Fu 2020

Science of the Total Environment 721 (2020) 137561
Contents lists available at ScienceDirect
Science of the Total Environment
journal homepage: www.elsevier.com/locate/scitotenv
Separation, characterization and identification of microplastics and

nanoplastics in the environment
Wanyi Fu a,b, Jiacheng Min a,c, Weiyu Jiang a,c, Yang Li d, Wen Zhang a,c,⁎
a
John A. Reif, Jr. Department of Civil and Environmental Engineering, New Jersey Institute of Technology, Newark, NJ 07102, USA
b
Shenzhen Environmental Science and New Energy Technology Engineering Laboratory, Tsinghua-Berkeley Shenzhen Institute, Tsinghua University, Shenzhen 518055, People's Republic of China
c
Department of Municipal and Environmental Engineering, School of Civil Engineering, Beijing Jiaotong University, Beijing 100044, People's Republic of China
d
State Key Laboratory of Water Environment Simulation, School of Environment, Beijing Normal University, Beijing 100875, People's Republic of China
H I G H L I G H T S G R A P H I C A L A B S T R A C T
• Separation, characterization and identifi-

cation approaches for microplastics are
summarized.
• Principles, applications, advantages and
limitations of each approach are discussed.
• AFM and hybrid AFM techniques are pro-
posed as emerging characterization plat-
forms.
• Standard experimental procedures and re-
liable characterization methods are on
demand.
a r t i c l e i n f o a b s t r a c t
Article history: Microplastics (MPs) have globally been detected in aquatic and marine environments, which has raised scientific inter-
Received 24 December 2019 ests and public health concerns during the past decade. MPs are those polymeric particles with at least one dimension
Received in revised form 16 February 2020 b5 mm. MPs possess complex physicochemical properties that vary their mobility, bioavailability and toxicity toward
Accepted 24 February 2020
organisms and interactions with their surrounding pollutants. Similar to nanomaterials and nanoparticles, accurate
Available online 2 March 2020
and reliable detection and measurement of MPs or nanoplastics and their characteristics are important to warrant a
Editor: Shuzhen Zhang comprehensive understanding of their environmental and ecological impacts. This review elaborates the principles
and applications of diverse analytical instruments or techniques for separation, characterization and quantification of
Keywords: MPs in the environment. The strength and weakness of different instrumental methods in separation, morphological,
Microplastics physical classification, chemical characterization and quantification for MPs are critically compared and analyzed.
Nanoplastics There is a demand for standardized experimental procedures and characterization analysis due to the complex trans-
Detection formation, cross-contamination and heterogeneous properties of MPs in size and chemical compositions. Moreover,
Characterization this review highlights emerging and promising characterization techniques that may have been overlooked by research
Plastic pollution
communities to study MPs. The future research efforts may need to develop and implement new analytical tools and
combinations of hyphenated technologies to complement respective limitations of detection and yield reliable charac-
terization information for MPs. The goal of this critical review is to facilitate the research of plastic particles and pollut-
ants in the environment and understanding of their environmental and human health effects.
© 2020 Elsevier B.V. All rights reserved.
⁎ Corresponding author at: John A. Reif, Jr. Department of Civil and Environmental Engineering, New Jersey Institute of Technology, Newark, NJ 07102, USA.
E-mail address: wen.zhang@njit.edu (W. Zhang).
https://doi.org/10.1016/j.scitotenv.2020.137561
0048-9697/© 2020 Elsevier B.V. All rights reserved.
2 W. Fu et al. / Science of the Total Environment 721 (2020) 137561
1. Introduction many other important techniques and instruments such as FCM, DLS,
HSI, and AFM. Thus, holistic reviews of available techniques for separa-
Microplastics (MPs), a group of plastic particles of b5 mm, have in- tion, characterization and detection or identification of microplastics are
creasingly been detected in various aquatic and marine environments, still limited (Hidalgo-Ruz et al., 2012). More importantly, some com-
which has raised scientific interests and public health concerns mon techniques that have widely been used in inorganic material or
(Arthur et al., 2009). Microplastics may derive from manufactured raw nanomaterial characterization have not been well adopted in the re-
plastics, including microbeads in facial cleanser, scrubbers and virgin search and characterization for microplastics.
plastic pellets (Andrady, 2011; Browne et al., 2007; Thompson et al., The main objective of this critical review is to delineate the princi-
2004). Several studies reported that sewage treatment plants are also ples and applications of the instrumental methods that have been re-
the significant sources of MPs and the sludge or biosolid applications ported for separation, detection, characterization and identification of
in agricultural systems present a major contribution to the environmen- microplastics in aqueous and solid samples. Different techniques were
tal MPs (Edo et al., 2020; Gatidou et al., 2019). Due to the broad applica- introduced to demonstrate their working principles, applications, limi-
tions, massive amounts of plastic-contained products end up in solid tations, and advantages, followed by a discussion of perspectives that
waste and enter waterways (Arthur et al., 2009). This poses potential shed new light on future research and directions. Important take-
risks to human health and ecological systems such as aquatic organisms home messages were given as of (1) how to accurately identify synthet-
or animals if ingested directly or indirectly through food chain (Browne ically engineered microplastics from interferences from naturally occur-
et al., 2007; Masura et al., 2015). ring polymers such as organism-secreted biopolymers; (2) how to
Microplastics may undergo complex transformations (e.g., aging, chemically label and enhance the visualization of microplastics from
fragmentation, and aggregation) and interactions with environmental complex matrices such as soil and surface water; (3) how to perform di-
matrix or species such as bacteria and pollutants (Harrison et al., rect identification and quantification of microplastics (without separa-
2011). The physicochemical properties of microplastics (e.g., shape, tion/extraction/concentration). This review is aimed to provide a
size, concentrations, surface charge, and hydrophobicity) affect the guideline for researchers in selecting proper methodologies and tech-
transformation, interaction, fate and bioavailability to aquatic organ- niques for microplastics research in different sample matrices. Particu-
isms (Wright et al., 2013). For instance, different sizes and shapes larly, we highlighted the great potential of emerging hyphenated
(spheres and plates) of microplastics provide different surface areas techniques such as hyperspectral imaging, AFM/Raman and AFM/IR in
for the deposition of water contaminants and may vary the biological microplastics research.
uptake of water contaminants (Bakir et al., 2014). Therefore, it is imper-
ative to investigate how microplastic properties relate to their environ- 2. Separation of microplastics
mental fate and biological impacts, which ultimately delivers new
insight into prevention and mitigation of the environmental risks of Separation of microplastics is usually achieved by sieves with mesh
microplastics. sizes ranging from 0.038 to 4.75 mm that are used singly or in a series.
Accurate acquisition of physical and chemical properties (i.e., shape, Moreover, filters with small mesh sizes (e.g., 0.02 μm–5 μm) are also
size, polymer compositions, and functional groups) is essential for un- used to separate small microplastics or nanoplastics (Hollman et al.,
derstanding the aquatic behavior and bioavailability of microplastics. 2013; Li et al., 2018a; Masura et al., 2015). For plastic particles b1 μm,
Research on the detection of plastic particles in complex environmental chromatographic techniques, active and passive separation, are typi-
samples provides at least three aims: (1) separation, extraction or con- cally used. Active separations, such as field flow fractionation (FFF)
centration; (2) visually identify and quantify microplastics; (3) assess technique (Mintenig et al., 2016), apply external fields into microfluidic
the dynamic physicochemical properties of microplastics. There are dif- environments for separation of dispersed particles; while passive sepa-
ferent characterization tools that could largely fulfil these research aims, rations, such as hydrodynamic chromatography (HDC) (Blom et al.,
such as optical, spectroscopic and chromatographic techniques that can 2003), utilize hydrodynamic and surface forces to separate particles in
reveal, identify and quantify microplastics (Mintenig et al., 2018; Shim liquid. FFF and HDC as representative active and passive separation
et al., 2017). The detection and characterization of microplastics typi- techniques and their applications in microplastic separation from liquid
cally involve three steps: (1) extraction from the matrix (Besley et al., samples are elaborated below.
2017); (2) separation, quantification and sizing; and (3) characteriza-
tion and/or identification of microplastics (Correia and Loeschner, 2.1. Field flow fractionation (FFF)
2018). The methodologies for sampling and extraction of microplastics
from beach sand (Besley et al., 2017), marine organisms (Claessens FFF is a useful separation technique typically for size and molar mass
et al., 2013), tissues (Avio et al., 2015), and sediments (Nuelle et al., fractionation of biopolymers, proteins, polymers, and nanoparticles
2014) have been elaborated in previous literature. Several recent re- (Wahlund, 2013). As shown in Fig. 1, a fluid suspension is pumped
views have examined the methods for sampling, identification and through a long and narrow FFF channel under a force field that is per-
quantification of microplastics in freshwater and marine environments. pendicular to the direction of flow. The specific field causes separation
For example, Fok et al. reviewed the methodologies used for the re- of the particles present in the fluid, depending on their differentiated
search of MPs in China, but particularly focused on methods for collec- mobility under the force field (Contado, 2017). The external field forces
tion and extraction of MPs (Fok et al., 2019). Hermsen et al. critically could be applied through asymmetrical flows via a semi-permeable
reviewed the literature on analytical methods employed to detect MPs membrane (AF4) (Podzimek, 2006), gravitational (Marassi et al.,
in marine biota samples (Hermsen et al., 2018). Stock et al. provided a 2018), centrifugal (sedimentation FFF) (Tadjiki et al., 2017), thermal-
review on the sampling and sample preparation of MPs samples from gradient (Greyling and Pasch, 2017), electrical (Ornthai et al., 2016),
water, sediment and biota of freshwater and marine environments, and magnetic fields (Samanta et al., 2016). Due to the field force exerted
but without sufficient discussions on analytic techniques (Stock et al., on the solute, the solute flow undergoes stratification and forms differ-
2019). Silva et al. discussed the issues associated with the analysis of ent thickness of solute layers as illustrated in Fig. 1. Solute layers are
microplastics in environmental samples, from sampling to identification then displaced by a longitudinal flow. Since the flow streamlines are
and quantification (Silva et al., 2018). For instance, this previous review at the slowest speed near the channel wall or accumulation wall, the
suggested standardized and uniform units should be used (e.g., mass analytes are retarded to different extent depending on their distance
per volume or number per volume) for the abundance of MPs. Silva away from the accumulation wall (Giddings et al., 1976). Different
et al. only discussed several commonly used identification methods from high performance liquid chromatography (HPLC), FFF does not re-
such as visual detection, SEM, FTIR, Raman, and Py-GC–MS, but ignored quire specific solvents as a mobile phase to separate analytes. However,
W. Fu et al. / Science of the Total Environment 721 (2020) 137561 3
Fig. 1. Simplified scheme of an FFF channel operating in different separation field.

The figure is adapted from (Contado, 2017) with permission.
an advanced instrument for generating an asymmetric flow (field) such dioxide (Kim et al., 2013)) efficiently in a continuous flow. Therefore,
as semi-permeable membrane, gravitational, and centrifugal devices is sedimentation FFF is a promising separation technique for microplastics
necessary (Huppertsberg and Knepper, 2018). or nanoplastics from different environmental matrices, which has not
FFF technique has been used in the characterization of microplastics been reported in literature so far probably because plastics particles
(Gigault et al., 2017; Huppertsberg and Knepper, 2018; Mintenig et al., have densities lower than water and thus are usually afloat in water.
2018). AF4 is one of the versatile FFF techniques with commercially The studies by Correia and Loeschner evaluated the separation of certain
available instrumentation. Correia and Loeschner presented a first types of nanoplastics using AF4, which may require adjustments of the
study employing AF4 coupled with multi-angle light scattering to detect separation principles for different types of nanoplastics (Correia and
spiked PS nanoplastics in a food matrix. However, this separation/detec- Loeschner, 2018). The environmental samples may contain more than
tion method may not work for other types of nanoplastics due to the one type of polymers and the purification of nanoplastics is usually re-
chemical-dependence of separation or detection principles (Correia quired to remove organic matters using acidic and enzymatic digestion.
and Loeschner, 2018). Particularly, environmental samples usually con- Besides, Correia and Loeschner spiked polystyrene in fish samples for
tain more than one type of polymers and coexist with contaminants the separation study, indicating that AF4 might be applicable only in
such as natural organic matters that need to be removed by acidic and laboratory studies (e.g., toxicity tests and uptake studies).
enzymatic digestion. Clearly, AF4 is expected to better serve the charac-
terization under well-controlled laboratory conditions. This study by 2.2. Hydrodynamic chromatography (HDC)
Correia and Loeschner also revealed that AF4 was superior especially
when cells/tissues have auto-fluorescence that may interfere the results Hydrodynamic chromatography (HDC) is a solution-phase liquid
from fluorescence microscopy and flow cytometry. By contrast, AF4 di- chromatographic separation method for particle size determination in
rectly separates and identifies the components of the mixture using the range from 10 nm to 1000 nm (Lespes and Gigault, 2011). HDC com-
field forces instead of optical characteristics. Mintenig et al. used AF4 bines the advantages of fluid dynamics and exclusion chromatography
and pyrolysis GC–MS to determine particle sizes and polymer types of to separate diverse nanoparticles (NPs), such as polystyrene (PS) NPs
MPs. Their study aimed to standardize the measurement methods of (Pirok et al., 2017), gold NPs (Gray et al., 2012), silver NPs (Chang
concentrations and sizes of micro- and nanoplastics, which is crucial et al., 2017), and SiO2 NPs (De Lange et al., 2011). As shown in Fig. 2,
for data accuracy and interpretation (Mintenig et al., 2018). Further- HDC separates analytes (e.g., particles or bubbles) based on the size dif-
more, Gigault et al. developed a programmed AF4 method to rapidly ferences (independent on their density differences). After the sample
quantify the microplastics populations in fullerene aggregates and poly- enters the packed column filled with solid beads, a velocity profile is
styrene (PS) latex standard (Gigault et al., 2017). This method reached established among the channels between the adjacent beads. According
an improved accuracy of AF4 when screening microplastic particles of to the mechanism of Brownian motion, for the particles in the range
1–800 nm at a high fractionation resolution in the range of from 10 nm to 1000 nm, their traces are more likely to be disturbed
10–400 nm (Gigault et al., 2017). However, two drawbacks were re- by the media grain, since small particles receive increasing impacting ef-
ported for AF4 with a porous semi-permeable membrane as the accu- fects from collisions with the media grains (Karatzas and Shreve, 1998;
mulation wall. One is the high sample dilution that occurs during Small, 1974). Under the influence of the viscous force such that the fluid
sample migration in the channel to the detector, which limits the velocity is greatest at the center and decreases toward the wall (Small,
mass sensitivity. The second drawback is that the membrane pore size 1974). Consequently, the larger analyte is kept near the center of the
imposes limitations on the analyte molar mass range (Wahlund, tube and passes through the streamline quickly, whereas the smaller
2013). For the microplastic characterization, this membrane pore size analyte migrates closer to the channel wall and passes slowly through
limitation may cause the exclusion of environmental microplastics the streamline because of the hydrodynamic effect and van der Waals
that are smaller than the membrane's molecular weight cut-off interactions (Striegel and Brewer, 2012).
(MWCO). The main advantages of HDC are the rapid separation of particles
Besides AF4, sedimentation FFF could be an important alternative only based on size differences (Striegel and Brewer, 2012). HDC has
separation methods for microplastics based on density separation an advantage over AF4 by separating the interference signals of dis-
(Huppertsberg and Knepper, 2018). At present, sedimentation FFF has solved species from analyte particles in water. For example, Gray et al.
been widely used to separate and characterize various nanoparticles utilized HDC to separate dissolved Au from Au-NP-associated elements
(e.g., silica (Contado et al., 2013), silver (Liu et al., 2012), and titanium (Gray et al., 2012). In microplastics research, several studies employed
3. Visualization techniques
3.1. Examinations with optical microscopes
Visualization is important for identifying microplastics in sample

materials or debris (e.g., shell fragments, algae, sand, and glass)
(Hidalgo-Ruz et al., 2012). Conventionally, large microplastics
(1–5 mm) are identified with the aid of an optical microscope or using
the naked eyes. By evaluating the color, shape and light transmission
of plastic particles, MPs is distinguishable from non-plastic (Song
et al., 2015). Fig. 3 shows a mixture of microplastic particles that are
green, blue and purple, which are likely derived from consumer prod-
Fig. 2. Mechanism of particle separation in HDC. ucts (Eriksen et al., 2013). Polypropylene (PP) fibers were found to be
typically blue or red in color (Vianello et al., 2013). The features of
milky white color, slight shine and amorphousness makes expanded
HDC to separate microplastics and even nanoplastics from environmen- PS very easy to identify by naked eyes (Song et al., 2015), which some-
tal media (Brewer and Striegel, 2010; Philippe et al., 2014). Philippe times could obfuscates PS particles with minerals such as perlite. White
et al. evaluated separation performances of two types of HDC pellets dominate the majority of the debris, followed by transparent and
columns with different separation range (20–1200 nm and 5–300 nm) colored pellets (Heo et al., 2013). Optical microscope is used for smaller
for PS nanoparticles and several metal nanoparticles (Philippe et al., microplastics to obtain images for analysis, which provide the shape and
2014). They found that the particle retention behavior is not affected number of microplastics particles. In particular, the polarized light mi-
by material types but dependent on particle shapes significantly. Pirok croscopy was used to obtain a stacked image at different sample height
et al. utilized HDC and size-exclusion chromatography (SEC) to obtain and estimate the number of microplastics in synthetic water samples
size distribution of PS and polyacrylate NPs in the suspension (Pirok (Rodríguez Chialanza et al., 2018). Though visual sorting and identifica-
et al., 2017). Compared with SEC technique, HDC as a chromatographic tion is feasible for large microplastics with disguisable color or morphol-
separation method is advantageous and efficient in separating polymers ogies, particles without identifiable color or shape are challenging for
and organic nanoparticles, because polymers undergo interstitial visual sorting with naked eyes. Thus, electron microscopy providing
stresses as they pass through SEC columns (Striegel and Brewer, magnified images is critical for identifying ambiguous plastic-like parti-
2012). This interstitial stresses may negatively affect the polymer sepa- cles (Song et al., 2015).
ration efficiency and even damage the mechanically fragile polymers or Scanning electron microscopy (SEM) coupled with energy disper-
microplastics. sive X-ray spectroscopy (SEM-EDS) are widely used for characterizing
Table 1 presents the applications of FFF and HDC as separation morphology of ultra-small materials and determine their elemental
techniques used for MPs characterization. FFF and HDC provide similar compositions (Goldstein et al., 2017). SEM could provide high-
size-based selectivity. The main advantage of HDC is its rapid resolution topography images of objects and facilitate the differentia-
separation, analytical repeatability, and easy operation. However, HDC tion of the microplastics from other plastic-like particles (Cooper and
yields low selectivity and poor size resolution relative to FFF, which Corcoran, 2010). EDS provides the elemental information of the samples
cause low efficiency of separation for multi-component MPs. Besides, via detecting the characteristic X-rays emitted from the elements within
the analyte adsorption onto packing materials such as solid beads has the sample by the electron beam (Goldstein et al., 2017), which enables
been noticed. By contrast, FFF resolves multi-component MPs with a certain capabilities of microplastic identification in sample matrixes.
greater resolution than HDC, but with longer run times. Besides, the Table 2 shows the applications of optical microscope in microplastics
collected size fractions from FFF must be further analyzed by FTIR (MPs) characterization. Fries et al. used SEM-EDS to detect the presence
spectroscopy, Raman spectroscopy or GC/MS for identification of MPs of inorganic additives (e.g., titanium-dioxide nanoparticles) in
(Correia and Loeschner, 2018). microplastics samples (Fries et al., 2013). However, as most of
Table 1
Applications of FFF and HDC in MPs characterization.
Place/origins MPs type MPs size Abundance Major objective/findings Refs.
France/stimulated PS b1 μm Unknown AF4 was used to quantify and characterize the MPs samples. This (Gigault et al., 2017)
sample study successfully applied AF4 to the characterization of complex
samples with submicron MPs.
Netherlands/tap water PS, PE 50, 100, 200, 500 260 mg L−1 AF4 in combination with py-GC–MS was used to identify MPs in (Mintenig et al., 2018)
and surface water and 1000 nm (PS); different size fractions. This research proposed a method to
90–106 μm (PE) determine MPs with a broad spectrum of sizes in aquatic
environmental samples.
Denmark/fish sample PS, PE 100 nm (PS); 1.3 mg g−1 AF4 was applied for the size separation of MPs from the fish (Correia and Loeschner, 2018)
200–9900 nm (PE) fish samples. This study proved that AF4 enabled separating the MPs
from the digested fish and to determine their size.
United PS 50, 100, 200, 300, 1.04 g cm−3 HDC coupled with inductively coupled plasma mass spectrometry (Philippe et al., 2014)
States/stimulated and 500 nm was used to characterize the standard MPs suspensions under
sample different environmental efficiency. This study demonstrated that
HDC-ICP-MS is a promising method for MPs characterization in
complex media.
Netherlands/stimulated PS, PACR 76 and 59 nm 0.1% (PS; This study combined HDC and size-exclusion chromatography (Pirok et al., 2017)
sample (PACR); 0.1–0.5% (SEC) to separate various PS and polyacrylate (PACR) nanoparticles
44–915 nm (PS) (PACR)) in a mixture based on their sizes and obtain the distribution of the
particle size and the molecular size of PS and PACR nanoparticles.
compete with the fluorescent dyes (Shim et al., 2016). Lee et al. used a
fluorescence microscope to observe three sizes of fluorescently labeled
PS microbeads and study size-dependent effects on growth behaviors
of marine copepods (Lee et al., 2013). However, plastic materials usually
show significant fluorescence background or auto-fluorescence when
irradiated by near-UV or visible light (Piruska et al., 2005). Moreover,
chemical additives in plastic formulations may also affect fluorescent
properties (Piruska et al., 2005). For example, the additives such as
dyes (Lenz et al., 2015) and microbiological (Käppler et al., 2016), or-
ganic (humic substance) or inorganic (e.g., clay minerals) materials
(Elert et al., 2017) could exhibit fluorescence and interfere the fluores-
cence microscopy measurements. Thus, the fluorescence from these im-
purities should be minimized with proper pretreatment (Elert et al.,
2017). Typical pretreatment includes surface rinsing by acids or oxi-
dants (e.g., hydrogen peroxide) as well as enzymatic digestion (Löder
et al., 2017). It is worth noting that these pretreatments can only re-
move surface impurities or contaminants. The potential inferences
Fig. 3. Color variation among different microplastics.
The figure is adapted from (Eriksen et al., 2013) with permission.
from the blended chemicals such as dyes or plasticizers inside
microplastics are probably difficult to rule out by the typical pre-
treatment.
microplastics are non-conductive, SEM-EDS requires substantial sample
preparation and analysis time (e.g., sample drying, and sample deposi- 3.3. Flow cytometry (FCM)
tion, and carbon or gold coating), which may introduce artifacts and in-
terfere the morphological analysis for ultra-small microplastics. FCM analyzes particles within a moving flow based on the detection
Moreover, due to exposure to the high-energy electron beam, some of light scattering and fluorescence by laser excitation and enables rapid
plastic particles such as polyvinyl acetate (PVA, melting point high-resolution imaging (Fig. 5) (Adan et al., 2017). FCM has been
35–38 °C) and polyvinyl chloride (PVC, melting point 115–120 °C) widely used in counting and imaging of biological cells ranging from
that are thermally unstable may be softened or burned during the yeast (Attfield et al., 2000), bacteria in the milk (Gunasekera et al.,
SEM examination. 2000), pathogens in food products (Comas-Riu and Rius, 2009) and im-
mune cells of the blood (Graham et al., 2010). Since most microplastics
3.2. Fluorescence microscopy scatter light and emit certain optical properties, FCM offers a rapid and
robust analysis for MPs (see Table 4) (Canesi et al., 2015; Long et al.,
Different from regular optic microscopes that rely on image contrast 2016; Maes et al., 2017; Schnekenburger et al., 2018; Sgier et al.,
from light reflection on sample surface, fluorescence microscopes col- 2016; Shim et al., 2016). Sgier et al. utilized FCM to detect and separate
lect fluorescent emission from samples that are excited by the excitation polystyrene microplastic particles from the biofilm samples to under-
wavelengths with proper selection of the filter cubes or lasers stand microbial community dynamics (Sgier et al., 2016). Other studies
(Lichtman and Conchello, 2005). Fluorescence microscopy has been utilizing FCM commonly include the detection of MPs in organisms,
widely used in studies of biological specimen (e.g., animal cell lines, bac- such as bacteria, invertebrates, and phytoplankton and highlight the po-
teria, and pollen) (Axelrod, 2001; Donnert et al., 2006; Fonseca et al., tential of interactions between microorganisms and microplastics
2002) as well as MPs. Table 3 gives some applications of fluorescence (Canesi et al., 2015; Long et al., 2016; Schnekenburger et al., 2018).
microscopy in MPs characterization. Qiu et al. counted the number of Besides, FCM has proven to be a promising approach to characterize
MPs using a fluorescence microscope (Fig. 4) and found that MPs ap- microplastics in seawater and study their impacts on marine aggregates
peared brightly-colored under the fluorescence microscope. The fluo- and settling rate (Long et al., 2016; Long et al., 2017; Schnekenburger
rescence signal was generated from the fluorescent whitening agents et al., 2018). Long et al. assessed the interactions and impacts of 2-μm
or additives during the production of plastics (Qiu et al., 2015). Typi- PS beads on marine phytoplankton using FCM. The particle counting
cally, a fluorescent dye (i.e., Nile Red) (Shim et al., 2016) is used to and formation of hetero-aggregates were both illustrated by FCM. It
label plastic particles, especially when detecting MPs in tissues or organ- was found that phytoplankton may contribute to the absence of MPs
isms (Cole et al., 2013). Before staining MPs in the environmental sam- on water surface as MPs can bind to microalgal cells and form aggre-
ples such as soil or sediment, the samples are usually density-separated gates that sink from surface water (Long et al., 2017). Woods et al. quan-
with a saturated NaCl solution by vigorously shaking and overnight set- tified the uptake, digestion, and egestion of polyethylene terephthalate
tling to remove proteins and organic matters that may interfere or (PET) microplastics fibers (Fig. 6) in blue mussels using the FCM and the
Table 2
Applications of optical microscope in microplastics (MPs) characterization.
Place/origins MPs type MPs Abundance Major objective/findings Refs.

size
USA/seawater PP, PE, PS, PA b5 mm 0.025 g mL−1 Stereomicroscope was used to observe the occurrence of MPs in sediments and (Fries et al., 2013)
chemical and morphological characterization was performed using SEM.
South EPS b1 mm 0–0.3 items L−1 Stereomicroscope was used to identify and count the MPs in seawater and (Song et al., 2015)
Korea/seawater (Seawater); 631 items beaches. This study found the microscope method for identification of MPs is
and beach L−1 (Beach) easier and faster, while the spectroscope method was more accurate.
United states/lake Unknown b1 mm 43,157 ± 115,519 SEM/EDS was used for microscopic and elemental analysis of MPs. This study (Eriksen et al., 2013)
water items km−2 found the presence of multi-colored sphere MPs in the Laurentian Great Lakes.
Italy/shallow PE, PP, PS b1 mm 672–2175 items kg−1 SEM-EDS was used to study the surface morphology of the MPs. This research (Vianello et al., 2013)
waters found that the abundance of MPs smaller than 1 mm were correlated with the
finer sediment fraction and the metal pollution index.
Table 3
Applications of fluorescence microscopy in microplastics (MPs) characterization.
China/sediment HDPE, PET, b5 mm 5.1–87.1 items g−1 Fluorescence microscopy was used to count the number of microplastics in the (Qiu et al., 2015)
PE and PS sediment extracted sediment samples, and this study evaluates the occurrence and
abundance of microplastics in China for the first time.
UK/stimulated PS 7.3–30.6 μm 635–3000 items Fluorescence microscopy was used to analyze the ability of zooplankton to ingest (Cole et al., 2013)
seawater ml−1 microplastics. This research showed that marine microplastic debris can
negatively impact upon zooplankton function and health.
USA/simulated PS 0.05, 0.5, 5 × 105–9.1 × 1011 Fluorescence microscopy was used to observe the presence of fluorescent (Cole et al., 2013)
sample 6 μm items ml−1 microplastics beads in the copepods. Results showed that micro- or nanosized PS
beads may cause a significant decrease in survival rate and fecundity of marine
copepods.
Sweden/coast Unknown 0.5–1 mm 0.01–0.14 items Fluorescence microscopy was used to observe the colored plastic fibers in the (Sweden, 2007)
water m−3 sample and this study measured the abundance of MPs in Swedish west coast
waters successfully.
Japan/stimulated Fluoresbrite 3, 6, and 1.5 × 105 Fluorescence microscopy was used to confirm the incorporation of microspheres (Okubo et al., 2018)
water carboxylate 11 μm microspheres mL−1 into the planktons and help the quantification of the microsphere.
concentrations of PET microplastics in mussels collected in filtered sea- 4. Physicochemical quantification and mapping
water are ranging from 3000 to 30,000 MPs per liter (Woods et al.,
2018). Furthermore, because of its real-time monitoring, FCM over- 4.1. Dynamic light scattering (DLS) for the hydrodynamic size and zeta po-
comes the limitations that traditional FTIR method requires the concen- tential measurements
tration of microplastics in liquid samples by filtration or centrifugation
since there are only a few particles in a huge amount of liquid DLS has intensiveley been used to investigate the hydrodynamic size
(Schnekenburger et al., 2018). Schnekenburger et al. used FCM with in- and surface charge of particles in liquid environments (Bhattacharjee,
frared light and quantitative phase contrast imaging to detect MP parti- 2016). As shown in Fig. 7, DLS uses a laser beam to pass through a liquid
cles and their interaction with bacteria in different detection channels suspension containing the analyte particles that scatter the incident
based on their size and refraction index properties. This novel combina- laser at different scattering angles (θdls). The Brownian motion of the
tion of optical spectroscopy proves to omit labor-intensive filtration detected particles induced the shift in light frequency, which varies
processes as pre-treatment, which significantly increases the through- with different particle sizes (Langevin et al., 2018). The shift in light fre-
put (Schnekenburger et al., 2018). Canesi et al. utilized FCM to evaluate quency would result in time-dependent fluctuations in the intensity of
how amino-modified PS nanoparticles (PS-NPs) induced apoptotic pro- scattered light. These fluctuations contain information about particle
cess of marine invertebrates and found that PS-NPs mainly target the size and shape (Verma and Maheshwari, 2018). The hydrodynamic ra-
immune function (Canesi et al., 2015). dius and size distribution of measured particles are calculated using a
However, there are several major limitations existing for the use of function of the scattered light signal over time in tandem with the
FCM: (1) the microparticles must be suspended separately and individ- Stokes-Einstein equation (Lim et al., 2013). Similarly, the electropho-
ually in the flow cytometer and thus the interactions between retic mobility of particles in an applied electric field can be measured
microplastics or between microplastics with other particles (e.g., bacte- through the detection of frequency shifts in the scattered light and fur-
ria, and sediments) could not be analyzed (Jahan-Tigh et al., 2012); ther used to determine the zeta potential of particles through the
(2) there is a lack of standardization in the instrument set-up and the Henry's equation (Kaszuba et al., 2010).
data analysis (Mullier et al., 2011); (3) the data process with spectral As a non-invasive technique that works on a wide range of liquid
compensation might cause the visualization artifacts (Erdbrügger samples with relatively low sample volumes (Stetefeld et al., 2016),
et al., 2014; Roederer, 2001); and (4) intensive data is generated during DLS has been extensively applied in biological, physical and chemical
the measurements and the flow data interpretation is complicated and fields (Xu, 2015), especially in the investigation of colloidal properties
labor-intensive (Jahan-Tigh et al., 2012). In order to overcome the lim- of nanoparticles and microparticles. Equivalently, DLS is also useful in
itations mentioned above, the researchers made some efforts, including: the characterization of microplastics and nanoplastics. For instance,
(1) developing the standardization strategies by using size-calibrated DLS was used to measure the size and the zeta potential of microplastics
microplastics and improving the detection of microplastics of smaller and nanoplastics in biological matrices such as Pacific oyster (González-
size (Lacroix et al., 2010); (2) trial of new kinds of fluorescent dyes Fernández et al., 2018) and planktonic crustaceans (Gambardella et al.,
(Ullal et al., 2010); and (3) technological advancements such as auto- 2017) as well as the aggregation of microplastics (Summers et al.,
mated instrument setup and compensation (Maecker et al., 2010). 2018). Additionally, DLS technique can be added into other systems to
Fig. 4. The fluorescence microscope images with 100× magnification of: (a) long, (b) middle, and (c) short class of microplastics.
The figure is adapted from (Qiu et al., 2015) with permission.
reported in the studies that involved multiple kinds or sizes of particles

in one aqueous sample (James and Driskell, 2013; Li et al., 2011; Zhang
et al., 2012a).
4.2. Nanoparticle tracking analysis (NTA)
NTA was developed and first commercialized by NanoSight Ltd. in

2006 (Filipe et al., 2010) to measure concentrations of poly-dispersed
samples in addition to the hydrodynamic size measurement (Malloy
and Carr, 2006). NTA applies intense laser light to illuminate free diffus-
ing particles to track their Brownian motion with monochrome imaging
(Bhattacharjee, 2016). Fig. 8 shows a typical operation diagram of NTA
detection system, where a laser beam passes through a prism edged
glass flat within the sample chamber into the particle suspension
(Carr and Wright, 2008). When the particles in suspension appear in
the scatter light path, they can clearly be visualized and recorded
frame by frame using a high-sensitivity camera or charged coupled de-
vice (CCD) detector. The motion trail of the particles can be obtained
and analyzed through the recorded frames (Fig. 9). Further calculation
of hydrodynamic sizes is completed with the average distance between
each particle, temperature and solution viscosity through the Stokes-
Einstein equation (Boyd et al., 2011).
Both DLS and NTA measure the Brownian motion of nanoparticles
and calculate the hydrodynamic diameter based on diffusion coefficient
through the Stokes–Einstein equation. Different from DLS, the NTA tech-
nique further visualizes particles with a microscope and analyzes the
motion of each particle frame by frame, which ultimately enables the
Fig. 5. Schematic diagram of a flow cytometer. calculation of particle concentration in the aqueous suspension (Carr
Figure is adopted from Ref. (Adan et al., 2017) with permission.
and Wright, 2008). And the accurate particle size distribution profiles
derived accordingly for individual particles (Malloy and Carr, 2006).
allow a convenient and instant identification for the degradation of Based on this advantage, individual particles from 10 nm to 1000 nm
microplastics. Gigault et al. connected a photo-reactor with DLS to in- can be detected to give particle-by-particle size and number distribu-
vestigate the photodegradation of marine microplastics under different tion data under NTA, rather than the average size data generated by
conditions without sampling and manipulation (Gigault et al., 2016). DLS (Carr and Wright, 2008). Besides, NTA provides individual particle
However, due to the complexity of the food matrix, DLS is unable to dif- intensity as well as motion videos that DLS does not provide (Hou
ferentiate microplastics from other particles that may also scatter light et al., 2018).
or laser beams (EFSA, 2016). However, the accuracy of NTA is restricted by Brownian motion lim-
In the DLS system, suspended particles scatter incident light with itations, because particles move randomly under Brownian motion in
signal intensity proportional to the 6th power of particle radii the beam of the laser at a speed related to their size, with larger particles
(Rademeyer et al., 2015). As a result, for the mixture of large and moving slower than smaller particles (Carr and Wright, 2008; James
small particles in a sample, larger particles scatter much more intensely and Driskell, 2013). Thus, to achieve the measurement accuracy of
than smaller ones, then the signals from the bigger particles may out- NTA, particles cannot be too polydisperse or too close together in size.
weigh the signals of smaller particles and thus overlook the presence In contrast, DLS relies on the intensity fluctuations of scattered light
of smaller particles (Carr and Wright, 2008). Therefore DLS can only resulting from particle Brownian motion and thus DLS is more sensitive
measure the average size. When aggregates of protein and gold nano- to larger particles than smaller ones (Yguerabide and Yguerabide,
particles formed in the suspension, the mean particle size would in- 1998). For examples, both DLS and NTA have been used to compare
crease significantly. This phenomenon, for instance, has been widely their performances in the measurement of particle size distribution.
Table 4
Applications of FCM in MPs characterization.
Swiss/stream water Unknown 0.2–200 μm Unknown FCM was used for detection and characterization of microplastics in stream (Sgier et al., 2016)
biofilms. This study presented a method for the analysis of biofilm community
structure and enabled the detection of microplastic contamination in field.
France/simulated PS 2 μm 3.96 μg L−1 FCM was used to quantify and characterize small microplastics in seawater and (Long et al., 2017)
water help to monitor their presence and compare the distinctions. The results
highlighted the potential for single phytoplankton cells and residual organic
matter to interact with microplastics.
France/simulated PS 2 μm 1.050 kg L−1 MPs concentrations in the aggregates were measured by FCM. This study found (Long et al., 2016)
water that MPs can bind to microalgal cells and thus be incorporated to aggregates in
surface water or later sink.
United Unknown 250 μm Unknown This study developed a method device concepts “MicroPlastiCarrier” to (Schnekenburger et al., 2018)
States/wastewater overcome the limitations of the microplastics' safe identification size of liquid
media in original FTIR method.
United PET ~460 μm 3 to 30 Imaging FCM was used to detect and measure change of MPs fiber caused by (Woods et al., 2018)
States/simulated particles the intake and ingestion of blue mussels. This study confirms that blue mussels
water mL−1 accumulate MPs fibers during filter-feeding.
Fig. 6. PET MPs fibers as imaged by the FCM.

The figure is adapted from (Woods et al., 2018) with permission.
The study about heat-induced effects on casein micelles demonstrated results of polystyrene concentrations of 107–109 particles mL−1. By con-
that the NTA could provide direct visual information on submicron par- trast, DLS is unable to quantify particle concentrations in liquid samples.
ticles, while the more reproducible and reliable estimate of the particle
size distribution was obtained from DLS results (Le et al., 2008). A re- 4.3. Fluorescence spectroscopy
search on aggregation of cerium oxide nanoparticles with Ca+ and algi-
nate showed that the NTA was more accurate in detecting small Fluorescence spectroscopy systems use an objective lens to focus ex-
aggregates, and the DLS was better in studying the large aggregates citation light into the sample and collect the fluorescence emission
(Hou et al., 2018). Thus, NTA and DLS are complementary. Table 5 com- (Fig. 10) (Cumberland et al., 2012). Fluorescence spectrophotometry is
pares the key features of NTA and DLS with guidance for researchers to commonly used to assess the presence of dissolved organic matters or
select proper techniques for sample measurements. carbons in surface and ground waters (Henderson et al., 2009; Hudson
Though NTA has demonstrated unparalleled sensitivity and accuracy et al., 2007). The development of fluorescence-scanning instruments
in the measurement of particle size and concentration in liquid, NTA has to produce excitation–emission matrices (EEMs) has enabled the fin-
mainly been used to study colloidal nanoparticles (Ryu et al., 2007; gerprint mapping of the fluorescent organic fractions in water samples
Studer et al., 2010) with very limited numbers of studies on via the identification and correlation of fluorophores with different
microplastics. For example, Lambert et al. applied NTA to characterize polymers or organic matters in water (Le Coupannec et al., 2000).
the formation of nanoplastic particles during the degradation of a dis- Fluorescence spectroscopy is shown to be useful to characterize tox-
posable PS coffee cup lid and the time-resolved evolution of particle icity and investigate the negative effects of microplastics for organisms
size distribution of PS nanoplastic particles has been successfully mea- in soil or water, such as inhibition of enzymatic activity and disorder
sured (Lambert and Wagner, 2016). Filipe et al. evaluated the NTA tech- of energy metabolism (Liu et al., 2017; Zhao et al., 2017a). Table 6 sum-
nique using polystyrene nanoparticles and compared the results with marizes the applications of fluorescence spectroscopy for the detection
DLS (Filipe et al., 2010). The NTA measurements rendered quantitative and quantification of microplastics in organisms and in water. For
Fig. 7. Optical configuration of the typical experimental setup for DLS measurements. The setup can be operated at multiple angles.
The figure is adapted from (Lim et al., 2013) with permission.
Fig. 8. Schematic of the optical configuration used in Nanoparticle Tracking Analysis (NTA).
The figure is adapted from (Carr and Wright, 2008) with permission.
example, Chen et al. utilized fluorescence spectroscopy to analyze the 4.4. Hyperspectral imaging (HSI)
interactions between PS microplastics and humic acid (HA), an aromatic
model dissolved organic matter (DOM), under different pHs. This study HSI generates images with spectral information that are pertinent to
explored the spectroscopic and microstructural changes of DOM-MPs the scanned materials in the sample. Based on the unique interaction
complex through the detection of increased fluorescence intensity between different chemical species in the sample and the incident
changes. The findings provided an analytical platform for evaluating light with different wavelengths, the specific light absorption or scatter-
MP heteroaggregation and the roles of MPs in the transportation of ing reflects as distinctive spectra over a wavelength range (Chang,
other contaminants in the environment (Chen et al., 2018). Fluores- 2003). These spectral signatures or fingerprint features are highly de-
cence spectrophotometer was also used to measure the nanoplastics pendent on the chemical composition and physical structure (e.g.,
concentrations in larvae (Chen et al., 2017a) and zebrafish (Chen shape, size and color) of different materials (ElMasry et al., 2012). The
et al., 2017b). Though fluorescence spectroscopy enables detection of generation of hyperspectral images are commonly performed in three
microplastics in single absorption line and emission line with high sen- modes, i.e., point scanning, line scanning, and plane scanning (Fig. 11)
sitivity, it demands the samples to be self-fluorescent or labeled with (Amigo et al., 2013). In the plane scanning mode, the light reflected
fluorescent dyes. As well, typical pretreatments including centrifugation from the tested object is scattered by the raster of the spectrometer
and digestion by acids or oxidants (e.g., hydrochloric acid and sodium onto photodetectors in different directions. The dispersed photons on
hydroxide) are required for purification of MPs in microglial cells the photodetectors induce electrical pulses and produce a two-
(Chen et al., 2017b). dimensional image. Then scanning across the sample surface enables a
Fig. 9. A typical video frame (a) and a path of one tracked particle recorded by NTA for the measurement of the particle size.
The figure is adopted from (Boyd et al., 2011) with permission.
Table 5 titanium dioxide NPs (Kuang and Zhang, 2016). For example, Théoret
Comparison of the characteristics of NTA and DLS techniques. et al. analyzed transformation kinetics of Ag NPs in wastewaters and vi-
NTA DLS sualized silver NPs in complex wastewater (Théoret and Wilkinson,
Size range 10 nm ~ 1000 nm 1 nm ~ 10 μm
2017). HSI has been used to evaluate particle sizes, shapes and polymer
Principle Brownian motion of nanoparticles Brownian motion of types of microplastics such as PP, PS and polyethylene (PE) in both ma-
nanoparticles rine and soil environments (Bonifazi et al., 2017; Karlsson et al., 2016;
Measurement Video of particle motion Fluctuation of scattered Serranti et al., 2018; Shan et al., 2018; Shan et al., 2019; Zhang et al.,
basis light intensity
2019b). Karlsson et al. monitored MPs in real seawater with HSI and de-
Advantages • Provide particle number • Measure zeta potential of
concentration and size of particles termined the particle recognition size limit of HSI technique is 300 μm
individual particles • Quick and user-friendly (Karlsson et al., 2016). Besides, Shan et al. employed HSI with chemo-
• Direct visual information with • Reproducible and reliable metrics to characterize white and black PE particles from soil through
particle motion video estimate of the particle size obtaining the mean hyperspectral spectrum of various materials
• More accurate in detecting small distribution
aggregates • More accurate in detecting
(Fig. 12) and differentiated the PE microplastics from the environmental
large aggregates surroundings including rocks, leaves, rubber and branches. This study
Limitations • The motion trail of some particles • Large particles might demonstrated the capacity of HSI for the chemical characterization
might be out of the camera view obscure the presence of and identification of microplastics (0.5–5 mm) with relatively simple
and cannot be measured smaller particles
sample preparation or purification of microplastics from the environ-
• Set-up parameters need to be • Cannot differentiate
adjusted to obtain high accuracya between different materials mental matrix. However, only the microplastics on the surface of the
• Not suitable for particles that are • Not suitable for soil were detected, whereas the microplastics underneath the soils are
too polydisperse or too close in gravitationally settling not observable by HSI.
size particles HSI is a rapid, label-free, non-invasive, non-destructive and reliable
Concentration • Limited (107–109 particles mL−1) • Broad (about 108–1012
imaging platform. HSI provides direct visualization of samples with pos-
range particles mL−1)
a
sible chemical identification and also enables the mapping of chemical
The parameters corresponding to the acquisition process such as the gain or sensi-
distributions of targeted components (Shaw and Manolakis, 2002;
tivity of the camera, the open time of the camera electronic shutter, and alternate gamma
can influence the measurement accuracy. Siripatrawan et al., 2011). However, the major drawback of HSI is the
operation complexity and the data processing step. HSI requires
model or well-known materials to calibrate the pixel information,
three-dimensional hyperspectral image hypercube, which contains the which is used to analyze unknown samples via a model transfer proce-
spatial and spectral information such as morphological features and dure (ElMasry and Sun, 2010). Since the hyperspectral mapping data
chemical characteristics of the analyte (Lu and Fei, 2014; Shaw and (pixels per lines) are massive, users have to develop customized
Manolakis, 2002). algorisms to extract the information they desire for (Lu and Fei, 2014;
HSI is widely used in the research fields of agriculture (Ravikanth Shukla and Kot, 2016). Besides, relatively low imaging quality compared
et al., 2017), medicine (Lall et al., 2017), food processing (Shi et al., to electron microscopes (Feng and Sun, 2012), the low scanning frame
2017), physics (Manolakis et al., 2016) and especially in nanomaterial rates and the requirements of academic training also hinder the realiza-
characterization such as graphene (Zhang et al., 2018), carbon nano- tion of the full potential of HSI (Roberts et al., 2018; Schneider and
tubes (Wang et al., 2018), cerium oxide NPs (Idelchik et al., 2018) and Feussner, 2017). In order to provide a reference for the researchers to
Fig. 10. Schematic diagram of a fluorescence spectrophotometer.

The figure is adapted from (Al-Rawashdeh, 2012) with permission.
Table 6
Applications of fluorescence spectroscopy in microplastics (MPs) characterization.
Place/Origins Material Size of MPs Concentrations Applications Refs.

of MPs
China/simulated PS 20 mm, 6 mm, 0–100 mg L−1 Map and characterize the effect of DOM on the microstructure of MPs (Chen et al., 2018)
water 500 nm and 80 nm to assess the environmental behavior of DOM and MPs.
China/simulated PS 5 μm 10 mg mL−1 and Detect microplastics accumulation in the gills, liver, and gut of crabs. (Yu et al., 2018)
water 25 mg mL−1
China/simulated PS Unknown 0.05 mg m L−1 Detect tryptophan protein-like substance in PS nanoplastics. (Feng et al., 2018).
water
UK/seawater Unknown 5–10 mm 0.6 mg g−1 and Detect cadmium, lead and bromine in microplastics from two (Massos and Turner, 2017)
30 mg g−1 beaches to track the potential sources of microplastics.
Denmark/simulated PS 2 mm and 100 nm 1 mg L−1 Detect microplastics in Daphnia magna (D. magna) bodies to quantize (Rist et al., 2017)
water animal body burdens of microplastic particles.
China/simulated PS 45 μm and 50 nm 1 mg L−1 Measure the nanoplastics concentrations in zebrafish larvae. (Chen et al., 2017a)
water
China/simulated PS 50 nm 1 mg L−1 Measure the nanoplastics concentrations in the supernatants of (Chen et al., 2017b)
water zebrafish samples.
China/simulated PS 100 nm 1–10,000 μg L−1 Detect nanoplastic particles accumulation in the medium to (Zhao et al., 2017a)
water characterize nematode absorption characteristics of nanoplastics.
select the proper physicochemical characterization tool, Table 7 com- (Fu and Zhang, 2018), microbial cells (Alsteens et al., 2007), polymeric
pares the respective analytical strength and limitations of DLS, NTA, membranes (Fu et al., 2017), and nanostructured surface (Kuna et al.,
fluorescent microscopy or spectroscopy and HSI. 2009). Compared to SEM, AFM enables holistic characterizations includ-
ing surface morphology (Bieletzki et al., 2010), stiffness (Zhang et al.,
4.5. Atomic force microscopy (AFM) and hybrid AFM techniques as emerg- 2012b), adhesiveness (Zhang et al., 2011), hydrophobicity (Fu and
ing characterization platforms Zhang, 2018), conductivity (Trotsenko et al., 2016), magnetization
(Middea et al., 2015), and work function (Bieletzki et al., 2010). More
AFM provides a unique feasibility for nanoscale characterization of importantly, the original sample can be preserved during the AFM anal-
materials (Last et al., 2010; Stawikowska and Livingston, 2013). ysis as the measurements can be operated in liquid and air (or vacuum)
Fig. 13a shows a schematic diagram of AFM, which operates by scanning with desirable conditions. Compared to the other techniques, AFM anal-
across the sample surface with a tiny tip (typical end diameter ysis requires relatively simple sample preparation such as spin coating
5–10 nm). As the tip approaches the sample surface, the force produced or mechanical trapping of samples on different substrates such as
by the tip-sample interaction causes the cantilever deflection, which is gold, mica and silicon wafer. For microplastic samples, adhesive pads
measured with a photodiode detector and transferred to obtain the sur- or tapes may be used to immobilize and mount samples onto steel
face information (Butt et al., 2005; Webb et al., 2011). AFM has been mounting disks. Recently, AFM has been applied to study bacterial ad-
widely applied in the nanoscale characterization of various samples, herence, degradation and destabilization of MPs in marine ecosystems,
such as soil particles (Cheng et al., 2009), engineered nanoparticles including plastic marine debris, such as polyvinylchloride (PVC) and PE
Fig. 11. Three common configurations in HSI devices.

The figure is adapted from (Amigo et al., 2013) with permission.
Fig. 12. (a) Hyperspectral imaging of soil covered with microplastics and other materials; (b) Region of interests of each type material; (c) Obtained spectra from region of interests of each
type material; (d) Region of interests of environmental surroundings and microplastics particle 1–5 mm (d1) and 0.5–1 mm (e1); and classification results for 1–5 mm microplastics (d2)
and 0.5–1 mm microplastics (e2) on the hyperspectral image (Shan et al., 2018).
(Dussud et al., 2018; Kumari et al., 2019). AFM detected morphological Raman or FTIR spectroscopy provides an average chemical information
changes on plastic surfaces after bacterial colonization and growth at a bulk area with limited spatial resolution for the detection of domain
(Kumari et al., 2019). Thus, AFM is a promising technique for character- differences within a sub-micrometer region (Miller and Dumas, 2010).
ization of MPs and nanoplastics and deserves further exploration and This limitation might hamper the analysis of MPs or nanoplastics with
application in future studies. size below the spatial resolution (down to 3 μm) (Lasch and
However, there are some limitations of AFM that could hinder its Naumann, 2006). AFM in combination with Raman (AFM-Raman,
wide applications. For instance, AFM usually scans samples at relatively Fig. 13b) and IR (AFM-IR, Fig. 13c) techniques to enable nanoscale
slow rates (b1 Hz, up to 1 μm per second) in order to acquire high- chemical identification and mapping of composites on sample surfaces.
quality images. The probe has limited motion flexibility (i.e., the probe's Hanna et al. used AFM-IR to study a blend of PS and polymethyl meth-
z-axis motion is restricted to 5 μm) and the maximum reported scan- acrylate (PS/PMMA) and present the chemical identification and distri-
ning size is 120 μm × 120 μm (Kasas et al., 2001) on AFM, which is bution of PS in the polymer blend at nanoscale (Fig. 14) (Hanna et al.,
much smaller than the scan rates and areas achieved on optical micro- 2013). Similarly, AFM-Raman has also been applied in polymer blend
scopic techniques. However, some advanced modes of AFM (e.g., characterization by Yeo et al., who investigated the surface composition
Bruker's PeakForce® and FastScan® modes) enables faster scanning on a blended polyisoprene (PI)/PS thin film and differentiated the distri-
speeds (up to 2.5 kHz, N2 mm per second), which are even faster than butions of PI and PS (Fig. 15) (Yeo et al., 2009). Clearly, hybrid AFM em-
the average scanning rate of SEM. Another limitation of AFM is that powers the identification and imaging of chemical components of MPs
the tip-sample interactions or the image-processing processes may in- with a high resolution.
troduce artifacts (Ricci and Braga, 2004; Ukraintsev et al., 2012). For in- So far, there have been a very limited number of studies using hy-
stance, when the tip is in contact with samples, the contact may result in brid AFM techniques (AFM/IR or AFM/Raman) to detect and charac-
release of fragments such as adhesive polymers that attach to the tip terize MPs. Part of the reasons are that AFM is often used to acquire
surface, which reduces the imaging resolution and even produces erro- nanoscale surface mapping and quantification. Large MPs as large
neous images of samples. as a few hundred micrometer or millimeters may not be suitable
Besides morphological information, probing chemical properties is for AFM examinations. Moreover, to perform such localized scan-
also achieved with the combination of AFM and Raman or IR techniques ning, AFM requires sample sizes and surface roughness to be as
(Dazzi et al., 2012; Fu and Zhang, 2017; Hung et al., 2015). Traditional small as possible (e.g., b100 nm), which is another challenge when
Table 7
Comparison of physicochemical characterization of microplastics by different analysis techniques.
Techniques Analytic capabilities Advantages Disadvantages
DLS Size distribution; zeta potentials Facile sample preparation, high throughput and The signals from the bigger particles might overwhelm the signals of
(Filipe et al., 2010) reproducibility (Fischer and Schmidt, 2016). smaller particles and obscure the presence of smaller particles,
causing significant bias on the size determination.
NTA Number concentration and size High sensitivity, size resolution, ease of use, and NTA data acquisition and analysis are highly affected by the selection
distribution; Video of particles availability of information on individual particle of analysis parameters in the software and the microscope for video
motion counts (Gruia et al., 2015). capture (Hole et al., 2013; Roursgaard et al., 2014).
Fluorescence Physical and chemical mapping; Low detection limit, high sensitivity, single Demanding sample preparation requirements (e.g. fluorescent dyes
Spectroscopy semi-quantitative analysis (Thiel, absorption line and emission line, and wide or labels); poor elemental sensitivity (Towett et al., 2013).
2001). linear range of standard curve.
HSI Direct visualization of physical and Label-free, non-destructive and reliable imaging HSI's signal quality is not as high as X-ray vision system.
geometrical features; Possible platform. HSI needs standardized calibration and model transfer procedures as
chemical identification an indirect method.
Potential interferences in chemical identifications from contaminants.
Fig. 13. Schematic diagram of (a) conventional AFM, (b) AFM-Raman and (c) AFM-IR.
The figure is adapted from (Aguayo and Bozec, 2016) with permission.
dealing with large MPs. For instance, the chemical mapping 5. Chemical identification
results from AFM-IR requires effective local IR absorption and
detectable thermal expansion (Dazzi et al., 2012). The thermal ex- 5.1. FTIR spectroscopy
pansion of MPs induced by the IR absorption could be too small to
be detected on MPs, which reduces the detection sensitivity. Other Fourier transform infrared (FTIR) spectroscopy acquires chemical in-
artifacts could also arise during the AFM-IR imaging due to the formation through detecting the vibration modes of sample molecules
peak tracking errors and cantilever damage or wear (Kenkel and at different infrared frequencies over a wide spectral range (Stuart,
Bhargava, 2019), especially under fast scanning rates. Usually, the 2005). Interferograms collected by detector are Fourier transformed
researchers could slow down the scanning speed to minimize the ar- into a conventional absorbance spectra against wavenumbers, at
tifacts but it results in much longer data collection time to an order of which characteristic absorbance or transmittance peaks correspond to
days or hours. specific chemical bonds or molecular vibrations (Smith, 2011).
Fig. 14. AFM topography image (a) and AFM-IR chemical mapping (3026 cm−1, benzene ring in the PS) of a PS/PMMA blend sample.
The figure is adapted from (Hanna et al., 2013) with permission.
Fig. 15. AFM topography images (a) and Raman spectra (b) of a PI/PS film.
The figure is adapted from (Yeo et al., 2009) with permission.
FTIR mainly has four sample analysis techniques: transmission 2012). In an ATR-FTIR mode, the IR light enters the ATR crystal and is to-
(Käppler et al., 2015), diffuse reflectance (Guo et al., 2017), true specu- tally reflected at the crystal-sample interface. The internal reflection
lar reflectance/reflection-adsorption (Roodenko et al., 2018) and atten- forms an evanescent wave that is attenuated as the sample absorbs en-
uated total reflection (ATR) (Ramer and Lendl, 2006; Tobin et al., 2016). ergy and after one or multiple internal reflections, the IR light exits the
In the transmission mode, the sample is directly placed in the IR beam crystal toward the detector to generate the IR spectrum (Ramer and
that passes through samples, and the transmitted IR signal is measured Lendl, 2006).
as a spectrum over different IR wavelengths (Käppler et al., 2015). The To get the accurate IR spectrum, the mode selection is mainly based
diffuse reflectance mode directs the infrared light on a sample and the on the properties of the measured samples. For instance, the diffuse re-
diffuse reflectance is produced by the sample surface's reflection of flectance mode is ideal for the fine powder samples with size smaller
the light in all directions. Such reflected or scattered IR light energy is than 10 μm (Radjenović et al., 2019). The samples that are thick or
collected by a detector and generate a characteristic spectrum related strong-IR-absorbent are usually measured by the ATR mode, while the
to the materials (Mitchell, 1993). Different from diffuse reflection that samples that are not soft enough to form good contact are difficult to
reflects light in all directions, the specular reflectance/reflection- study with ATR mode (Tobin et al., 2016). Transmission mode works
absorption mode collects the reflected energy from a sample surface on relatively thin samples that allow the IR beam to pass through the
at a given angle of incidence and the reflected IR light energy depends sample. True specular reflectance/reflection-adsorption analyzes the
on the absorption or refractive index of the sample (Khoshhesab, samples with large, flat and reflective surfaces (Käppler et al., 2015).
Table 8
Advantages and applicable samples of different operating modes in FTIR.
Modes Advantages Applicable samples Applicable forms of MPs
Diffuse reflectance • Little to no sample preparation • Samples that can be ground into • Thin films (b1 μm)
• No need for pressed KBr pellets a fine powder • Irregularly shaped
▪ Soft powders and powder
mixtures
▪ Tablets
▪ Rigid polymers
Attenuated total reflection (ATR) • Little to no sample preparation • Strongly absorbing or thick • Thin and thick fibers
• Nondestructive analysis samples • Powders
• Ideal for thick or strong-IR-absorbent samples ▪ Plastics • Thin and thick films
▪ Laminates • Irregularly shaped
▪ Rubbers
▪ Paints
Transmission • Well established • Samples that can be passed by IR • Thin films
• Excellent spectral information beam • Powders
• Great for quantitative work ▪ Thin polymer films • Thin fibers
▪ Soluble polymers
▪ Thermoplastic powders
True specular • Sensitivity to monolayer samples • Samples having large, flat, • Smooth and thick films
reflectance/reflection-absorption • Nondestructive analysis reflective surfaces
▪ Metallic surfaces
▪ Silicon wafers
▪ Laminated materials on metals
Micro-FTIR • Provide chemical mapping • Applicable for all samples • Regularly shaped MPs for
• Detect the characteristic bands of samples with sizes as micro-reflectance mode;
small as 10 μm • Thick and opaque MPs for
micro-reflectance mode;
•Transparent MPs for
micro-transmittance mode
• Almost all the MPs applicable for
micro-ATR mode.
In both ATR and transmission modes, FTIR analysis requires thin sam- 2019), surface water (Wu et al., 2019), sediments (Peng et al., 2020;
ples to avoid complete absorption of infrared beam (Käppler et al., Zhang et al., 2019a), sewage (Yang et al., 2019), leachate (Su et al.,
2016). Table 8 summarizes the advantages and applicable samples of 2019b), atmosphere (Liu et al., 2019), food (Li et al., 2020), and
different operating modes in FTIR, providing a reference to the readers. organisms such as mussels, shrimps, and fish (Li et al., 2019) (Nan
FTIR spectroscopy has been reported in the identification of MPs in et al., 2020; Su et al., 2019a) have been identified and characterized by
costal environment (Frias et al., 2010) and the frozen ice in Arctic sea μ-FTIR, especially for samples that are too small to be chemically ana-
(Browne et al., 2011). Moreover, FTIR combined with a microscope (re- lyzed by conventional FTIR techniques (Hommerich, 2016). Micro-
flectance mode) was used to identify the occurrence and extent of MPs FTIR collects IR signals at high spatial resolution (the beam size can be
with high spatial resolutions (Fig. 16). For instance, various types of MPs as small as 5 μm), and has great potential for the characterization of
(e.g., PP, PE, polyester and PTFE) in the Ross Sea water was imaged by compositionally complex samples (Harrison et al., 2012). Zhang et al.
FTIR, which identified the presence of PE and PP (Cincinelli et al., used μ-FTIR to test the polymer types of microplastic and identified
2017). For the environmental samples with limited amounts of MPs, eight kinds of polymers, including rayon, PE, PP, PA, PET, PS, poly
the analyses typically start with a filtration step for concentration and (methyl methacrylate) (PMMA) and polyurethane (PU) (Zhang et al.,
proceed directly on the dried filter (Cincinelli et al., 2017). Alternatively, 2019a).
increasing the acquisition time or the collection runs can also increase Löder et al. presented the first study to employ a focal plane array
the signal to noise ratio. Meanwhile, FTIR relies on surface contact anal- detector-based micro-Fourier-transform infrared imaging to analyze
ysis, which may compromise the sample integrity for fragile small-size microplastics from environmental samples in 2015 (Löder et al.,
MPs. For instance, MPs fragments may be attached to the probe tip in 2015). This study successfully measured the surface (N10-mm diame-
ATR mode due to sample-tip adhesion or electrostatic interaction ter) of membrane filters with microplastics from marine plankton and
(Shim et al., 2017). sediment samples. Plastic particles with a size of 20 μm were rapidly de-
In recent years, the combination of IR spectroscopy with an IR micro- tected with a high lateral resolution. Furthermore, Mintenig et al. first
scope has emerged as micro-FTIR (μ-FTIR) for the characterization of applied micro-FTIR imaging to detect microplastics in large volumes of
sample with sizes down to 10 μm (Löder and Gerdts, 2015). Micro- organic-rich treated wastewater. This research combined ATR-FTIR
FTIR has widely been applied in microplastic researches (see Table 9) with micro-FTIR to characterize the microplastics down to a size of
(Corami et al., 2020; Löder et al., 2015; Mintenig et al., 2017; Tagg 20 μm, which found that wastewater treatment plants (WWTPs)
et al., 2015; Zhang et al., 2019a). MPs in freshwater bodies (Luo et al., could not only be a sink but also a source of MPs (Mintenig et al., 2017).
(a) (b)
100μm 100μm
(c)
Fig. 16. Typical data obtained from FTIR microscope: (a) the visible light map showing a MPs fragment on a filter; (b) the corresponding IR mapping image at 3291 cm−1 (N\ \H stretch).
The intensity of the band increases as follows: blue b green b yellow b red; (c) the FTIR spectra of the MPs. The figure is adapted from (Cincinelli et al., 2017) with permission.
Table 9
Applications of micro-FTIR in MPs characterization.
China/surface Rayon, PE, PP, 34.97–4983.73 μm 499.76 items kg−1 μ-FTIR was applied to identify eight polymer types of MPs from (Zhang et al., 2019a)
sediments PA, PET, PS, sediment samples in Sishili Bay, North Yellow Sea. These results
PMMA and PU indicate that the MPs pollution was mainly sourced river and
sewage discharge and maritime activities.
−1
China/sewage PET, PS, PP 681.46 0.59–12 items L μ-FT-IR was used to analyze the MPs in municipal sewage from (Yang et al., 2019)
± 528.73 μm China's largest water reclamation plant. The results found that the
treatment technologies employed at the chosen sewage treatment
plant are efficient to remove the majority of MPs.
Challenger PET, PP, PS, 73–491 μm b71.1 items kg−1 μ-FTIR was used to identify the polymer type of MPs from the (Peng et al., 2020)
deep/sediments Nylon sediment sediments of the Challenger Deep located in Pacific Ocean. This
study proposed that most MPs that are disposed in the ocean will
sink into the hadal trenches eventually.
−3
China/atmosphere PET, PE, PES, 23.07–9555 μm 0–4.18 items m μ-FT-IR was used to confirm the presence of airborne MPs in the air. (Liu et al., 2019)
PAN, PAA, RY, This study estimated that the total annual weight of suspended
EVA, EP, ALK atmospheric MPs in Shanghai is 120.72 kg and each adult might
inhale 21 MPs every day.
China/surface PE, PP, PS, PVC 0.1–1 mm 3.5–25.5 items L−1, This study analyzed the spatial-temporal distribution of MPs surface (Wu et al., 2019)
water and water; 25–560 item water and sediment of the Maozhou River by μ-FTIR. The results
−1
sediments kg sediments showed wide distribution and high abundance of MPs in
Guangdong-Hong Kong-Macao Greater Bay Area.
−1
China/freshwater PES, rayon, PP, 20 to 5000 μm 0.9–2.4 items L The polymer types of MPs in different water bodies from urban (Luo et al., 2019)
bodies PA, nylon creeks to coastal waters were analyzed with μ-FTIR spectroscopy.
This study suggested that MPs pollution in small freshwater bodies
was more serious than in estuarine and coastal waters.
China/organisms PE, PS, 1.0–5.0 mm 0.85–1.02 items per μ-FTIR was used in this study to verify the random pick-up of MPs by (Li et al., 2019)
Polyamide mussel the organisms in aquatic environments. The results suggest that
MPs can contact and fuse with the byssus of mussels during their
formation.
Australia/shrimp PS, rayon 0.190–4.214 mm 0.40 ± 0.27 items The occurrence and types in the shrimp P. australiensis from fresh (Nan et al., 2020)
L−1 waterbodies in eastern Australia are identified using μ-FTIR. This
study suggested that P. australiensis might be a good bioindicator to
assess MPs pollution in freshwater environment.
China/fishes PE, PP, PES 20–500 μm 0.3–5.3 items per fish This study identified the MPs found in gills and guts of fish samples (Su et al., 2019a)
from coast and estuary area of east China by μ-FTIR spectroscopy.
5.2. Raman spectroscopy applications of micro-Raman to identify MPs in seawater, freshwater,

wastewater, sediment, aquatic organisms, food, drink and cosmetics.
Raman spectroscopy is another popular chemical identification Different from FTIR, significant advantages for Raman is that sample
mapping technique that utilizes the frequency shift of inelastic scattered thickness or the presence of liquid or water/moisture will not negatively
light from the sample based on Raman effect to obtain the vibrational affect the measurement. For example, the substance (fluorescence or
modes and identify chemical species of samples (Ribeiro-Claro et al., piglet) may affect the scattering of incident light and interfere the detec-
2017). An input of energy into the molecule will cause the molecule to tion. Thus, sample purification is often essential for Raman spectroscopy
vibrate and each vibrational mode initiated by a specific frequency analysis to eliminate potential interferences and increase the sign/noise
and the Raman spectrum was formed as a result of a molecular vibration ratio. Moreover, some fluorescence interferences can be overcome by
in the samples (Smith and Dent, 2019). Raman spectroscopy has been applying baseline removal algorithms and using more efficient detec-
proven to be a highly reliable technique for identification of MPs in dif- tors (Araujo et al., 2018). Some samples may have laser-induced degra-
ferent environmental samples (Löder and Gerdts, 2015). For instance, dation and the laser power beyond certain threshold levels may damage
by comparing with massive spectral database, copper phthalocyanine to samples that may not be thermally stable or susceptible to thermal
pigmented MPs are confirmed by the Raman spectra (Fig. 17) (Van degradation.
Cauwenberghe et al., 2013). Zhao et al. used an excitation laser at
785 nm (near-infrared) in the Raman microscope system to identify 5.3. Other identification methods
the polymer additives on Raman-transparent calcium fluoride windows
and proved the dual density separation was useful for separating MPs 5.3.1. Gas chromatography–mass spectrometry (GC–MS)
from marine snow samples (Zhao et al., 2017b). GC–MS couples GC separation with MS to identify and quantify vol-
Though able to characterize MPs, Raman spectroscopy usually de- atile organic species (Sparkman et al., 2011). Fig. 18 demonstrates a
tects MPs greater than about 10 μm, whereas micro-Raman spectros- schematic diagram of a GC/MS instrument. GC utilizes a capillary col-
copy is capable of detecting MPs with higher resolution of up to 1 μm umn, in which the stationary column medium materials have different
(Imhof et al., 2016; Käppler et al., 2016). Schymanski et al. and Oßmann relative affinity toward the analyte molecules and result in differenti-
et al. successfully applied micro-Raman spectroscopy to detect and an- ated travel times. The travel retardation allows mass spectrometer to
alyze small MPs (down to 1 μm) in the bottled water and indicated analyze the eluting molecules for chemical species. Mass spectrometer
the release of MPs from the packaging materials (Oßmann et al., 2018; ionizes analyte molecules and detects these charged fragments at differ-
Schymanski et al., 2018). Meanwhile, the previous studies using μ- ent mass-to-charge ratios (Karasek and Clement, 2012). GC–MS has
FTIR spectroscopy failed to detect MPs smaller than 20 μm in drinking been widely used in detection and analysis of drugs, explosives, addi-
waters and wastewater treatment plants due to the low resolution of tives and environmental pollutants (Hübschmann, 2000).
μ-FTIR (Mintenig et al., 2017; Mintenig et al., 2014). The number of pub- In microplastics research, GC–MS is usually applied to measure the
lications in the applications of micro-Raman for MPs characterization is dissolved or extracted polymer components of MPs, the adsorbed or-
steeply increasing as summarized in Table 10, which shows the ganic matters such as persistent organic pollutants (POPs) as well as
Fig. 17. Identification of MPs extracted from sediment with Raman spectroscopy: (a) the visible light image of MPs; (b) Raman spectrum of MPs; and (c) the reference spectrum matching
the sample spectrum.
This figure is adopted from (Van Cauwenberghe et al., 2013) with permission.
organic plastic additives (OPAs) that may release from MPs. Moreover, information (Halket and Zaikin, 2006). In this way, compared with
GC–MS was also utilized to analyze the specific degradation products GC–MS, Py-GC/MS is able to analyze higher molecular weight com-
of MPs such as PP, PE and PS (Dümichen et al., 2017). Table 11 shows pounds and provide a more complete overview of the whole sample
the application of GC–MS in the characterization of microplastics in and a more accurate evaluation for the real, complex chemical nature
river water, seawater, beaches, soil and sediments. For example, Men- of the sample (Tianniam et al., 2010). Fischer et al. utilized Pyr-GC/MS
doza et al. utilized GC–MS to measure the concentrations of for successful characterization of MPs in fish samples, proving that
polychlorinated biphenyls (PCBs) compounds associated with Pyr-GC/MS offers a sensitive polymer identification and mass-related
microplastics collected from seawater, which indicated that the concen- quantification method (Fischer and Scholz-Böttcher, 2017).
trations of PCBs on microplastics were 1 to 223 ng per gram of plastics Similarly, TD-Pyr-GC/MS couples the thermal desorption (TD) de-
and the main polymer components in these collected microplastics vice to Pyr-GC/MS for the qualitative and quantitative analysis of the
were PP and PE (Mendoza and Jones, 2015). sample's complex components. The TD device collects and concentrates
Moreover, GC–MS coupled with other techniques such as sequential the volatile organic compounds into a small volume fundamentally
pyrolysis (Pyr-GC/MS) (Fischer and Scholz-Böttcher, 2017; Fries et al., through the adsorption with sorbents and further release into a gas
2013; Nuelle et al., 2014) and thermal desorption pyrolysis (TD-Pyr- flow by heating the sorbents (Woolfenden and Poole, 2012). The TD de-
GC/MS) (Dehaut et al., 2016) were also explored in MPs characteriza- vice is installed on the top of GC injector and operated by direct heating.
tions. Pyrolysis is a process in which the sample is heated and The injected samples pass through the TD device and generate pyro-
decomposed to small molecules that are further separated by GC and lyzed fragments into Pyr-GC/MS for analysis (Hu et al., 2014). Compared
detected using MS (Peacock and McEwen, 2006). The sample is put with solvent extraction in general GC–MS, TD-Pyr-GC/MS is more ad-
into contact with pyrolyzers and rapidly heated to 600–1000 °C in an vantageous because it is operated without undesired organic solvent
isothermal furnace. This process breaks down the large molecules at and the contamination of sample from impurities in solvents is avoided
the weakest bonds to produce smaller and more volatile pieces, which (Hu et al., 2014). Thus, various organic plastic additives (e.g., benzophe-
are further separated by GC to acquire a chromatogram and analyzed none and 1,2-benzenedicarboxylic acid) have been determined by TD-
by MS to identify individual fragments and obtain structural Pyr-GC/MS (Dümichen et al., 2015).
Table 10
Applications of micro-Raman in MPs characterization.
Place/origins MPs MPs size Abundance Major objective/findings Refs.

type
Germany/bottled PET, PP 1–500 μm 0–253 items L−1 This study analyzed 38 mineral water samples by micro-Raman (Schymanski et al.,
water spectroscopy and MPs were found in every type of water, with 2018)
almost 80% sized between 5 and 20 μm. The findings indicate that
plastic packaging emit MPs that might be ingested directly by
consumers.
Northwestern PE, PP b5 mm 1.0 × 104 items km−2 This study did the field observation of MPs pollution in the (Pan et al., 2019)
Pacific Ocean and Northwestern Pacific Ocean with the μ-Raman spectroscopic
nylon analysis. The results indicate that the major compositions of MPs
are PE, PP and nylon.
China/urban PP b2 mm 2425–7050 items m−3 This study investigated eight urban lakes in Changsha, China and (Yin et al., 2019)
lakes found polypropylene was the dominant type in the studied
waters. The results can provide a valuable reference for a better
understanding of microplastic pollution in urban areas of China.
China/Poyang PP, PE, b0.5 mm 5–34 items L−1 (surface waters); This study found that PP, PE and PVC were the major polymer (Yuan et al., 2019)
Lake PVC, 54–506 items kg−1 (sediments); types of MPs detected in water, sediment and biota of the Poyang
nylon 0–18 items per crucian Lake, indicating that domestic sewage and fishing activities might
be the main sources of microplastics in the lake.
Malaysia/fish PE, PP, 180–7800 μm 3.6 items g−1 fish meal Chemical composition of MPs in three Malaysian commercial (Karbalaei et al., 2020)
meals PET, brands of fish meal was investigated using micro-Raman spec-
nylon troscopy. This study demonstrates high levels of MPs exposure to
customers via MP contaminated fish/shellfish in fish meal
products.
Mexico/milk PES b0.5 mm 3–11 items L−1 The Micro-Raman identification results in this study revealed that (Kutralam-Muniasamy
and polyethersulfone and polysulfone were common types of et al., 2020)
PSU microplastics in milk samples, which are highly used membrane
materials in dairy processes. This study finding developed a
baseline outlook for microplastics contamination in dairy
products.
India/Vembanad PS, b5 mm 252.8 items m−3 Identification of the polymer components of MPs was done using (Sruthy and
Lake LDPE, micro Raman spectroscopy. This study, being the first report from Ramasamy, 2017)
HDPE, India on MPs in lake sediments, found the extensive distribution
PP of MPs in aquatic systems spread across India.
Eastern PS, PP b5 mm 6.7 MPs m−3 surface water; 4.68 This study is the first that investigated microplastics pollutions in (Kazour et al., 2019)
Mediterranean and PE MPs g−1 sediments; 2.9–8.3 MPs the three matrices (water, sediments and biota) in the Eastern
basin per oyster Mediterranean by micro-Raman. The results indicate the
potential MPs sources from coastal landfills.
5.3.2. Matrix-assisted laser desorption/ionization time-of-flight mass and applied to the sample wells in a target plate as Fig. 19 shows. Sec-
spectrometry (MALDI-TOF-MS) ond, the sample matrix is irradiated with a pulsed laser, causing the
MALDI-TOF MS is a MS technique in which samples are ionized into sample and matrix molecules desorbed from the target plate. Finally,
charged molecules by MALDI ion source and ratio of their mass-to- the analyte molecules are ionized by being protonated in the hot
charge (m/z) is measured by TOF mass analyzer (Fig. 19). MALDI is an plume of ablated gases, and then analyzed by the MS (Karas and
ionization technique that uses three steps to ionize the sample into Krüger, 2003). Meanwhile, TOF MS determines the ions' m/z ratio via ac-
small fragments with the laser energy (Hillenkamp et al., 1991). First, celerating ions in an electric field of known strength and length. The
the sample is mixed with a suitable matrix material consists of crystal- time taken for ions to flight through a fixed distance depends on the ve-
lized molecules (e.g., sinapinic acid and 2,5-dihydroxybenzoic acid) locity of the ions, and further is used to calculate the m/z ratio and
MS
GC
Fig. 18. Schematic diagram of a gas chromatography quadrupole mass spectrometer (GC/MS).
The figure is adapted from (Fischer and Scholz-Böttcher, 2017; Kim et al., 2017) with permission.
Table 11
Applications of GC–MS in MPs characterization.
Germany/fish PE, PP, PS, PVC, b1 mm b20 μg/fish Pyr-GC/MS was used to identify and quantify eight common types of MPs in fish (Fischer and
samples PA6, PMMA, PET, sample samples at a trace level. Scholz-Böttcher,
and PC 2017)
USA/seawater PP and PE 5 mm 0.025 g mL−1 Pyr-GC/MS quantified the concentrations of PCBs released from MPs and identified (Mendoza and
the main polymer materials of these collected MPs were PP and PE. Jones, 2015)
−3
Germany/sediment PE 0.2 mm 1.15 g cm The components of the MPs as well as their carried organic pollutants from the (Fries et al.,
sediment samples were identified with GC/MS. 2013)
France/simulated CA, HDPE & LDPE, 1–5 mm 1.37 g cm−3 The identification of MPs in biological samples was achieved with GC/MS after an (Dehaut et al.,
water PA, PC, PET and PS digestion of biological tissues using a KOH 10% solution with no significant 2016)
degradation on MPs.
Germany/soil PE 1 mm 0.03 mg μL−1 This study developed a method enabling the identification and quantification of MPs (Dümichen
in unknown solid environmental sample by combining TD-GC/MS with et al., 2015)
thermogravimetric analysis (TGA).
Germany/rivers PE, PP, PS, PA6 and 630 μm 0.013 mg μL−1 TD-GC/MS was used in this study for fast identification and quantification of MPs in (Dümichen
PET real environmental samples from three rivers and bio gas plant, and found PE and PS et al., 2017)
were the main MPs.
Portugal/beaches PS, PP and PE 0.5–1 mm 0.05 g mL−1 The MPs collected from Fonte da Telha beach are mainly consisted of PE and PP. The (Frias et al.,
concentrations and species of POPs in the MPs are also identified with GC/MS. 2010)
Germany/marine PE, PP, PVC, PET, 1 mm 4–6 particles This study used Pyr-GC/MS to analyze MPs samples in marine sediments from the (Nuelle et al.,
sediments PS and PUR mL−1 North Sea island Norderney and found the types of MPs are PP, PVC and PET. 2014)
identify the ion (Boesl, 2017). For example, the lighter ions of the same of polytrimethylene terephthalate (PTT) in the temperature range of
charge present lower velocity than the heavier ions. In a word, the 250–360 °C under non-oxidative conditions and detected the degradation
MALDI ionize the sample into small fragments and TOF mass analyzer products (Jang et al., 2012). In addition, MALDI-TOF MS coupled with im-
further identify the ions with measured m/z ratios (Clark et al., 2013). aging techniques (MALDI MSI) can provide morphological information
MALDI-TOF MS has been applied to the analysis of polymers (Dimzon such as size and shape of particles, but also the chemical structure
and Knepper, 2012), proteins (Caprioli et al., 1997), peptides (Kondo changes of polymers during degradation under aerobic and denitrifying
et al., 2006), dendrimers (Peterson et al., 2003) and sugars (Ren et al., conditions (Rivas et al., 2016). Therefore, the potential to detect different
2005). The analysis of polymers with MALDI-TOF MS usually provides polymer materials with a high degree of selectivity makes MALDI-TOF MS
the molecular weight distribution and copolymer compositions as well a promising technique for MPs such as the analysis of compositions, and
as the polymerization mechanism (e.g., molecular structures and end direct detection of additives or adsorbed pollutants on MPs surface
groups) (Rizzarelli and Carroccio, 2014). Sreerama et al. utilized MALDI- (Huppertsberg and Knepper, 2018).
TOF MS to analyze the oligomeric impurities formed during click cycliza- Microplastics were also studied by another thermal technique, differ-
tion of PS polymer, which demonstrates that MALDI-TOF MS is a critical ential scanning calorimetry (DSC), which identify chemical species
tool for the characterization of complex polymer (Sreerama et al., 2014). through monitoring the melting temperatures of plastic samples during
Jang et al. utilized MALDI-TOF MS to characterize thermal degradation heating at a temperature range (Rodríguez Chialanza et al., 2018). A
Fig. 19. The schematic principle of MALDI-TOF mass spectrometer.

The figure is adapted from (Patel, 2015) with permission.
drawback of DSC technique is the dependence of particle size on DSC sig- focuses on their respective principles, advantages and limitations.
nal, which requires a proper sample pretreatment method (i.e., separating The key learning points of this literature review are: (1) optical mi-
particles by their size by multiple sieving). Besides, sensitive DSC sensors croscopes, although simple to operate for routine analysis of sam-
are needed when the mixtures of polymers have close melting points or ples, are unable to accurately differentiate synthetic microplastics
some polymers have low thermal conductivity. Thus, these weak points from plastic-like particles like natural minerals. (2) Raman spectros-
of DSC limited its applications in MPs characterization. copy could identify microplastics in both solid and liquid samples (as
opposed to FTIR). However, Raman analysis could be affected by the
5.3.3. High-performance liquid chromatography (HPLC) presence of color, fluorescence, additives and contaminants
HPLC is a common analytical instrument used to separate, identify, adsorbed on or imbedded within microplastics. (3) FTIR is a comple-
and quantify organic compounds in liquid (Shui and Leong, 2002). For in- mentary technique for Raman spectroscopy that also generates
stance, HPLC has been applied into pharmaceutical development to ob- chemical information and mapping. However, FTIR requires dry sam-
tain and ensure product purity in the manufacturing field (Siddiqui ples that must be prepared as thin films or ground to powders prior
et al., 2017), as well as the detection of illicit drugs in urine, such as doping to the FTIR analysis. Besides, the prerequisite for acquiring the IR ab-
agents (Deventer et al., 2009). As shown in Fig. 20, the sample is injected sorption is the change of the dipole moment of chemical bonds. Thus,
into the solvent (as mobile phase) and pumped into a column that con- FTIR is mostly used to analyze polymers with the polar functional
tains a packing of small porous particles (stationary phase) (Engelhardt, groups such as carbonyl groups. The Raman spectroscopy relies on
2012). The different solubility and polarity of the sample components in laser scattering detection and detects the polarizability of chemical
the mobile and stationary phases cause different flow rates for each com- bonds. Therefore, Raman analysis is mainly used to analyze materials
ponents as they are flushed out of the column, and thus separating these or chemicals with aromatic bonds (e.g., double carbon bonds);
components. Then, the concentration of each component can be calcu- (4) Mass spectrometry-based methodologies are reported to detect
lated by comparing the measurement record of liquid absorbance at dif- the components in polymers and very recently from microplastics
ferent retention times with the standard calibration curve. as well. Mass spectrometry requires polymer specimen to be rela-
Similar to GC, HPLC has been used widely to measure the absorbed tively purified and concentrated, followed by vaporization before en-
or released organic matters and degradation products from MPs. Li tering the mass spectrometry analysis. Therefore, mass spectrometry
et al. used HPLC technique to detect the absorbed antibiotics composi- has not become a routine or popular analysis for microplastics re-
tions and adsorption amounts on PS, PE, PP, and PVC MPs (Li et al., search due to the labor intensive extraction and purification (e.g., liq-
2018b). Ma et al. used HPLC to measure the accumulation of 14C- uid/liquid or solid phase extraction). Moreover, the vaporization
phenanthrene on MPs (50 nm–10 mm) and found that 50-nm NPs step, for instance, under laser ablation, may alter or destruct plastic
with surface adsorption of phenanthrene had increased toxicity toward sample characteristics. (5) NTA, FCM and HSI show promising
D. magna (Ma et al., 2016). Wang et al. used HPLC to quantify the power for the in situ imaging and particle counting in liquid. Accu-
amounts of depolymerized building block compounds, i.e., bisphenol A rate identification and quantification of microplastics using these
(BPA) and para-phthalic acid (PTA) from polycarbonate (PC) and PET techniques requires further improvements in reducing potential in-
microplastics, respectively (Wang et al., 2017). Bagheri et al. analyzed terferences from chemical coating, modifiers and contaminants
the degradation processes of PET MPs in simulated seawater and fresh- that surround microplastics or co-exit inside microplastics.
water through the detection of lactic acid monomer formed from the As a unique scanning probe technique, AFM and its combinations
degradation of PET microplastics (Bagheri et al., 2017). Compared with IR and Raman open up new opportunities in microplastics and
with MS, which is usually applied as an ending detection method be- nanoplastics characterization. AFM has broad applications in detection
cause of its high sensitivity, HPLC is more commonly used to identify and quantification of various material properties such as mechanical
large, polar, thermally unstable and nonvolatile compounds that could elasticity, surface electric and chemical properties (e.g., hydrophobic-
be derived from or associated with microplastics. ity). More importantly, AFM requires relatively simple sample prepara-
tion and detect plastics or polymers based on different detection
6. Conclusions and future perspectives mechanisms such as localized thermal expansion in AFM/IR or tip-
enhanced Raman effects in AFM/Raman. Finally, AFM performs analysis
6.1. Strength and limitations of current microplastics characterization in both liquid and air (or vacuum), which conserves the original sample
methods conditions during the AFM analysis. However, as a common limitation
of all scanning probe microscope, AFM requires relatively flattened
This review summarizes current separation, characterization and and smooth surfaces of the samples to obtain high-quality imaging or
identification methods available for microplastic research with the mapping.
Fig. 20. Schematic diagram of a HPLC system.

This figure is adopted from (Czaplicki, 2013) with permission.
6.2. Demand for standardized experimental procedures and characteriza- CRediT authorship contribution statement
tion analysis
Wanyi Fu: Writing - original draft, Writing - review & editing.
Due to the complex nature of plastic particles, MPs are potential ab- Jiacheng Min: Resources, Writing - review & editing. Weiyu Jiang:
sorbents and carriers for environmental pollutants such as heavy Resources, Writing - review & editing. Yang Li: Supervision, Writing -
metals, pathogens, and organic substances. Moreover, MPs may experi- review & editing. Wen Zhang: Supervision, Writing - review & editing.
ence photochemical, mechanical or biological degradation that leads to
the production of nanoplastics, release of internal additives or
Declaration of competing interest
byproducts such as co-polymers or monomers. These naturally occur-
ring processes clearly make MPs undergo extremely complex transfor-
The authors have no competing interests to declare.
mation and increase the difficulties of characterization. For instance,
surface adsorbed chemicals may increase artifacts and interfere the
Acknowledgement
result interpretation. Besides, without proper treatment such as pu-
rification, detection of microplastics can be interfered by natural
This study was supported by the New Jersey Water Resources Re-
polymers (e.g., cellulose, chitin, and chitosan) in the environment.
search Institute (NJWRRI) Grant (Project Number: 2018NJ399B), and
Therefore, it is urgent to establish consistent, reliable, and standard-
the National Natural Science Foundation of China (Grant Number:
ized protocols for separation, purification and detection of MPs or
21677015).
nanoplastics. Plastic extraction, enumeration and identification
sometimes differ or conflicts among different studies due to the in-
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Science of the Total Environment 721 (2020) 137561

Contents lists available at ScienceDirect

Science of the Total Environment

journal homepage: www.elsevier.com/locate/scitotenv

Separation, characterization and identiﬁcation of microplastics and

• Separation, characterization and identiﬁ-

Fig. 1. Simpliﬁed scheme of an FFF channel operating in different separation ﬁeld.

3.1. Examinations with optical microscopes

Visualization is important for identifying microplastics in sample

Place/origins MPs type MPs size Abundance Major objective/ﬁndings Refs.

Place/origins MPs type MPs Abundance Major objective/ﬁndings Refs.

Place/origins MPs type MPs size Abundance Major objective/ﬁndings Refs.

reported in the studies that involved multiple kinds or sizes of particles

4.2. Nanoparticle tracking analysis (NTA)

NTA was developed and ﬁrst commercialized by NanoSight Ltd. in

Place/origins MPs type MPs size Abundance Major objective/ﬁndings Refs.

Fig. 6. PET MPs ﬁbers as imaged by the FCM.

Fig. 10. Schematic diagram of a ﬂuorescence spectrophotometer.

Place/Origins Material Size of MPs Concentrations Applications Refs.

Fig. 11. Three common conﬁgurations in HSI devices.

Techniques Analytic capabilities Advantages Disadvantages

Modes Advantages Applicable samples Applicable forms of MPs

Place/origins MPs type MPs size Abundance Major objective/ﬁndings Refs.

5.2. Raman spectroscopy applications of micro-Raman to identify MPs in seawater, freshwater,

Place/origins MPs MPs size Abundance Major objective/ﬁndings Refs.

Place/origins MPs type MPs size Abundance Major objective/ﬁndings Refs.

Fig. 19. The schematic principle of MALDI-TOF mass spectrometer.

Fig. 20. Schematic diagram of a HPLC system.

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