017)
cm3 Cost effective
Recovery rates of 99%
Recovers polypropylene, low density polyethylene, polyethylene, high
density polyethylene, polystyrene, polyvinyl chloride, polyethylene
terephthalate and polyamide
Lithium 1.62 g Easy methodology Costly (Quinn et al., 2017)
metatungstate cm3 Greater density than NaCl Unknown recovery rates
Recovers polyvinyl chloride, polyethylene terephthalate Unidentified Effect on polymers
Canola oil – Recovers polystyrene, polyvinyl chloride, polyester fiber, and polyamide, Additional cleaning for further analysis (Crichton et al., 2017)
recovery rate 96%
Cost effective
Ethanol 0.8 g Cost effective Not able to separate sediment from (Herrera et al., 2018)
cm3 Best method for separation from vegetal matter plastic
Recovers polypropylene, polyethylene, polystyrene, polyamide
Olive oil – Cost-effective Polytetrafluoroethylene was not (Scopetani et al.,
Recovers polystyrene, polyvinyl chloride, polyethylene terephthalate, removed 2020a)
polycarbonate, polyurethane
Recovery rate for low, medium and high density microplastics is up to
90–92%, 95–97% and 94–95%
Polystyrene expanded foam and extruded foam floats (as the density of rinsed three times and sonciated to remove all the attached micro
ethanol is 0.8 g/cm3 which is lower than plastics) with biogenic debris, plastics and further observed under the microscope. The recovery rate
but it was removed easily with forceps (Herrera et al., 2018). Canola oil for large microplastics (>1 mm) 93%, medium microplastics200μm-1
can also be used to segregate microplastics, as plastics are lipophilic in mm) 81% and small microplastics (<20 μ) 92% (Grbic et al., 2019).
nature, excessive oil can be removed by ethanol (Crichton et al., 2017).
Canola oil showed 92–97% recovery rate for various environmental 2.2. Chemical method
samples like seawater, beach sediments and shoreline. But there were
traces of canola oil on the microplastics, which hampers the identifica 2.2.1. Digestion of samples or pre-processing of sample
tion process further. This limitation was resolved by Scopteani et al., by For proper identification and characterization of the microplastic
using olive oil to separate microplastics from soil and compost samples. components of the water sample, a pre-processing step to remove other
They used PTFE cylinders in which sample and olive oil was mixed interfering organic matter becomes significant. There are chances that
vigorously, allowing it to settle for 2 h and frozen at − 40 ◦ C. From the ice microplastics are embedded inside the biological tissues of the sample,
column, oil layer can be removed easily and filtered through the filter and thus may not be detected and separated by physical method.
paper. The filter paper was rinsed with water and then with hexane to Overestimation is also a major issue in microplastic identification as
remove the oil traces. Olive oil showed a recovery rate of 90–92%, biotic substances are frequently confused with plastics. Hence, a diges
95–97% and 94–95% for low, medium and high-density microplastics tion method which has the ability to degrade biotic substance without
respectively (Scopetani et al., 2020a). Separation of high density altering the chemical or structural integrity of plastic particle is needed
microplastics is still challenging and use of different types of salt and (Prata et al., 2019).
chemicals does partial or complete degradation of microplastics, which
hinders further analysis. A novel separation technique was demon 2.2.2. Acid digestion
strated by Felsing et al. and his co-workers, they used an electrostatic Many acids like HCl, HNO3 are used for the dissolution of organic
separator to reduce the mass of the different types of samples. Here dry materials present in the sample before separation (Stock et al., 2019).
samples are passed through a vibrating conveyor, after that it was HNO3 is being demonstrated to be the best reagent for acid digestion of
electrostatically charged and separated on basis of their conduction biogenic compounds present in the sample during microplastic analysis
property in different sample collector according to their speed of experiments. On the other hand, much preference is not given to HCl
discharge. Biogenic matter and sediments being conductive discharge since it distorts the polyethylene terephthalate and polyvinyl chloride
early, while microplastics being non-conductive discharges slowly. surface (Karami et al., 2017), and HCl mediated acid digestion results
Electroseparation reduces the maximum sample volume and the recov are also inconsistent and inefficient to digest biogenic compound (Cole
ery rate of microplastics is almost 99%, making it a successful and et al., 2014; Foekema et al., 2013). Desforges in his study showed that
promising density separation technique (Felsing et al., 2018). Another one-hour treatment of sample with HNO3 result in complete dissolution
separation technique was developed by (Grbic et al., 2019) using hy of the zooplankton tissues, while a mixture of HNO3 and HCl broke the
drophobic Fe nanoparticles to magnetize various types of microplastics zooplankton body into smaller fragments (Desforges et al., 2015).
and by use of a magnet, microplastics are isolated. The magnet was
4
2.2.3. Alkali digestion 2017). Table 3 is a compilation of different digestion methods.

In this method, samples are digested using a strong alkali like NaOH
or KOH. The effect of strong alkali has been tested to check the suit 2.4. Self-contamination
ability for separation and identification of microplastic residues in bio
logical samples like marine organism body parts. Some fish were During the whole sampling process there are chances of self-
digested by adding 10 M KOH solution to the samples to collect contamination. Various studies have been conducted for microplastics
microplastics. This process is time taking as total organic matter was sampling, in which some of the studies are disputed and questioned for
digested in 2–3 weeks of time interval. According to studies, major types self –contamination. Scopetani et al. and co-workers validated in their
of microplastic residues released after digestion of biogenic organic work how self-contamination occurs from the researcher's garment, they
matter of the sample are resistant to KOH degradation except cellulose used cotton as the representative of synthetic fibers. In the study, sam
acetate based plastic material (Kühn et al., 2017). Karami et al., has plers intentionally wore red cotton, an old blue and a new bright pink
demonstrated a high performance protocol for digestion of plastic shirt. In all the sample matrices red fibers were found. to confirm this
polymers in presence of 10% KOH incubated for 48-72 h at 40 ◦ C study, the red fibers were further subjected to FTIR analysis and iden
(Karami et al., 2017). While performing alkali digestion; researchers tified as non-aged cotton (Scopetani et al., 2020b). Thus wearing inap
have also used 10 M NaOH. However, NaOH also results in the degra propriate clothing can cause overestimation of microplastics.
dation of plastic polymers like polyethylene terephthalate, polyvinyl
chloride, polycarbonate and cellulose acetate along with the organic 3. Analytical techniques for identification and chemical
matter present in the sample limiting its application. Thus, KOH is rec composition detection of microplastics
ommended for microplastics sample analysis and processing as it was
very efficient in digesting mussels, crab and whole fish without affecting Identification and detection of microplastics in the succeeding step
the microplastic characteristics (Dehaut et al., 2016). after sampling and a complex procedure. This step confirms that the
separated particle is a microplastic or a false microplastic. There are
2.2.4. Digestion by other chemicals various techniques for identification and chemical composition detec
In chemical digestion protocols effect of other reagents like hydrogen tion some are SEM-EDS, FTIR, NIR, Raman and NMR Spectroscopy.
peroxide (H2O2) has also been tested. H2O2 is an efficient and well SEM-EDS is a powerful microscope that provides information about
known oxidizer used for the removal of organic material. A concentra microplastic surface and additives present on it. FTIR and Raman
tion of 30% H2O2 when added to sample it digests organic matter with spectroscopy are possibly the best technique for chemical character
minimum effect on the plastic polymer within 7 days. H2O2 slightly ization. This technique is accurate, does not damages the sample and
modifies the polymer texture by making it smaller and thinner during spectra is produced, on interaction of the molecule with light. FTIR
the course of digestion (Nuelle et al., 2014; Liebezeit and Dubaish, analysis is feasible for particles upto 20 μm, while Raman is applicable
2012). H2O2 mediated digestion is a slow and concentration dependent upto 1 μm particles. Recently NIR and NMR spectroscopy has also been
process. On increasing the concentration of H2O2 to 35% the time used for microplastics identification. In NIR pre-treatment is not
required for the complete digestion of all kinds of biogenic material was required and can detect upto 1 mm size in an environmental sample.
found to be 7 days with simultaneous effect on the nature of the NMR analysis provides quantity of microplastics present in the sample.
microplastics contents (Cole et al., 2014). Attempts have been made to
reduce the influence of H2O2 on the characteristic property of sample 3.1. SEM-EDS
microplastic content by reducing the concentration and incubation time.
In this regard Frias et al. (2018) recommend 10% H2O2 concentration Scanning electron microscopy (SEM) employs high intensity beam of
with an exposure time of 18 h for complete digestion of organic matter electrons to irradiate the sample for imaging, the signals produced from
with minimum effect on the microplastics residues. the interaction of sample and electron beam emit secondary electron
which is used to generate information about the morphology and
2.3. Biological/enzymatic digestion topography of the sample. This electron sample interaction also pro
duces characteristic x-ray photons (which are element specific) when
Enzymes have been used in many studies to degrade or hydrolyse the electrons move to lower energy states after collision with the inci
biological tissues, as they do not distort or degrade the plastic polymers, dent beam. An EDS(Energy Dispersive Spectroscopy) detector differen
unlike chemical digestion, however enzymatic digestion is also a time tiates these characteristic x-rays of different elements in the sample
taking procedure and every enzyme works on its optimal pH and tem (Schwaferts et al., 2019). Pan et al., revealed in his studies that during
perature condition which has to be monitored and maintained through EDS elemental analysis of microplastics strong nitrogen peaks were
the experiment (Stock et al., 2019; Lusher et al., 2017; Miller et al., found on the surface of polystyrene, polypropylene and polyethylene
2017). Enzymes reported being used in enzymatic digestion process which could be a proxy for biomass. The presence of intense nitrogen in
cellulase, lipase, chitinase, protease, proteinase-K. In one of the studies microplastics samples signifies bioaccumulation which revealed a strong
proteinase K has been added to the sample in order to separate micro interaction between biota and microplastics (Pan et al., 2019).
plastic from the biogenic tissues. The sample was incubated with the SEM-EDS helps in fast screening of non-plastic pellets vs plastics
enzyme at 50 ◦ C for 2 h in presence of sodium perchlorate (NaClO4) with pellets and can also detect small particles which are missed in visual
a digestion efficiency of >97% (Cole et al., 2014). Karlsson et al. and co- detection. The technique used backscattered electron images and
worker tested the digestive ability of proteinase-k enzyme in presence of elemental spectra to check for strong carbon signals and other elements
CaCl2 followed by further treatment using H2O2 to remove the organic present on pellets. Plastic pellets showed strong carbon peak accompa
matter. The recovery rate was found to be 97% but a layer of calcium nied by some weak elemental peak, while in non-plastic pellets there
deposition was found on the plastic surface (Karlsson et al., 2017). A was the absence of a strong carbon peak (Blair et al., 2019). Cooper et al.
basic enzymatic purification protocol (BEPP), was designed, which uses and co-workers revealed that SEM provides high resolution topography
a series of treatment steps like detergent treatment (sodium dodecyl images of microplastics, where they confirmed in their studies that
sulfate (SDS)) followed by three enzymatic treatments (using a mixture plastic particles are embrittled by chemical and physical weathering.
of three enzymes namely protease, cellulose and chitinase) and use of Because of weathering there are fractures, grooves, pits, horizontal
H2O2. This protocol was found to be very efficient leading to reduction notches and vermiculate mixtures on the surface of plastic particles, and
of the organic matter up to 98% and a recovery rate of 83%, the sepa making it prone to further degrade in smaller particles (Cooper and
rated particles can be further analyzed by FTIR technique (Löder et al., Corcoran, 2010).
5
Table 3
Summary of different digestion methods for removal of organic residues from microplastics surface.
Digestion treatment Polymer degradation Organic matter Recovery rate Identification Reference
degradation method
Acid HNO3 heated at 60 ◦ C for 1 h Fibers were not retrieved – 94–98% – (Claessens
et al., 2013)
HNO3 (55%) RT 1 month Whitening of polyvinyl chloride, – – Optical (Naidoo et al.,
degradation of polyamide 2017)
100% HNO3 80 ◦ C for 30 min Some fraction of polymer Oil residue – (Desforges
et al., 2015)
HNO3 (35%), 60 ◦ C 1 h Fusion of polyethylene 100% – (Catarino
terephthalate and High density et al., 2017)
polyethylene; destruction of
Polyamide
1:1 v/v of HCl and HNO3, 80 ◦ C for 30 min – Smaller – (Desforges
fragments et al., 2015)
HNO3 (65%) + HClO4 (65%) 4:1 overnight, Polyamide degradation, yellowing – – (Dehaut et al.,
boiled 10 min, dilution 80 ◦ C distilled water 2016)
37%HCl at 25 ◦ C, 96 h Polyethylene Terephthalate and >97% – Optical (Karami et al.,
polyvinyl chloride melted, formed 2017)
clumps
Alkali 10%KOH 24 h 60 ◦ C Cellulose acetate Raman (Dehaut et al.,
2016)
10% KOH at 40 ◦ C for 48–72 h no >95% reduced – Optical (Karami et al.,
examination 2017)
KOH (1 M), RT 2 days Degradation of Low density Most organic – (Kühn et al.,
polyethylene, Cellulose acetate, matter gets 2017)
Cradonyl and Polyamide dissolved
10 M NaOH 60 ◦ C, 24 h Yellowing of polyvinyl chloride, – – Raman (Dehaut et al.,
polyethylene terephthalate 2016)
degraded
10 M NaOH 60 ◦ C Discoloration of nylon, polyvinyl 91% – Optical (Cole et al.,
chloride, polyethylene and 2014)
damaged
NaOH (20 g L− 1) + NaClO (14%) at 60 ◦ C, 24 – Some tissues are – Optical (Railo et al.,
h left microscope, 2018)
FTIR
1 M NaOH +SDS 0.5%, 50 ◦ C for 48 h, Polyethylene Terephthalate Chitin partially 84 ± 15% Stereo (Budimir et al.,
filtration, showed slight changes digested microscope 2018)
If calciferous material remain at filter, 2 M HCl
is added followed by 30% H2O2
Oxidative 30% H2O2 for 7 days Transparent, thinner or smaller 50% – Optical (Nuelle et al.,
2014)
H2O2 (35%), RT, 40 ◦ C 96 h Decrease in Raman peaks of – – Raman (Karami et al.,
Polyvinyl Chloride and Polyamide 2017)
H2O2 (30%), 60 ◦ C for 1 h, 100 ◦ C for 7 h – – – Optical (Erni-Cassola
et al., 2017)
H2O2 (6%) 70 C for 24 h
◦
– – 78% Raman (Sujathan
(Polyethylene) et al., 2017)
Enzymatic Proteinase –K At 50 ◦ C for 2 h with NaClO4 No >97% – Optical (Cole et al.,
and ultrasonicated examination 2014)
Pepsin (0.5%) and HCL (0.063 M), 35 ◦ C 2 h No Partial – Raman (Dehaut et al.,
2016)
Proteinase –K With CaCl2 h, shaken 20 min, Formation of Calcium layer No 97% Raman (Karlsson
incubated 60 ◦ C 2 h, 30 ml H2O2 (30%) et al., 2017)
overnight
Tripsin incubate at 38◦ -42 ◦ C for 30 min No 88% – FTIR (Courtene-
Jones et al.,
2017)
Collagenase incubate at 38◦ -42 ◦ C for 30 min No 76% – FTIR (Courtene-
Jones et al.,
2017)
Papain incubate at 38◦ -42 ◦ C for 30 min No 72% – FTIR (Courtene-
Jones et al.,
2017)
SDS 50 ◦ C incubate for 24 h – 98% 83% FTIR (Löder et al.,
Protease incubate 50 ◦ C for 24 h 2017)
Cellulose TXL incubate for 50 ◦ C for 4 days,
35% H2O2 incubate for 50 ◦ C for 24 h,
Chitinase incubate for 37 ◦ C for 5 days, H2O2
for 24 h at 37 ◦ C
SDS,24 h, 70 ◦ C + mixture of enzymes (1:1 No – – Optical, FTIR (Railo et al.,
Biozym F: Biozym SE) 48 h, 37.5 ◦ C 2018)
6
Environmental scanning electron microscopy (ESEM) is a type of microplastics study in wild Mytilus edulis by ATR-FTIR, revealed the
SEM that is used for environmental analysis of samples, wet samples are majority of ingested microplastics were fibrous in nature. The spectra
kept at low pressure nitrogen atmosphere, which enables imaging of obtained from particles were matched with reference library collection
samples otherwise in high vacuum the sample would degrade (Schwa to assist the analysis and characterization of percentage transmittance
ferts et al., 2019). In ESEM-EDX sample is not coated with metal or spectra (Courtene-Jones et al., 2017). In another study ATR-FTIR was
carbon, which makes the subsample artifact free, for further FTIR and used with a combination of single-element MCT (Mercury Cadmium
Raman analysis (Wagner et al., 2017). Wagner et al., and co-workers Telluride) detector to identify different types of microplastics from the
used this technique as a screening tool for the identification of only debris of the beach. Spectra of the samples were recorded at spectral
microplastic residue neglecting the presence of non-microplastics com resolution of 8 cm− 1, 128 scans were taken for single spectra in 4000-
ponents and rule out mineral species from fish gut. It was found that 650 cm− 1 spectral range (Andrades et al., 2018). Jung et al. and co-
microplastics surface adhered thin biofilm, mineral crust, fish scales, workers created criteria to validate the ATR-FTIR spectra results. They
crustaceans and radiolarians, which makes it resemble like a marine created their own database to identify the absorption band of each
organism, but due to strong C peak, it was confirmed to be microplastics. microplastics, which was compared with the absorption band of
Minerals particles like shell fragments, cellulose, chitin, silicate (clay different types of microplastics present in the database. Four absorption
and sand) protein and carbohydrates, exhibit brighter Scattered Electron bands were mandatory to be matched with the given library, to confirm
(BSE) due to rich inorganic contents like Ca and Si (Wagner et al., 2017). the type of microplastic. Thus ATR-FTIR was able to identify various
types of microplastics ingested in the marine organisms, including dif
3.2. FTIR ferentiation between low density polyethylene and high density poly
ethylene which is challenging (Jung et al., 2018).
Fourier-transform infrared (FTIR) spectroscopy is the most widely In addition, the ATR mode produces stable spectra from irregular
used technique for the detection of microplastics due to several reasons microplastic surfaces. However ATR has some disadvantages like it can
like directness, reliability, non-destructive approach (Ojeda et al., 2009) damage the fragile or highly weathered microplastics due to high
and it also produces individual band patterns by specific infrared spectra pressure produced by the probe and tiny microplastic particles could
for different plastics types (Hidalgo-Ruz et al., 2012). When a sample is stick to the probe tip due to electrostatic force (Shim et al., 2017).
irradiated by infrared light (wave number range 400–4000 cm− 1 for Focal plane array (FPA)-FTIR offers analysis and identification of
Mid-IR) depending upon the molecular structure of the microplastics, microplastic particles <20 μm by scanning the isolated microplastics
radiation is absorbed and measured in reflection or transmission mode residues on a filter paper with a high degree of lateral resolution without
(Käppler et al., 2016). On absorption of IR, the chemical bonds of sample pre-sorting the filter area (Löder and Gerdts, 2015). FPA uses grid of
change their dipole moment making polar functional group (e.g. detectors to record several spectra in a single measurement or thousands
carbonyl group) detectable (Büchtemann, 1993). FTIR can not only of spectra in a minute for microplastic analysis. FPA-based reflectance
accurately identify the polymer types of microplastics, but also provide micro FTIR images the entire membrane filter area containing micro
further information about physiochemical weathering of microplastics plastics residues, where each pixel corresponding to microplastics pro
by analyzing their oxidation intensity (Cooper and Corcoran, 2010). duces an independent infrared spectrum. Thus, FPA-FTIR filter images
FTIR has three optimizing technologies: Attenuated total reflection provide better information regarding small size microplastics with high
(ATR), Focal –plane array (FPA) and micro-FTIR. resolution at a faster rate, which leads to robust results with minimal
FTIR has a limitation in that it can only detect microplastics upto 20 analytical bias (Tagg et al., 2015). FPA-micro FTIR images the whole
μm, this can be overcome by using micro-FTIR. Micro-FTIR has the filter to a spatial resolution of 20 μm. False-color images were produced
ability to characterize the sample below 10 μm (Löder and Gerdts, in two polymer specific regions: firstly 1480 and 1430 cm− 1 and sec
2015). Harrison et al., tested the effectiveness of micro-FTIR and ondly 1790 and 1700 cm− 1. Images derived from this color scheme are
reflectance micro-FTIR techniques for the detection of microplastics in proportional to area above and below the baseline. Potential micro
marine sediments and successfully demonstrated the potential of such plastics were marked on basis of this information and the spectra were
techniques through molecular mapping based on their spectral charac identified via library search. Dimensions were also recorded for every
teristics (Harrison et al., 2012). particle size and colo (Mintenig et al., 2017). Primpke et al. and co-
For identification of mixture of natural fibers and semi-synthetic fi workers improved FPA-FTIR by using an automated software based
bers a characteristic band method has been developed. By transmittance data analysis tool. All spectra obtained from the sample are compared
mode in micro-FTIR the bands are checked. If the band value falls in against a database of different natural and synthetic polymers present in
1105 cm− 1 which is the characteristic band for semi-synthetic fibers, it the software library which is obtained by benchmark tests with a focus
confirms the presence of semi-synthetic. Usually, the samples collected on quality and accuracy. This helps to gain unbiased information of each
from the environment have a different composition, they are weathered and every microplastic detected and tells its particle size, polymer type
and biofouled, which makes it difficult for the matching algorithm to and particle number (Primpke et al., 2017). FTIR microscope equipped
match with the spectral library which is commercially available, so there with FPA was used to identify the ingested microplastics in the Buno
is a need to enhance the polymer spectra library (Cai et al., 2019). dosoma cangicum a sea anemone. It provided 2D imaging maps at a
ATR-FTIR is another reliable and fast detection tool for polymer spatial resolution of 5.5 μm, allowing numerous independent spectra on
characterization isolated from water and biological samples (Käppler microplastics. Microplastics were identified by matching at least four
et al., 2018). ATR-FTIR are best for the analysis of large microplastic characteristics absorption band on the basis of Jung et al. criteria (Jung
articles, sample preparation is not required for thick or opaque samples. et al., 2018) after identification it was classified on the basis of their
ATR–FTIR measurement is a form of surface contact analysis. In ATR- tendency to sink or float based on the density. The intensity of charac
FTIR, plastic sample needs to be in contact with the crystal (Crawford teristic bands was mapped in false color, to see how each band is
and Quinn, 2017; Shim et al., 2017). Kyoung et al., analyzed sea-surface representative of the spectra of a single map. Various microplastics were
microlayer and beach sand samples for presence of microplastics identified by this approach low density polyethylene, high density
employing ATR-FTIR technique. They identified small microplastics of polyethylene, polyethylene terephthalate, polyvinyl chloride, poly
size <50 μm and also concluded that with decrease in the size of styrene, nitrile, polyamide, polyurethane, cellulose fibers (Morais et al.,
microplastic the efficiency of microplastics detection increases due to 2020).
abundance in the concentration of microplastics in the sample. The FTIR
also confirmed the polymer type and provided additional information
like polymer origin and behavio (Kyoung et al., 2015). Ingested,
7
3.3. Near Infrared Spectroscopy (NIR) identified by matching it with the available library (rapid), this
approach improved the point mapping (Schymanski et al., 2018).
NIR region light can also be used to differentiate plastics. NIR In Raman spectroscopy auto-fluorescence background from organic
spectroscopy has an advantage over FTIR, as it penetrates deeper into matter present at on microplastics is a great hindrance for identification
the plastic material. In this technique, sample preparation is not of the microplastics, as it overshadows the raman peaks. To overcome
required and bulk samples can easily be examined. When NIR light is this limit Ghosal et al. used an automated algorithm to remove the
irradiated on the plastic, the plastic molecules absorb electromagnetic fluorescence background from raman microspectroscopy and reveal the
radiation to produce molecular overtone and combination vibrations. underlying polymer spectrum. On subtracting the background fluores
Consequently, plastic materials can be identified by differences in the cence, polymer peaks are clearly visible, which can be then matched
characteristic C–H, N–H and C–O bands typically observed with these with library matching software to obtain the information regarding size,
types of materials (Crawford and Quinn, 2016). chemical composition and morphology of the microplastic residues
Few studies have been conducted on microplastics identification by (Ghosal et al., 2018).
NIR spectroscopy. Corradini et al. with help of vis-NIR spectroscopy Early mapping of a single particle was difficult or direct analysis of
predicted the concentration of microplastics in the soil samples. Vis-NIR natural samples was very difficult. Sobhani et al. with help of a confocal
spectra from the samples were recorded by a spectroradiometer having raman microscope, identified and visualized microplastics from a soil/
spectral resolution of 3 nm for 350-1000 nm region and 10 nm for sand background. They demonstrated that the procedure does not
10,000–2500 region. Soil samples without any pre-treatment were require any sample preparation, or involved addition of any dye, a non-
allowed for direct measurement by spectroradiometer through a spot destructive approach and negligible interference from water organic
size of 10 mm. Five readings were taken per sample in the quincunx matter to fluorescent background. They identified five microplastics
pattern. Virgin microplastics and bare soil depicted different reflectance, types (polystyrene, polyethylene terephthalate, polyethylene and poly
while on mixing microplastics with soil, the reflectance of soil shrinked vinyl chloride, polypropylene). After mapping, each particle gave a
as the quantity of microplastic was added as a pollutant. Thus as the distinct raman spectrum which can be picked at each pixel, and can be
concentration of microplastics was increased in the soil, soil reflected verified by comparing with their fingerprint spectra. By merging, the
less light at near and shortwave infrared region (Corradini et al., 2019). mapping images of each particle from their characteristic peaks, a
A high throughput NIRS spectroscopy combined with chemometrics complete picture of microplastics distribution is obtained (Sobhani
was used to examine the presence the microplastics in soil samples and et al., 2019).
also determine the size, number and age of plastic. During each run 64
spectra were produced, these spectra were evaluated by The Unscram 3.5. Nuclear Magnetic Resonance (NMR)
bler software. NIR was able to detect polyethylene, polypropylene,
polystyrene, polyterephthalate and polyvinyl chloride in soil samples at Application of 1HNMR spectroscopy (qNMR) can be applied for
1 mass%. Support vector machine (SVM) model was able to recognize quantitative and qualitative analysis of microplastics. Till date very few
microplastics in artificial soil samples and real samples (Paul et al., studies have been conducted which have applied qNMR for quantifica
2019). tion of microplastics. Quantitative determination by qNMR is based on
To identify different types of microplastics found in marine, Pak the fact that signal intensities or the integral value of the signal are
homova et al. demonstrated a Micro-NIR spectrophotometer. A spectral proportional to the proton numbers that give rise to a particular reso
library was created which contains the most common microplastics nance. qNMR can achieve precise quantification and high quantitative
found in marine litter. Spectra produced from the microplastics were accuracy of >98%. In NMR spectroscopy dissolution of the microplastics
processed and analyzed by MicroNIR Pro software. Spectral match value in the suitable deuterated solvent is required.
was further used to identify the different types of polymer. Identification The very first application of 1H NMR spectroscopy was done by Peez
accuracy was further identified by ATR-FTIR. MicroNIR was able to et al., they identified and quantified polyethylene, polyterephthalate
identify microplastics of size >1 mm in the environmental samples and and polystyrene particles in model samples. For analysis polyethylene
was able to identify 96% of the particles from the real samples. Thus, was deuterated in toluene and deuteron, polyterephthalate was
MicroNIR is an excellent tool that can be used on site for microplastic deuterated in chloroform and trifluoroacetic acid, and polystyrene was
identification (Pakhomova et al., 2020). deuterated in chloroform. Spectra obtained was loaded in NMR program
MestReNova. For method validation, different parameters have been
3.4. Raman spectroscopy determined such as linearity, range, limit of quantification, stability,
precision and accuracy. The calibration curve method was used for the
For microplastic identification Raman spectroscopy is also used, it is quantitative determination. By the calibration curve method, micro
a vibrational spectroscopy technique that delivers information in the plastics can be determined by high precision in model samples (Peez
form of vibrational spectra, on basis of inelastic scattering of light. The et al., 2019b). Peez et al. (2019a) in another study used qNMR with
spectrum obtained is like a fingerprint of chemical structure, which al integration method and calibration curve method (INT-qNMR). After the
lows identification of particles present in sample (Araujo et al., 2018). It chemical digestion method, there are overlays of matrix signal which
shows better spatial resolution for minute samples, highly sensitive to can be reduced by applying peak fitting method (PF-qNMR). Using this
non-polar functional groups, spectral bands are narrowed down and low mathematical technique signal overlaps can be deconvoluted allowing
interference due to water are few benefits of Raman spectroscopy over for area integration of extracted signals. It is an advantage over FTIR and
FTIR techniques (Elert et al., 2017; Ivleva et al., 2017; Käppler et al., Raman spectroscopy, as FTIR is sensitive to matrix effect and Raman
2016). Raman microspectroscopy has the ability to detect microplastics spectra are influenced by fluorescence. The amount of PET fibers in
as small as 1 μm and deliver its chemical and structural characteristics, environmental sample were quantified by INT-qNMR combined with
which is not possible with other spectroscopic techniques (Crawford and calibration curve method (Peez et al., 2019a).
Quinn, 2017). In a recent study Peez et al., tried quantifying polyvinyl chloride
Schymanski et al. with help of Raman microspectroscopy of bottled powder, acrylonitrile butadiene styrene granules and polyamide fibers.
water revealed that packaging materials release microplastics in the Here Peak Fitting method was used as an alternative to the integration
water stored. A single particle explorer (rapID) software was used for method to validate microplastics signals even without baseline sepa
automatic detection of particles larger than 5 μm. the analysis resulted in rated. Thus qNMR can detect microplastics of any shape, size or polymer
the creation of a spectral map representing spectra for each microplastic type (Peez and Imhof, 2020). Table 4 is a compilation of different
analyzed in the sample. Spectra obtained from each particle was spectroscopic techniques used for microplastic characterization.
8
Table 4 et al., 2017).

Techniques for chemical characterization of microplastics by FTIR, NIR, Raman
and NMR. 5. Conclusion
Technique Finding Reference
ATR-FTIR Ideal for thick or strong- IR- (Fu et al., 2020; Käppler et al., This review summarizes and evaluates the different sampling and
absorbent samples, Thin and 2018; Shim et al., 2017; characterization methods for microplastics. Sampling, processing and
thick fibers, Irregularly shaped Kyoung et al., 2015; Jung et al., identification of microplastics are very difficult due to their small size.
microplastics, confirm polymer 2018; Andrades et al., 2018) Methods like visual sorting or optical microscopy are prone to error
type,
FPA-FTIR Detection to the size of 20 μm, (Tagg et al., 2015; Primpke
because of microplastics resemblance to other organic matter. For
automated mapping with et al., 2017; Löder et al., 2015; digestion of biogenic material KOH is the most suitable chemical agent
software gives information about Morais et al., 2020) as it degrades the tissue of fishes and crabs without interfering with the
particle number, size, polymer polymer's property or morphology of microplastics. Density separation
type, in short duration of time,
is the most common technique using ZnCl2 as the ideal separator salt
Micro-FTIR Provide chemical mapping, detect (Tagg et al., 2015; Harrison
microplastics as small as 10 μm, et al., 2012; Cai et al., 2019; which helps in the separation of high density polymers easily and to
with characteristic bands natural Käppler et al., 2016; Löder maximum level. SEM/EDS helps to identify the plastic polymer due to its
and synthetic fibers can be et al., 2015; Mintenig et al., strong carbon intensity. For identification and characterization of
distinguished, filter paper is 2017) microplastics FTIR or Raman spectroscopy is also recommended tech
scanned with a speed of 20 min-
nique. FTIR and Raman both are complementary techniques to each
19 s/mm2
NIR It penetrate deeper in the plastic, (Paul et al., 2019; Pakhomova other and generates chemical mapping information, FTIR can detect a
no pre-treatment is required, et al., 2020; Corradini et al., particle upto a size of 10 μm, but Raman Microscopy can go down to a
detection limit of the size is >1 2019) size of 1 μm. automated raman mapping enables fast detection of plastic
mm, concentration of
particles with minimal operating time. Apart from FTIR and Raman, NIR
microplastics in soil samples can
be predicted spectroscopy can also be used, it can detect up to the size limit of >1
Micro Detection to the size of 1 μm, (Elert et al., 2017; Ghosal et al., mm. For quantifying concentration of microplastics qNMR can be used,
Raman automated scanning of filter 2018; Schymanski et al., 2018; it is size-independent, fast as well as simple method. Still there is lack of
paper with different software, Sobhani et al., 2019; Käppler techniques for proper identification and characterization of micro
each particle location gave et al., 2016)
plastics. Still there is tremendous scope for development of advanced
Raman spectra, spectra was
identified by automated matching standardized methodologies and analysis techniques in the field of
library, an automated logarithm microplastics research.
was used to remove fluorescence Future research needed:
background, mapping of mixture
of 5 microplastics together
1
H NMR Size –independent and fast for (Peez et al., 2019b, 2019a; Peez
▪ Standard method for sampling and analysis of microplastic
microplastics analysis. and Imhof, 2020) using quality assured methods.
Quantification of number of ▪ Real time analysis of microplastics in environment.
microplastics in environmental ▪ Toxicological testing to get more data associated with human
samples, organic matrics signal
health risk by ingestion.
are reduced by peak fitting. Thus
qualitative and quantitative ▪ Enhanced and standard matching libraries should be made for
determination of microplastics in identification of microplastics from environmental samples.
samples. ▪ Reliable methods are needed to track down the original source
of microplastics in fresh water.
4. Quality control
Declaration of competing interest
Contamination is a critical issue in microplastics research. During
sample collection and processing of sample, there are huge chances of The authors declare that they have no known competing financial
contamination by atmospheric fallout, equipment, contaminated glass interests or personal relationships that could have appeared to influence
ware and cloths. Measures should be taken to reduce the error: the work reported in this paper.
contamination free glass and metal equipment should be used, to ac
quire the degree of clean glassware. They can be rinsed with Milli-Q Acknowledgment
water followed with ethanol always before and after every use. Usage
of plastic equipment should be avoided. Polyester clothes should not be We express our sincere thanks to Director, National Institute of
worn during sampling or processing, white cotton labs should be used. Technology, Raipur and MHRD, GOI for providing scholarship and
To protect samples from air contamination, sample should always be giving the opportunity to conduct research.
covered with aluminum foil or kept in close/capped containers, clean
the work place with 70% ethanol, use open petri dishes as control at
every step of analysis in order to check the aerial source of any plastic Ethical approval
contamination in the laboratory condition. Preferably samples should be
Handled in laminar air flow (Wesch et al., 2017; Cole et al., 2014; Sun None.
et al., 2019).
Loss of sample during extraction of sample is a major problem in Funding details
microplastic detection. Microplastics recovery test is recommended after
the extraction process. In this test, a definite quantity of microplastics No external funding for this work.
with known color and size are added to Milli-Q water and subjective to
similar treatment procedure of extraction (this is treated as control). A
Data availability
deviation in the number of microplastic count of the sample in com
parison to control is utilized for calculating the recovery rate (Löder
None.
9
CRediT authorship contribution statement Crawford, C., Quinn, B., 2016. Microplastic Pollutants, Microplastic Pollutants.
Crawford, C., Quinn, B., 2017. 8-Microplastic collection techniques, microplastic
pollutants. In: Microplastic Pollutants. Elsevier, pp. 179–202. https://doi.org/
AT conceived and drafted the manuscript. LU proof read the 10.1016/B978-0-12-809406-8.00008-6.
manuscript. Crichton, E.M., Noël, M., Gies, E.A., Ross, P.S., 2017. A novel, density-independent and
FTIR-compatible approach for the rapid extraction of microplastics from aquatic
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Robbens, J., 2014. Quality assessment of the blue mussel (Mytilus edulis):
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https://doi.org/10.1016/j.marpolbul.2014.06.006.
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Marine Pollution Bulletin 170 (2021) 112604

Contents lists available at ScienceDirect

Marine Pollution Bulletin

Microplastics: An overview on separation, identification and

2.2.3. Alkali digestion 2017). Table 3 is a compilation of different digestion methods.

Table 4 et al., 2017).

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