Water Air Soil Pollut (2024) 235:189
https://doi.org/10.1007/s11270-024-06964-2
Microplastics in Soils and Sediments: a Review
of Characterization, Quantitation, and Ecological Risk
Assessment
Archana Prajapati · Ashish Dehal ·
Asirvatham Ramesh Kumar
Received: 4 September 2023 / Accepted: 30 January 2024
© The Author(s), under exclusive licence to Springer Nature Switzerland AG 2024
Abstract This study presents a comprehensive
review of the characterization, quantification, and
ecological risk assessment of microplastics (MPs) in
soils and sediments. MPs, defined as plastic particles
of size smaller than 5 mm, have been less studied in
these environments compared to aquatic ecosystems.
Broadly, all analytical methods include the follow-
ing steps: sampling, extraction, polymer identifica-
tion, and quantitation/particle counting. This review
highlights the variation in current methodologies
for sampling, extraction, and quantification of MPs,
which hinders data comparison across studies. This
poses a real challenge to compare the data of vari-
ous studies. Hence, there is an urgency to develop
standardized methodologies for analyzing MPs in
different environmental matrices. Spectroscopic tech-
niques such as FT-IR and Raman are the most widely
used techniques for polymer identification. Adopting
proper quality control and quality assurance measures
A. Prajapati · A. Dehal · A. R. Kumar (*)
Chemical and Hazardous Waste Management Division,
CSIR-National Environmental Engineering Research
Institute, Nagpur 440020, India
e-mail: ar_kumar@neeri.res.in
A. Prajapati
Rashtrasant Tukadoji Maharaj Nagpur University,
Nagpur 440033, India
A. Dehal · A. R. Kumar
Academy of Scientific and Innovative Research (AcSIR),
Ghaziabad 201002, India
will improve the reproducibility and comparability of
results. This review calls for further research on MPs’
effects on soil and sediment environments to inform
standardization efforts and improve our understand-
ing of MPs pollution.
Keywords Extraction · FT-IR · Microplastics ·
Raman spectroscopy · Sediment · Soil
1 Introduction
Since the commercialization of plastics in the 1950s,
global plastic production has only grown exponentially,
and over the years, plastics have become an inevitable
material for humans. It is estimated that, in 2022, 21
million tonnes (Mt) of macroplastics (plastics larger
than 5 mm) leaked into the environment globally
which is about one-third more than that leaked into the
environment a decade earlier. In addition, plastics gen-
erate a variety of lifecycle impacts including 3.8% of
contribution to total global greenhouse gas emissions
(1.9 ­GtCO2 e in 2022) (OECD, 2023). Apart from
being cheap, plastic became widely popular due to its
properties such as durability, corrosion resistance, low
thermal conductivity, and lightweight (Andrady, 2011;
Andrady and Neal, 2009; Imhof et al., 2012). A sig-
nificant quantity of processed and manufactured plastic
is meant for single use. In most developing countries,
these single-use plastics (SUPs) are disposed off with-
out proper segregation and treatment, making SUPs
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 189 Page 2 of 42
the major contributor to the municipal solid waste.
The natural degradation of plastic is very slow, and it
takes decades to completely decompose plastic mate-
rial in the environment (Hidalgo-Ruz et al., 2012).
Consequently, discarded plastics get collected in the
environment over time and transported to other regions
through air, water, and wind, eventually ending up in
the seas (Thompson et al., 2004). Thus, plastic is omni-
present, regardless of how heavily inhabited or isolated
a location is (Möller et al., 2020).
The first report to establish the evidence on marine
plastic pollution dates back to the 1970s (Carpen-
ter and Smith, 1972). Since then, more and more
studies have documented the widespread plastic
contamination in different environmental matrices
(Campanale et al., 2022). The most used polymers for
plastic manufacturing and packaging are polyethylene
(PE), polypropylene (PP), polystyrene (PS), poly-
ethylene terephthalate (PET), and polyvinylchloride
(PVC) (Thompson et al., 2004). Table 1 lists the most
commonly used polymers, their properties, applica-
tions, and hazard statement.
Due to biotic and abiotic processes, discarded
plastics disintegrate into diverse shapes and sizes
ranging from meters to micrometers (Barnes et al.,
2009), which can vary from > 20 mm for macroplas-
tics, 20–5 mm for mesoplastics, < 5 mm for MPs,
and < 1 µm for nanoplastics. Microplastics (MPs)
are plastic particles of size < 5 mm. MPs are classi-
fied into (1) primary MPs, which are produced for
that size as beads or pellets. They are used in per-
sonal care products, sand blasting (as abrasives), and
domestic cleaning agents. (2) Secondary MPs are
formed from the disintegration of discarded plastics
(De Souza Machado et al., 2018). The disintegra-
tion is induced by biological, physical, or chemical
factors (Andrady, 2011). Figure 1 depicts the lifecy-
cle of plastics and MPs in soil and sediments. MPs
are observed in numerous shapes, for example, bead,
pellet, foam, film, fragments, and fiber/filament. The
term MP was first introduced by Richard Thompson
in 2004 to refer to the microscopic plastic particles
of size 20–2000 μm found in British beach water col-
umns and sediments (Thompson et al., 2004). Later,
the MPs size range was extended to include plastic
particles of size up to 5 mm, such as pellets (Arthur
et al., 2009).
Professional bodies, such as the Joint Group
of Experts on Scientific Aspects of Marine
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Water Air Soil Pollut (2024) 235:189
Environmental Protection (GESAMP), considered
the nano-sized particles (1 mm to 1 µm) to be MPs
(Möller et al., 2020). There is no universally accepted
and unequivocally defined size range for MPs. The
dispersion and bioavailability of MPs in the environ-
ment depend on their shape, size, density, color, and
chemical makeup. Since most plastic debris makes its
way from land to water bodies and eventually to sea,
the accumulated plastics in the ocean cause death of
many aquatic organisms that mistake MPs for food.
The initial research on MPs in aquatic or marine
environments aimed to understand MP’s occurrence,
abundance, fate, and impact on aquatic/marine organ-
isms. Because contamination control must happen at
the source, studies on MPs got expanded to terrestrial
ecosystems (Campanale et al., 2022). This is evident
from Fig. 2, which indicates that the number of arti-
cles on MPs in soil and sediments increased from the
year 2015 onwards (Web of Science database). Plastic
garbage generated on land is primarily disposed of in
soil or aquatic ecosystems. In the terrestrial ecosys-
tem, littering, surface runoff, application of biosolids,
compost on agricultural soil, and farming methods
utilizing plastics, such as mulching, expose urban and
agricultural soil to MPs contamination (De Souza
Machado et al., 2018; Li et al., 2018; Liu et al., 2018).
Due to biofouling and weathering, the density of
MPs fluctuates over time and eventually, soil and
sediments become the sink for MPs (Bläsing &
Amelung, 2018; Cunningham et al., 2020; Katare
et al., 2022). Higher-density MPs sink and accumulate
in sediments, while beach sand can amass floating,
partly buoyant, and sink plastics. MPs can also sorb
and transport heavy metals, organic contaminants, and
pathogens, making them a cocktail of contaminants
(Bayo et al., 2018; Bhagat et al., 2022). The presence
of MPs can alter the chemical and physical properties
of soil and sediments, ensuing disturbances in the
food chain. Due to biomagnification, MPs ascend
along different trophic levels, causing organisms of
all the trophic levels exposed to MPs, raising food
safety concerns (Rainieri & Barranco, 2019). Soil and
sediments are non-homogenous, hence pose challenges
to MPs analysis. So far, no standard analytical method
is available to study MPs in soil or sediments. Thus,
the reported data on MPs in various matrices are
associated with different levels of inaccuracies
(Hidalgo-Ruz et al., 2012; Zhang & Liu, 2018).
 Table 1  List of commonly used polymers with their properties, applications, and hazard statement
Sl. no Polymer type
1 High-density polyethylene 0.94–0.97
2 Low-density polyethylene 0.91–0.93
3 Polyvinyl chloride
4 Polypropylene
5 Polyethylene terephthalate 1.34–1.39
6 Polystyrene
7 Polycarbonate
8 Polyurethane
9 Polyamide
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Density (g/cm3) Crystallinity Polarity Uses Hazard statement
Water Air Soil Pollut
70–95% Non-polar Plastic bottles, toys, chemical containers, Extremely flammable gas
pipes May cause drowsiness or dizziness
45–60% Non-polar Milk cartons, utensils, plastic bags, wire Extremely flammable gas
insulation May cause drowsiness or dizziness
1.38 High Polar Pipe insulation, blood collection bags, win- Carbon dioxide, carbon monoxide, hydrogen
dow frame, packaging chloride, and other toxic fumes generated
Causes eyes irritation
(2024) 235:189
0.85–0.94 50–80% Non-polar Packaging material, medical devices, toys, Extremely flammable gas
carpets, electrical insulation, automotive Dust can cause mechanical irritation of the
eyes, skin, nose, and throat
High (30–40%) Highly polar Bottles of carbonated drinks, Thermal Harmful if swallowed
insulation, seat belt, automobile tire yarns, Causes eye, skin, and respiratory tract irrita-
disposable medical garment, cookware tion
0.96–1.05 Low Non-polar Foam thermocol, packaging material, auto- May be fatal if swallowed and enters airways
motive parts, electronics, insulator, food Causes skin, eye, and respiratory tract irrita-
packaging tion
Causes damage to organs (hearing organs)
through prolonged exposure
Harmful to aquatic life with long lasting
effects
1.20 Low Highly polar Fencing, barriers, storefront windows, bullet Fumes produced during melt processing may
resistant material, safety glasses cause eye, skin, and respiratory tract irrita-
tion
1.20–1.26 - Highly polar Tires, refrigerator insulation, footwear, bed- Harmful when in contact with skin
ding foam, thermal insulation Causes serious eye irritation
Harmful if inhaled
Suspected of causing cancer
May cause damage to organs through pro-
longed or repeated exposure
1.12–1.14 35–45% Highly polar Textiles, ropes, gears, raincoats, cellophane, Harmful in contact with skin
windshield wipers Harmful if swallowed
May cause respiratory irritation
Causes severe skin burns and eye damage
Page 3 of 42
189
 189 Page 4 of 42 Water Air Soil Pollut (2024) 235:189

Fig. 1  Lifecycle of plastics and microplastics in soil and sediments

Fig. 2  a Number of 750

published papers on 700 Soils 687 688
microplastics in soils from Sediments
2016 to 2023; b number of 650
published papers on MPs 600
570
in sediments from 2013 to
550
2023; however, in 2012,
Number of publications

500 494
2011, and 2006, the number
of publications is 6, 4, and 1 450 427
respectively
400
350
310
300 285 290

250
206
200 185
150
106
100 89
44 55
50 42
10 20 17
1 4 6 5
0
2006 2011 2012 2013 2014 2015 2016 2017 2018 2019 2020 2021 2022 2023
Year of publications

2 Microplastics Effect on Soil and Sediment
Environment
MPs in soils affect soil structure and reduce infiltra-
tion rate of soils; besides, they cause a negative impact
on water holding capacity and soil porosity (Wang et al.,
2023); hydraulic conductivity, and soil particle size dis-
tribution (Jing et al., 2023). MPs also tend to reduce the
concentrations of ­PO43– and ­NH4+ in leachate water
posing a serious threat to soil biota (Guo et al., 2023;

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Water Air Soil Pollut (2024) 235:189
Kiran et al., 2022). MPs run off in the soil causes bio-
turbation (Hurley & Nizzetto, 2018). If MPs are present
in high quantities, they clog and obstruct soil pores, thus
reducing soil infiltration capacity. This will disrupt the
nutrient cycles in the soil, change the microbial com-
munity, and eventually negatively impact plant growth
(Dong et al., 2021; Lwanga et al., 2022). Soils also
functions as a sink for MPs, and recent researches are
focused on how MPs affect the soil ecosystem (Wang
et al., 2023; Jing et al., 2023). Figure 3 shows typical MP
particles found in soil samples (Unpublished results).
Several studies (Chua et al., 2014; Avio et al.,
2015) have revealed the vector property of MPs,
i.e., carriers of harmful chemical pollutants in the
soil matrix. Some of the commonly used additives/
chemical pollutants in plastics include polychlorin-
ated biphenyls (PCBs), phthalates, nonylphenol, poly-
fluorinated alkyl substances (PFAS), Polyaromatic
hydrocarbons (PAHs), UV-stabilizers, and bromi-
nated flame retardants such as polybrominated diphe-
nyl ethers (PBDEs) (Chakraborty et al., 2022; Praja-
pati et al., 2022). The important reservoirs for MPs
are thought to be urban and agricultural soils (Hurley
& Nizzetto, 2018). Mulching processes leave behind
Fig. 3  Identification of color, size, and type of microplastics in soil using optical microscope; a–f represents film; g–l represents
fragments; m, n represents granules and o represents fiber. Scale bar: 100 µm (unpublished data)
Page 5 of 42 189
plastic residues, which are transformed into MPs over
time and through environmental factors. These MPs
scatter in the soil and adhere to other pollutants such
as persistent organic pollutants (POPs), heavy metals,
and pesticides.
According to Li et al., (2023) and Rochman,
(2018), sediments appear to be a long-term sink for
MPs. The phenomenon of biofouling involves organ-
isms colonizing on the surface of plastic particles by
secreting organic matrices, which is facilitated by the
hydrophobic nature of the plastic. The swift absorp-
tion of organic compounds leads to the formation of
a "conditioning film," enabling the beginning of a
biological process. It begins with the colonization of
bacteria and progresses to the attachment of micro-
algae and, potentially, various invertebrate groups
(Artham et al., 2009; Fazey & Ryan, 2016). Several
other studies also highlighted the emergence of MPs
in sediments, the buildup of biofilms, and the accu-
mulation and adsorption of pollutants (Kooi et al.,
2017; Xiong et al., 2022).
From the MPs analytical perspective, soils and
sediments are complex matrices. The specific fac-
tors that influence these complexities have not
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been discussed in detail (Campanale et al., 2022;
Cao et al., 2021; Dong et al., 2021). However, few
reviews report the MPs pollution in beach sand and
sediments and focus on particular geographic areas
such as Latin America and the Caribbean, the Asian
coast and the Mediterranean region (Curren et al.,
2021; Grillo et al., 2022). These reviews mainly
concentrate on the quantification, the available ana-
lytical standards and the guidelines for MP analysis,
rather than the analytical methods employed. Other
review articles examine the migration and the behav-
ior of MPs and MP additives (Li et al., 2023; Luo
et al., 2022b), and others evaluate the effect of the
extraction methods used, sometimes even highlight-
ing one specific protocol such as density separation
and the use of different salts (Cutroneo et al., 2021)
or the assessment and the degradation of MPs in the
environment to determine if these methods are eco-
friendly or not (Kasmuri et al. 2021). Moreover, no
review has been published since 2017 that exclu-
sively focuses on the state-of-the-art in the analysis
of MPs in soils and sediments, especially matrix spe-
cific challenges and guidance on how to deal with
them.
This review discusses the analytical methods for
the determination of MPs in soils and sediments.
We cover the latest developments in the methodolo-
gies (during the last 5 years) for the separation and
the extraction of MPs, as well as the innovative ana-
lytical tools that are used for their identification and
quantification with the emphasis on standardization
of analytical protocols and results reporting. Table 2
summarizes typical studies on MPs abundance in dif-
ferent soil and sediment samples.
3 Analytical Methods
The general analytical scheme followed for MPs anal-
ysis in soil and sediment samples is given in Fig. 4.
Often, the complexity of samples and the objectives
of the study necessitates additional steps for the
extraction and purification of MPs.
3.1 Soil and Sediment Sample Collection
The acquisition of the environmental sample is
the first step in the analytical procedure. A suit-
able sample site must be chosen, as the choice of an
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Water Air Soil Pollut (2024) 235:189
appropriate sample location can significantly influ-
ence the total MPs content in a particular location;
hence this is a crucial step in the overall analytical
method (Liu et al., 2018). According to the European
Commission’s Marine Strategy Framework Directive
(MSFD) guidelines, the number of sampling sites
that must be used to represent a particular region is
unrestricted, but enough replicas must be collected
to address the non-uniformity of the chosen region
to generate representative samples. The survey area
should be appropriately defined as this determines
how many samples must be collected to obtain useful
information regarding the sampling site.
3.1.1 Soil Sampling
Single-site/grab sampling or composite sampling
may be adopted depending on the sampling site and
objectives of the investigation (Möller et al., 2020;
Zhou et al., 2018). Composite sampling is preferred
for agricultural soil sampling, as this soil undergoes
regular alterations due to farming and soil condition-
ing. Single-site sampling is appropriate for soil that
is exposed to fewer human activities. Sampling tools
used include stainless steel spade, soil auger (Corra-
dini et al., 2021; van den Berg et al., 2020), shovel
(Liu et al., 2018; Zhou et al., 2018), corer (Crossman
et al., 2020; Helcoski et al., 2020), and lenz sam-
pler (Lv et al., 2019). Handpicking using a tweezer/
forceps can also be used in cases where the MPs are
distinguishable from the rest of the matrix (Gwin-
nett et al., 2021). Soil samples can be collected from
small sampling units called quadrats of dimensions of
5 × 5 cm, 10 × 10 cm, 20 × 20 cm or as defined by the
scope of the study.
The extent of pollution or agricultural activities
happening in an area can be used to determine sam-
pling depth. According to various studies, the sam-
pling depth may range between 0 and 30 cm (depend-
ing on tilling depth) (Cooper & Corcoran, 2010;
Browne et al., 2011 Yang et al., 2018). Non-agri-
cultural soil will have a relatively shallow sampling
depth than agricultural soil, typically 5 cm. Other
soils are sampled at a shallower depth of less than
5 cm. Stratified sampling is preferred to determine the
depth of pollution within the soil profile. If the ver-
tical distribution of MPs needs to be examined after
cultivation, sampling depth should be varied depend-
ing on the type of cultivation (Bläsing & Amelung,
 Table 2  Summary of typical studies on microplastics abundance in different types of soil and sediment samples by utilizing different analytical approaches
Country/loca- Type of Diges- Density Polymer identifi- MP’s Shape Polymers Size range Abundance Advantages Limitations Reference
tion soil tion separation cation counting detected
method

Brazil (Todos Mangrove 30% ZnCl2 Visual Visual Fibers, frag- - 196 μm 7735 items/kg to The study contributes to The study Paes et al.,
Santos Bay) soil ­H2O2 identification- count- ments 8417 items/kg the limited knowledge focuses 2022
Water Air Soil Pollut

Stereomicro- ing on microplastics on six

scope Polymer contamination in mangrove
identification- mangrove soils; Study sites; Lack
Micro-Raman employs a standardized of source
spectrometer methodology, which identifica-
SEM enhances reliability and tion; Lacks
comparability long-term
monitoring
(2024) 235:189

Bangladesh Agricul- 30% NaCl Visual Visual Fibers, frag- Polycarbon- 1–5 mm 2 particles/597 First comparative study No estab- Himu et al.,
tural soil ­H2O2 identification- count- ments, films ate (PC), ­m2 (rural) of microplastics pol- lished and 2022
n = 32 Stereomicro- ing Acry- 9 parti- lution in agricultural appropriate
scope Polymer lonitrile cles/469.3 ­m2 farmlands of rural, sub- procedure
identification- butadiene (suburban) 6 urban, urban, and near for sample
ATR-FT-IR styrene particles/655.2 a metropolitan area collec-
2
(ABS), ­m (urban) 5 tion and
LDPE, PP, particles/756.7 prepara-
HDPE, ­m2 (near tion; NaCl
PET, Eth- metropolitan is used
ylene vinyl city) which is
acetate not a good
(EVA), PS, density
polymethyl separation
meth- solution
acrylate
(PMMA)
Chile Soils from - Distilled Visual Visual Fibers, films, Acrylates, 1 μm 306 ± 360 Study covers various land Not found Corradini
crop water identification- count- fragment, PU, var- particles/kg use systems, including correlation et al.,
lands, NaCl Stereomicro- ing pellets nish, PE, (crop land) crop lands, pastures, between 2021
pastures, ­ZnCl2 scope Polymer PP, nitrile 184 ± 266 rangelands, and natural microplastic
range- identification- rubber, PS particles/kg grasslands; Findings and other
lands, μ-FT-IR (pastures) challenge the common pollutants
natural belief that microplas- to urban
grass- tics are ubiquitous areas and
lands roads;
n = 240 Study did
not provide
clear
evidence to
identify the
sources of
Page 7 of 42

microplas-
tics in the
soils
189

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 Table 2  (continued)
189

Country/loca- Type of Diges- Density Polymer identifi- MP’s Shape Polymers Size range Abundance Advantages Limitations Reference
tion soil tion separation cation counting detected
method

13
Vol:. (1234567890)
Shishli Bay, Surface 30% NaCl Visual Visual Fragments, rayon, PE, 0–5000 μm 499.76 ± 370.07 Study identified the main Study did not Zhang
China sedi- ­H2O2 identification- counting films, pellets PP, PA, items/kg sources of microplas- address the et al.,
ments Stereomicro- (Nano PET, PS, tics in the area, such potential 2019
Page 8 of 42

scope Polymer Meas- PMMA as river and sewage ecological

identifica- urer) and PU discharge and maritime impacts of
tion- ATR-FT- activities microplastic
IR Surface pollution;
morphology- NaCl used
FESEM in the study
is a weak
density
separator
China Farmland 30% NaCl Visual Statistical Fibers, frag- PP, PE, 20 μm–5 mm 78 ± 12.91 Strict quality control Quantifica- Liu et al.,
(Suburbs of soil ­H2O2 identification- analysis ments, films, polyester 0.03–5 mm items/kg measures were tion of 2018
Shanghai) Stereomicro- pellets (shallow soils) implemented to reduce microplas-
scope Polymer 62.50 ± 12.97 contamination use of tics in soil
identification- items/kg (deep statistical analysis pro- is described
μ-FT-IR soils) vides a robust means of as a big
analyzing the data and challenge;
determining significant Lack of
differences among dif- stand-
ferent groups ardized
methods
for plastic
quantifica-
tion in soil
Iran (south- Agricul- 30% ZnCl2 Visual Visual Fiber (promi- PET, Nylon, Length Field 1 40–830 Use of a portable wind Study only Rezaei
central Iran) tural soil ­H2O2 identification- count- nent), spher- PS, PS- > 1000 μm numbers/ tunnel to estimate the focuses on et al.,
(loamy) Stereomicro- ing ules, film, nylon, PP kg Field 2 erodibility and flux of two agricul- 2022
scope Polymer fragment 200–1100 microplastics from the tural fields
identification- numbers/kg soil surface; Insights in a specific
Micro-Raman into the potential region;
spectrometer impact of microplastics Study does
SEM on agricultural soils not inves-
Water Air Soil Pollut

tigate the
potential
effects of
microplas-
tics on crop
growth or
soil health
(2024) 235:189
 Table 2  (continued)
Country/loca- Type of Diges- Density Polymer identifi- MP’s Shape Polymers Size range Abundance Advantages Limitations Reference
tion soil tion separation cation counting detected
method

Switzerland Floodplain 65% 27% NaCl FT-IR (transmit- Box plots - PE, Latex, 125–500 μm 5 mg/kg Use of a method that Analysis of Scheurer
soil ­HNO3 CaCl2 tance mode) PVC, (88%) allows for the extrac- certain and
Water Air Soil Pollut

styrene tion, identification, and plastics in Bigalke,

butadiene quantification of MPs the small 2018
rubber in a time- and cost- MP range
(SBR), PS effective manner due to high
density or
disinte-
gration
during the
(2024) 235:189

oxidation
of organic
matter
Spain Agricul- - Distilled Visual identifi- Shapiro– - LDPE - Soil 2116 ± 1024 Study highlights the The study Beriot et al.,
tural soil water cation-Stere- Wilk’s particles/kg environmental impact acknowl- 2021
n=6 omicroscope test Feces 1000 of intensive agriculture edges the
particles/kg management and other limited
sources number
of studies
designed
to assess
the adverse
health
effects
of plastic
ingestion on
livestock,
indicating
a gap in
understand-
ing the
potential
impacts
of plastic
debris on
animal
health
Bangladesh Intertidal 30% ZnCl2 Visual identifi- Visual Fibers, films, - 1–5 mm 368.68 ± 10.65 First study to assess Study may Hossain
(Cox’s sedi- ­H2O2 NaCl cation-Stere- count- fragments (Major) items/kg microplastic pollution have biases et al.,
Bazar) ments + omicroscope ing in Cox’s Bazar ensured due to the 2021
n = 24 ­FeSO4 a broad coverage of selection of
the area sampling
Page 9 of 42

locations or
methods
189

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 Table 2  (continued)
189

Country/loca- Type of Diges- Density Polymer identifi- MP’s Shape Polymers Size range Abundance Advantages Limitations Reference
tion soil tion separation cation counting detected
method

13
Vol:. (1234567890)
Brazil Riverbed 30% ZnCl2 Visual identifi- - Fibers - 417–8178 Findings show a Study was Gerolin
Sedi- ­H2O2 cation-Stere- particles/kg relationship between conducted et al.,
ment omicroscope (0.063–5 mm) microplastic concentra- during a 2020
Page 10 of 42

(n = 7) 0–5725 tion and local hydraulic single dry

particles/kg characteristics season
(0.063–1 mm) which
may not
represent
year-round
conditions
Brazil Beach - NaCl Visual identifi- Visual Foams frag- - 1–5 mm 23.1 The study area includes Microplas- Mengatto
(Paranagua sedi- cation-Stere- count- ments pellets Brazil’s second- tics were & Nagai,
Estuarine ment omicroscope ing largest grain port and identified 2022
Complex) Micro-Raman protected areas like the visually,
spectrometer RAMSAR site without
SEM chemical
analysis
confirma-
tion
China Estuarine 30% NaCl Visual Visual Fiber (93%), Rayon, < 1 mm 121 ± 9 items/kg Study suggests that wash- The density Peng et al.,
(Changjiang sediment ­H2O2 identification- count- fragment, polyester, ing clothes is a primary separation 2017
estuary) n = 53 Stereomicro- ing pellet acrylic, source of microplastics, method
scope Polymer PET, PS, highlighting a specific used may
identification- Poly(ethy area for pollution not capture
μ-FT-IR lene:prop management all types of
(transmittance yilene:di micro-
mode) ene) plastics,
particularly
those
denser than
the saline
solution
used
Water Air Soil Pollut
(2024) 235:189
 Table 2  (continued)
Country/loca- Type of Diges- Density Polymer identifi- MP’s Shape Polymers Size range Abundance Advantages Limitations Reference
tion soil tion separation cation counting detected
method

Egypt (Alexan- Onshore NaCl Visual Thermal Films, frag- PP, PE, 50–200 μm 11.7 ± 9.5 items/ It documents ingested Concentrated El-Sayed
dria beaches) sediment identification- gravi- ments, fila- PA, PET, (major) fish MPs in fish species of on the et al.,
Water Air Soil Pollut

n = 22 Stereomicro- metric ments polyethyl- high economic value in Mediterra- 2022

scope Polymer analysis ene-vinyl Egypt for the first time, nean Coast
identification acetate contributing valuable of Egypt,
Differential (PEVA), data to the field which may
Scanning polyte- limit the
Calorimetry trafluo- generaliz-
roethylene ability of
(PTFE), the findings
(2024) 235:189

PS to other
regions
Germany Beach - NaI Visual - Fibers PP, PE, PET, 100 μm (small- 1.7, 1.3, and 2.3 Utilizes thermal desorp- Encounters Dekiff
(North Sea sediment identification- PVC, PS, est particle particles/kg tion pyrolysis gas difficulties et al.,
island of (n = 12) Stereomicro- PA size) chromatography/mass in distin- 2014
Norderny) 3 sites scope Polymer spectrometry (TD-Pyr- guishing
identification- GC/MS) for identifying microplas-
Pyr-GC/MS microplastics tics from
natural
substances
India (South- Mud 30% NaCl Visual Visual Fragment, PS, PP, PA, < 1 mm - The research evaluates The study James et al.,
west coast) ­H2O2 identification- count- filament, film, HDPE, the variability in micro- focuses 2022
Stereomicro- ing pellet, foam, PET plastic distribution dur- mainly on
scope Polymer fiber ing different monsoon polypropyl-
identification- periods and depths; It ene, which
ATR-FT-IR highlights the role of may not
environmental factors represent
like wind speed and the full
wave patterns in micro- spectrum of
plastic distribution in a microplas-
transient ecosystem tics
Page 11 of 42
189

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 Table 2  (continued)
189

Country/loca- Type of Diges- Density Polymer identifi- MP’s Shape Polymers Size range Abundance Advantages Limitations Reference
tion soil tion separation cation counting detected
method

13
Vol:. (1234567890)
India (Ship Intertidal - NaCl Visual - Fragments PU, nylon, 1.6 μm–5 mm 81 mg/kg It offers The study acknowledges Reddy
breaking sedi- identification- PS, insights that the small plastic et al.,
yard at ments Stereomicro- polyester, into the fragments identified 2006
Page 12 of 42

Alang- n = 10 scope Polymer glasswool environmen- may not represent the

Sosiya) identification- tal impact full range of materials
FT-IR Mor- of ship- present in the sedi-
phological breaking ments
study-SEM activities,
highlighting
the accu-
mulation of
plastics in
marine sedi-
ments
Iran (Qarasu Estuarine 30% ZnCl2 Visual Statistical Fibers, frag- PP, PE, PA, 200–5000 μm 182 ± 111 parti- Statistical Focuses only on the Gholizadeh
estuary) sediment ­H2O2 identification- analysis ments, films PS cles/kg dw correlation Qarasu estuary, which & Cera,
n = 10 + Fen- Stereomicro- revealed the may not represent 2022
ton’s scope Polymer correlation other estuarine system
rea- identification- between
gent FT-IR microplastics
abundance
and sediment
clay content

Turkey Susur- Lake 30% NaCl Visual Visual Fibers(major), PP, PET, PS, 0.049– 276 N/m2 1297 Utilizes pale- Difficulty in obtaining Almas
luk Basin sedimen ­H2O2 identification- count- fragments, PVC, poly- 4.951 mm fibers olimnologi- clear spectra for small- et al.,
n=2 + Fen- Stereomicro- ing film acrylates 0.18–4.9 mm cal methods sized fibers, indicating 2022
ton’s scope Polymer to track a need for more
reag- identification- historical detailed analyses
net ATR-FT-IR microplastic
accumu-
lation,
providing
long-term
data; Offers
Water Air Soil Pollut

insights into
microplastic
pollution in
freshwater
systems,
which is
less studied
compared to
marine envi-
(2024) 235:189

ronments
 Table 2  (continued)
Country/loca- Type of Diges- Density Polymer identifi- MP’s Shape Polymers Size range Abundance Advantages Limitations Reference
tion soil tion separation cation counting detected
method

Uttrakhand River sedi- 30% ~5 M Morphological Visual fragments, films, PT, HDPE, 5–1 mm 955 particles One of the The study does not Chauhan
( river ments ­H2O2 NaCl study- SEM count- pellets PVC, first study to assess the ecologi- et al.,
Water Air Soil Pollut

alaknanda) n=5 Visual identi- ing LDPE, PP investigate cal or human health 2021
fication-Stereo and PS microplastic impacts of microplas-
microscope pollution in tic pollution; No unit
an Indian is provided and just
river; Study particle count is given
covers five
sites along
the river,
(2024) 235:189

which can
capture
the spatial
variation of
microplastic
pollution
Tunishia River sedi- 10% NaCl Polymer identifi- Visual Fragments - - 611 items/m2 Highlights The study is limited Chouchene
(Kerkennah ments KOH cation- ATR- count- Fibers Foams the ubiquity to the southwestern et al.,
archipelago) n = 20 FT-IR ing Tubes of MPs in Kerkennah archi- 2021
marine envi- pelago, which may not
ronments represent other marine
and their environments
potential
impact on
human
health and
ecosystems

PC Polycarbonate; ABS Acrylonitrile butadiene styrene; LDPE Low-density polyethylene; PP Polypropylene; HDPE High-density polyethylene; PET Polyethylene terepthalate;
EVA Ethylene vinyl acetate; PS Polystyrene; PMMA Polymethyl methacrylate; PU Polyurethane; PE Polyethylene; PVC Polyvinyl chloride; SBR Styrene butadiene rubber; PA
Polyamide; PEVA Polyethylene-vinyl acetate; PTFE Polytetrafluoroethylene; CaCl2 Calcium chloride; NaCl Sodium chloride; NaI Sodium iodide; ZnCl2 Zinc chloride; H2O2
Hydrogen peroxide; FeSO4 Ferrous sulfate; μ-FT-IR Micro-Fourier transform infrared spectroscopy; ATR-FT-IR Attenuated total reflectance-Fourier transform infrared spectros-
copy; Pyr-GC/MS Pyrolysis gas chromatography mass spectrometry; SEM Scanning electron microscope; KOH Potassium hydroxide
Page 13 of 42
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 189 Page 14 of 42 Water Air Soil Pollut (2024) 235:189

Fig. 4  Flowchart of the overall analytical scheme involved in the analysis of microplastics present in soil and sediment sample

2018; He et al., 2018). The sample quantity collected
should always be higher than required for the analy-
sis, as these samples can be used as laboratory control
samples or for repetition and determination of soil
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properties (Möller et al., 2020). Collected samples
should be stored in stainless steel containers or glass
bottles. Care must be taken to avoid the interaction of
the sample with any plastic tool or surroundings that
 Table 3  Sampling methods for soils and sediments
Soil sampling
Type of method Description
Simple random sampling The sampling points are chosen randomly under the
premise that each point has an equal chance of being
selected. The method is feasible to implement, and
focuses on specific sampling zones
Systematic grid sampling It is the distribution of sampling points along the nodes
of a regular pattern. First point is selected at random
and remaining points of sample are spaced at regular
intervals from initial point. The method provides even
coverage
Transect sampling The sampling is one-dimensional systematic sampling
method. Points are chosen on regular intervals along
one or more straight lines
Unaligned grid sampling This sampling technique combines the benefits of ran-
dom sampling and systematic grid sampling. Sampling
points are situated randomly within the grid compart-
ments
Stratified sampling In this sampling method, the sampling area is divide into Depth integration method
smaller compartments known as strata. The contamina-
tion within each stratum is homogeneously distributed
than in the sampling site as whole
Judgmental sampling Judgemental sampling is based on the expert information Bed materials sampling
for example historical utilization, visual inspection. It
is simple to implement but is biased and may only be
suitable for studies which focuses on sampling zones
like hollows
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Sediment sampling
Water Air Soil Pollut
Type of method Description
Shore sediment sampling Multiple transects at a right angle from the water line and
the placement of quadrats along the transects. Transects
may be visually scanned for bigger microplastics in the
field. The surface layer can be removed to a proximate
depth and sieved or transferred to the laboratory for
(2024) 235:189
subsequent steps
Sediment manual grab methods Utilize tools such as hand spades and stainless steel spoon
for littoral and beach environments
Deeper sediment sampling Deep sediment sampling provides data on the change of
MP’s abundance and other characteristics spanning a
century to present day. Some examples are Ekman and
Van Veen grab samplers
Point integration method A sampler is lowered to stream at a specific point where
the sediment should be collected
In this method, suspended sediment is iso-kinetically
collected by lowering and raising a sampler in a constant
transit rate in a stream. Depth integration is done either
by Equal Discharge Integration (EDI) method or by
Equal Width Increment (EWI) method
Most commonly used methods for bed material sampling
are grab sampling, dredge sampling, and core sampling
for example Van Veen, Smith-Mclntyre, Ponar, Peterson,
orange peel bucket, Birge-Ekman, and Shipek are most
commonly used grab samplers
Bed load sampling This method is normally used where the sediment move-
ment and velocity of water is close to the bed, e.g., box
and basket type samplers, pan-type samplers
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 189 Page 16 of 42 Water Air Soil Pollut (2024) 235:189

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 Water Air Soil Pollut (2024) 235:189
◂Fig. 5  Sampling techniques, density separation, extraction,
and analysis methods for microplastics found in a soils and b
sediment sample (2018–2022) (n = 25)
are exposed to plastic contamination. Table 3 shows
various sampling techniques for soil samples. Obtain-
ing a representative soil sample is always challenging
due to the heterogeneous nature of soil MPs distribu-
tion; hence, a sufficiently large quantity of samples is
required (Corradini et al., 2021). Various sampling,
extraction, and identifications used for MPs are given
in Fig. 5.
3.1.2 Sediment Sampling
The first step in sediment sampling is to identify a
suitable sampling location based on which the sam-
pling approach is decided. When sampling a beach
site, transects are commonly used, with quadrats of
variable dimensions. At least two transects (50 m
apart) should be defined in each sampling area, and
their placement should be set to reflect the whole
site. It is a widely observed practice to place the
transects along the strandline as this region contains
more MPs. However, this approach is likely to pro-
duce biased results (Mendoza et al., 2021). The quad-
rats are assigned inside the transects, and the repli-
cate samples are taken (at least 5 m apart). In beach
sediments, MP’s vertical distribution is influenced
by the movement of air and water or physical activi-
ties; hence, samples must be collected from different
depths (Browne et al., 2011; Cooper & Corcoran,
2010). Studies given in Table 3 have employed differ-
ent sampling depths, ranging from 0 to 32 cm.
Bulk, selective, and volume-reduced sampling
are different types of sampling procedures. Bulk
sampling is the collection of the entire sample vol-
ume without any previous reduction. Bulk samples
are the preferred choice when visual identification
of MPs becomes challenging due to low abundance
requiring large volumes of water or sediments or
their small size making them tough to detect with the
naked eye. Selective sampling is considered when
MPs can be identified with the naked eye, and this
strategy is more prominent with sediment surfaces.
This method is only suitable for particles of size
1–5 mm and is not preferred when additional debris
adheres to MPs. Therefore, this approach is prone to
Page 17 of 42 189
bias and misidentification; hence warrants care while
sampling.
Sieving is commonly used for volume reduction.
Sediments present on the river bank can be sampled
with the help of shovels, spoons, trowels, spatula etc.
(Eo et al., 2019; Horton et al., 2017; Lenaker et al.,
2019; Sarkar et al., 2019). In contrast, sediments from
the riverbed can be collected using Van Veen grab
sampler, drill corers, sediments corer, Petite Ponar
Grab, peterson grab, Ekman dredge sampler etc.
(Castañeda et al., 2014; Crew et al., 2020; He et al.,
2020; Rao et al., 2020). Two recent approaches for
collecting undisturbed sediment sampling include
“diving bell vessel” of Mani et al., (2019), and “freeze
core sampling” of Frei et al., (2019). However, these
procedures are feasible for research but may pose
challenges for monitoring programs. Generally, sam-
ples are kept in glass or stainless-steel containers to
evade plastic contamination. Table 3 shows various
sampling methods adopted for sediment samples.
3.2 Extraction of MPs from the Sample
Once the samples are brought to the laboratory, pre-
liminary sample processing, such as sieving or hand-
picking, is adopted to remove larger particles. Fol-
lowing sieving, the required quantity of samples is
weighed accurately and dried in an oven at < 70 ◦ C
to remove moisture. However, the drying tempera-
ture and duration depend on the moisture content and
sample characteristics, for example, reported temper-
ature for drying ranged from 50 to 90 ℃ for 24 h or
overnight (Hossain et al., 2021; Liu et al., 2018; Paes
et al., 2022). In some cases, air drying method have
been used to reduce moisture (Fakour et al., 2021;
Weber et al., 2023). But, drying temperatures > 70 ℃
for longer time periods may result in surface modi-
fication of MPs (Munno et al., 2018), which is rec-
ommended by authors too. The next step is the sepa-
ration of MPs from the bulk matrix, which includes
density separation, filtration, sieving, and visual sort-
ing. Because of the complexity of soil and sediment
samples, selecting a suitable separation procedure is
challenging, especially when the particle size of the
soil/sediment and the MPs decreases (Peng et al.,
2017). Both soil and sediments generate aggregates
that could trap MPs; hence, the approach chosen
must effectively disperse the aggregates without trig-
gering the fragmentation of MPs (Fries et al., 2013;
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 189 Page 18 of 42
Li et al., 2018). The Munich Plastic Sediment Sepa-
rator (MPSS), developed by Imhof et al., (2012), is
a highly efficient tool for extracting MPs from sedi-
ments based on density separation (Rocha-Santos &
Duarte, 2015; Löder et al., 2015). The extraction effi-
ciency of MPSS for larger MP particles (1 to 5 mm)
and smaller particles (< 1 mm) were 100 and 95.5%,
respectively. Additionally, the MPSS demonstrates
the capability to extract MPs from large volume of
sediment samples, i.e., 5–6 kg of sediment in a single
operation. Furthermore, the Sediment-Microplastic
Isolation (SMI) unit offers a convenient and portable
solution for extracting MPs from diverse sediment
types with a recovery rate of 95.8% in a single step
(Coppock et al., 2017).
Another recently designed technique is the com-
pact glass, Japan agency microplastic-sediment sepa-
rator (JAMSS). The JAMSS comprises two parts:
a lower and upper modified glass plate. When the
two plates are used together, the lower container and
upper tube form a single, cylindrical container into
which the sample can be poured. The plates can then
be slid against each other to separate the lower and
upper halves of the sample by introducing a lid and
bottom (the glass plate) to each half. The recovery
rates for MPs < 1000 µm size are 94.0–97.8% (Naka-
jima et al., 2019), which is close to the previously
developed separators such as MPSS (Imhof et al.,
2012) and SMI (Coppock et al., 2017). All the units
were tested with actual field sediment samples to
understand the recovery rates. JAMSS can be proven
to one of efficient system to separate MPs from soils
and sediments.
3.2.1 Digestion
Alkali and Acid Strong acids, e.g., perchloric acid,
nitric acid, and hydrochloric acid, and strong bases,
e.g., potassium hydroxide and sodium hydroxide,
have been employed for digestion to remove organic
matter from MPs (Zou et al., 2019; Scheurer and
Bigalke, 2018; Munno et al., 2018). However, the
analytical results may show wide variation depending
on the rigor of the digestion procedure. For example,
Cole et al., (2014) examined the usage of NaOH and
HCl for separation MPs from organic-rich marine
species and seawater samples and observed that 1 M
NaOH provided better recovery (90.0 ± 2.9%) than
2 M HCl (72.1 ± 9.2%). Similarly, alkaline digestion
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Water Air Soil Pollut (2024) 235:189
(KOH, 10% 60 °C, 24 h) has yielded better recover-
ies of MPs from biological matrices. (Dehaut et al.,
2016; Zou et al., 2019). However, it is important to
note that strong acids or alkaline digestion solutions
may lead to varying degrees of MPs degradation
(Enders et al., 2019; Munno et al., 2018). Zou et al.,
(2019) compared the extraction efficiencies of the six
most commonly used digestion reagents to extract
PS-MPs from biological samples and found that KOH
digestion did not affect the surface morphology and
had the least impact on PS’s fluorescence intensity.
However, all other digestion procedures (­ HNO3: HCl,
NaOH, ­HNO3, ­H2O2, and H ­ NO3:HClO4) caused PS’s
surface to aggregate, bubble, scratch, and depressed,
as well as to diminish its fluorescence intensity to
varying degrees (Zou et al., 2019).
Several researchers have used hydrogen perox-
ide oxidation (HPO) to remove organic matter from
different types of samples, such as water (Wang
et al., 2017a, b), soil (Wang et al., 2021), sediment
(Ding et al., 2019), sludge (Li et al., 2018), and ani-
mal tissues (Lv et al., 2019). However, the reaction
time, reaction temperature, and H ­ 2O2 concentration
employed in the digestion procedures varied widely.
For example, Liu et al., (2018) utilized 30% ­H2O2 for
24 h at 70 °C to remove soil organic matter, whereas
Ding et al., (2020) used the same concentration of
­H2O2 at 65 °C for 72 h. Different reaction conditions
may be required depending on factors such as sam-
pling site, soil type, and organic matter concentration;
however, strong reaction conditions may cause par-
ticular types of MPs to degrade or even discolor or
fragment (Prata et al., 2019). It has been demonstrated
that when 70% H ­ 2O2 is used at 70 °C, 96–108% of
the organic matter in loamy-sandy soil is destroyed,
with the concomitant degradation of Polyamide (PA)
and PS MPs (Hurley et al., 2018). Temperature plays
a significant role in the degradation of polymers
(Luo et al., 2022a). Tang et al., (2018) demonstrated
that PVC placed in an oven at 50 °C did not show
any changes in FT-IR spectra, whereas PVC kept at
100 °C showed new absorption peaks after 9, 25, 45,
and 83 days. Treatment of PE and PP with 30–35%
­H2O2 at room temperature for 7 days decreased the
MPs by about 17% (Nuelle et al., 2014). Therefore,
the digestion conditions must be selected carefully. It
is suggested that Fenton’s reagent, rather than ­H2O2
alone, below 40 °C is more efficient in organic matter
removal from MPs in soil samples (Cao et al., 2021;
Water Air Soil Pollut (2024) 235:189
Hurley et al., 2018). Table 2 provides more details on
different digestion methods, nature of soil samples,
polumer types, and other details.
Enzymatic Digestion Enzymatic digestion gener-
ally destroys organic matter in soil, biological and
wastewater samples (Löder et al., 2017; Mbachu
et al., 2021). Löder et al., (2017) reported the basic
enzymatic purification protocol (BEPP) to remove
organic substances from various environmental sam-
ples, such as water, biota, sediment, and food. The
BEPP procedure focuses on three specific enzymatic
reactions: protease, cellulase, and chitinase. An ini-
tial incubation with sodium dodecyl sulfate (SDS)
and ­H2O2 treatment is employed to extract MPs from
environmental samples. Similarly, Mintenig et al.,
(2017) successfully extracted and purified MPs from
treated wastewater using enzymatic reactions, includ-
ing lipase, protease, and cellulose. Enzymatic diges-
tion has proven to be an effective, selective, and mild
method, making it a potentially useful technique for
removing soil organic matter and extracting MPs
(Railo et al., 2018; von Friesen et al., 2019). Cao
et al., (2021) demonstrated that combining proteases,
lipases, cellulases, hemi-cellulases, oxidant sample
pretreatment, and density separation could efficiently
reduce up to 90% of the organic matter in soil sam-
ples. Möller et al., (2022) studied the effect of enzy-
matic oxidative digestion methods (protease, pecti-
nase, viscozyme L, and cellulase) with various MPs
such as polylactic acid (PLA), PE, PVC, PET. Except
for PLA, the remaining MPs were unaffected by
enzymatic digestion, and the organic matter removal
efficiency was 77%. PLA showed evidence of deg-
radation and a decreased molecular weight distribu-
tion after protease treatment (Möller et al., 2022).
López-Rosales et al., (2021) analyzed MPs recoveries
with various methods of digestion and found that the
enzymatic treatment showed unaltered plastics parti-
cles and good recoveries for tested polymers (> 81%),
which is comparable to the oxidation approach
(recovery > 83%). Despite these merits, enzymatic
digestion for soils and sediments has received rela-
tively little attention since it requires more time and/
or is costlier than other digestion techniques (Cao
et al., 2021; Tirkey and Upadhyay, 2021). In case of
extraction process, authors suggest using H ­ 2O2 and
fentons reagent together for better recovery.
Page 19 of 42 189
3.2.2 Separation of Microplastics from Matrix
Density Separation An aliquot of soil/sediment is
added to high-density salt solutions; thereby, MPs are
made to float, i.e., density separation. This step helps
to separate MPs from the matrix; however, some non-
plastic particles are also likely to float if present in the
sample. In the beginning of MPs research, a saturated
NaCl solution (0.8–1.4 g/mL) was used (Möller et al.,
2022). Whereas high-density polymers such as PLA
(1.32 g/mL), PBT (polybutylene terephthalate) (1.34–
1.39 g/mL), PET (1.5 g/mL), PVC ( 1.58 g/mL)
require salt solutions such as NaI (ρ = 1.8 g ­cm–3)
(Coppock et al., 2017; Stock et al., 2019), ­Na2WO4
(ρ = 1.4 g ­cm–3) (Frias et al., 2018), ­ZnCl2 (ρ = 1.6–
1.7 g ­cm–3) (Coppock et al., 2017; Masura et al.,
2015a, b), and NaBr (ρ = 1.55 g ­cm–3) (Frias et al.,
2018; Kedzierski et al., 2017). For extraction of MPs
from soil, ­CaCl2 solution has been used by Li et al.,
(2019) as ­Ca2+ act as a bridge between organic mol-
ecules’ positive and negative charges, making it eas-
ier to separate soil organic material. Table 4 lists the
commonly used salts for the density separation pro-
cess with their merits and demerits. Almost all studies
employ density separation as a simple way to separate
MPs, either in a single step or a double-step utilizing
low-density and high-density solutions consecutively.
Although the two-step extraction is reported to yield
higher recoveries, most studies employ a single-step
extraction using a salt solution of density > 1.4 (Zhao
et al., 2017 and Nuelle et al., 2014). Even though NaI
and ­ZnCl2 solutions have high density, the recovery
and recycling of these solutions are difficult due to
their toxic and corrosive nature. However, most of
the studies reported only one-step density separation
method, i.e., after digestion as reported by Paes et al.,
(2022) and Rezaei et al., (2022) which is recom-
mended by the authors too.
3.2.3 Filtration
Sieving can be repeated after density separation to
separate bigger plastic particles if necessary. Based
on the mesh size employed, sieving also aids in deter-
mining the particle size. Following sieving, vacuum
filtration isolates the MPs from the supernatant solu-
tion. The filtration is carried out using a filter paper of
appropriate pore size, where recommended pore size
is 0.25 µm and 0.45 µm, that can retain MPs on filter
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Table 4  Salts used for the density separation of microplastics along with their solution density and pros and cons involved with them
Sl. no Salt Density of salt Pros and cons Adverse effect on environment Cost References

13
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solution (g/
cm3)

1 Sodium chloride (NaCl) 1.15–1.3 Easily available, economic, can- NaCl is non-toxic, environment $ 34.37/kg Li et al., 2019
Page 20 of 42

not separate denser polymers friendly but high chloride

2 Calcium chloride ­(CaCl2)
3 Sodium bromide (NaBr)
4 Sodium tungstate dihydrate
(Na2WO4.2H2O)
5 Monosodium phosphate
(NaH2PO4)
6 Sodium polytungstate
3Na2WO4.9WO3.H2O
7 Lithium metatungstate
­(Li2WO4)
8 Zinc bromide (­ ZnBr2)
levels can inhibit growth of
aquatic species
1.3–1.35 Economic, environment friendly Moderate effect on environment $ 311.28/kg Barnes et al., 2009
which includes excessive
chloride loading and heavy
metal contamination
1.37–1.4 Economic, non-toxic, non- Bromide ion markedly impaired $ 117.58/kg Quinn et al., 2017
corrosive reproduction in both crusta-
ceans and fishes in aquatic
system
1.4 Minor severity of hazard Low potential to affect aquatic $ 223.16/500 g Pagter et al., 2020
life as it has no BOD
1.4–1.45 May cause skin and serious eye Reacts slowly on exposure $ 91.75/500 g Zhang et al., 2018
irritation to (moisture) with (some)
metals. On burning: release
of toxic and corrosive gases/
vapors (phosphorus oxides)
1.4–1.65 Expensive, hazardous Causes harmful effect on $ 233.43/100 g Cunningham et al., 2020
aquatic life, fire, and spillage
in water can also cause pollu-
tion of watercourses
1.62 Non-hazardous It is not toxic to the aquatic $ 115.59/25 g Masura et al., 2015a, b; Quinn
environment et al., 2017
1.7 Higher recovery rate, hazardous Chronic aquatic toxicity $ 164.70/500 g Quinn et al., 2017
Water Air Soil Pollut

9 Potassium iodide (KI) 1.7 Hazardous The chemical is dangerous for $ 78.46/500 g Cutroneo et al., 2021; Mu et al.,
water, soil, tap water, drains 2019
10 Zinc chloride (­ ZnCl2) 1.5–1.8 Aqueous solution is corrosive It is very toxic to aquatic organ- $ 142.22/kg Li et al., 2019
and toxic, suitable for separa- isms
tion of higher dense polymers
11 Sodium iodide (NaI) 1.55–1.8 Expensive, suitable for separa- It is very toxic to aquatic life $ 158.21/500 g Li et al., 2019; Quinn et al., 2017
tion of higher dense polymers with long lasting effect
(2024) 235:189

12 Potassium formate (HCOOK) 1.91 Expensive, classified as irritant Irritating to eyes, respiratory $ 71.97/kg Zhou et al., 2018
system, and skin
Water Air Soil Pollut (2024) 235:189
paper (Sørensen et al., 2021). A wide range of diam-
eters (25 to 125 mm) and pore sizes (0.2 to 5 µm) of
filter papers have been reported for MPs filtration
(Hidalgo-Ruz et al., 2012; Maes et al., 2017; Claes-
sens et al., 2011; Frias et al., 2010; Crichton et al.,
2017). Filter papers that are commonly used include
silicon membrane, glass fiber (GF), nitrocellulose and
polytetrafluoroethylene (PTFE) filters. The type of
filter paper used for MPs characterization may vary
based on the instrumental technique used. For exam-
ple, optical microscopy-based techniques employ GF
or nitrocellulose filters, whereas for automated imag-
ing with IR spectroscopy, reflective or IR transparent
filter papers such as silica, alumina, silver oxide are
used. In the case of mass spectroscopy approaches,
the filter paper should not interfere with the plastic
signal; therefore, glass fiber filter paper is suitable for
pyrolysis gas chromatography/mass spectroscopy (pyr
GC–MS). Table 5 gives details of the various types of
filter papers, pore sizes, characteristics, specific appli-
cations, and approximate cost.
3.3 Identification and Quantitation
Various analytical methods are used to identify poly-
mer types, including visual sorting with the help of
the naked eye or microscope, pyr-GC–MS, and ther-
mogravimetric and spectroscopic techniques such
as Raman or Fourier transform infrared (FT-IR)
spectroscopy.
3.3.1 Visual Identification and Counting
An optical microscope or stereomicroscope is the
most common technique used for MP’s identifica-
tion and quantitation. This method is reported to
have error rates ranging from 20 to 70% (Song et al.,
2015). This could be overcome by using a stereomi-
croscope in conjunction with spectroscopic tech-
niques that are capable of distinguishing MPs from
the rest of the sample. These include the “hot needle
test,” or comparing microscopic images of the sample
before and after heating. This procedure leads to the
disintegration of MPs and hence helps in the identifi-
cation of MPs. However, these techniques are also not
error-free and come under destructive analytical tech-
niques where the sample cannot be recovered after-
wards for further analysis.
Page 21 of 42 189
Another way for visual identification using the
stereomicroscope is to stain the sample, in which a
lipophilic dye (e.g., Nile Red) selectively stains the
MP particles, which can then be analyzed based on
their fluorescence (Maes et al., 2017). However, the
efficiency of this approach for soil and sediment sam-
ples is debatable because, given the complexity of the
matrix, other lipophilic detritus present in the sam-
ple has the probability of absorbing the dye, adding
difficulty to the identification of MPs (Möller et al.,
2020). Quantitation is done by manually counting
the MPs in a unit area (1 × 1 cm) of the filter paper
and then extrapolating it to the entire area. The dis-
advantage of this method is that it is very susceptible
to error and false identifications, leading to inaccurate
observations. Integrating microscopy with spectros-
copy is useful in confirming the presence of MPs, as
in the latter, identification is based on the polymer
type.
3.3.2 Chromatography
When combined with additional approaches, chro-
matographic techniques can provide quantitative
and qualitative identification of different polymers.
Several studies have utilized methods such as sol-
vent extraction with size exclusion chromatography
(SEC), Pyr GC–MS (Dekiff et al., 2014; Fries et al.,
2013; Hendrickson et al., 2018), and Pyr GC–MS
with attenuated total reflectance-Fourier transform-
infrared (ATR-FT-IR) spectroscopy (Dümichen et al.,
2017; Fischer & Scholz-Böttcher, 2017; Löder et al.,
2015). However, the practical efficiency of these
approaches is limited due to the small pyrolysis cap-
sule size and sample amount per run, in addition
to the extensive sample clean-up required in the case
of high-volume samples (Peñalver et al., 2020). This
renders the procedure to be extremely time-consum-
ing and ineffective for bulk samples. These drawbacks
are overcome in the technique thermal extraction
desorption-gas chromatography-mass spectrometry
(TED-GC–MS) in which the gaseous degradation
products are trapped in a solid phase and analyzed by
GC–MS. Apart from sample grinding and mixing to
achieve homogeneity, this procedure does not require
much sample pre-treatment. Compared to other meth-
ods, TED-GC–MS can handle more samples and
takes less run time. However, the drawback is that it
is a destructive analytical approach; therefore, MPs
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 Table 5  Various filter papers with their features and applications in microplastics characterization
189

Type of filter paper Pore size Key features Applications Working Tempera- Chemical compat- Cost Hydrophobic Hydrophilic
ture ibility

13
Vol:. (1234567890)
Nylon 0.1 to 10 µm This filter paper Filtration of biologi- Upto 100ºC Compatible with $ 170.97/100 ea ●
requires very low cal samples, envi- aqueous and most
extractable content ronmental samples, organic solvents
Page 22 of 42

and do not contain and particulate Autoclave friendly

any wetting agents, matter It can withstand
detergents, or temperatures up to
surfactants. It is 180 °C
versatile to use and
consistent perfor-
mance
Glass fiber 0.3 µm to 2.7 µm Fast flow rates, high Contaminated air or Upto 500ºC Excellent compat- $ 225.21/100 ea ●
loading capacity, exhaust air escap- ibility with organic
wide-range thermal ing control solvents and strong
tolerance, excel- Removal of sedi- acids (apart from
lent precipitate ment and coarse hydrofluoric acid)
retention, and ideal particulate and bases. Either
for gravimetric used as a prefilter
analyses or as a final filter
Polycarbonate 0.1 µm to 10 µm It is precise with uni- These membrane Upto 140ºC It is compatible with $ 212.88/100 ea ●
form pore size and filters are com- aqueous solution
it is surface capture monly used in of pH 4–8 and
of sample race element with some solvents
and particulate and hydrocarbons
analysis, gravi-
metric analysis,
water analysis, and
general filtration
Nitrocellulose 0.22 to 8 μm It has high non- Sample preparation Upto 75 °C Compatible with $ 711.63/25 ea ●
specific adsorp- Microbiological acetic acid, carbon
tion behavior and studies tetrachloride,
Water Air Soil Pollut

contains no support Filtration of aqueous chloroform, cresol,

fabric or detergents. solutions and phenol
It is Compatible
with commonly
used transfer condi-
tions and detection
methods such as
(2024) 235:189

staining, immuno-
detection
 Table 5  (continued)
Type of filter paper Pore size Key features Applications Working Tempera- Chemical compat- Cost Hydrophobic Hydrophilic
ture ibility

Cellulose acetate 0.22 to 8 μm It has high flow rate, General filtration, Upto 50 °C Compatible with $178.79/100 ea ●
thermal stability cytology, binding aqueous solution,
Water Air Soil Pollut

and lo w absorp- studies most alcohols,

tion hydrocarbons, and
oils
Microglass Fiber 1.5 to 3 μm Made of 100% pure environmental Upto 500 °C Excellent compat- $ 39.61/100 ea ●
Filter borosilicate glass. analysis for water, ibility with organic
It has intrinsic wastewater, solvents and strong
properties espe- testing of soils, acids (apart from
(2024) 235:189

cially when fine air pollution hydrofluoric acid)

filtration and high and monitoring, and bases
loading capacity is research and pro-
required cess biochemistry,
and gravimetric
analysis involv-
ing ignition of
samples, filtration
of hot
gases and liquids,
and in pre-filtration
Silver membrane 0.2 to 5 μm Made of 99.97% Used for air moni- Upto 550 °C Chemically resistant $ 408.57/50ea ●
pure inorganic toring of carbon to:
metallic silver, black, coal tar alcohols, fuels,
they are chemi- products, coke hydrocarbons,
cally inert and oven emissions & natural and
resistant to high silica synthetic oils,
temperatures for alkalis, cryogen-
sampling aggres- ics, photoresists,
sive contaminants ether, propellants,
and are Conductive oxidizers, halogen-
in nature ated hydrocarbons,
esters, most organ-
ics and acids
Page 23 of 42
189

Vol.: (0123456789)
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 Table 5  (continued)
189

Type of filter paper Pore size Key features Applications Working Tempera- Chemical compat- Cost Hydrophobic Hydrophilic
ture ibility

13
Vol:. (1234567890)
Aluminum oxide 10 to 200 nmThey are uniform, HPLC sample and Upto 400 °C Compatible with $ 1418.61/50 ea ●
membrane densely-packed mobile phase most solvents and
honeycomb pore filtration can be aqueous material
Page 24 of 42

structures that con- done. Filtration of

tribute to precise aggressive organic
retention and high solvents, virus
porosity char- concentration
acteristics. Fast and analysis, and
filtration, efficient analysis of micro
separation, and plastic in water
high purity
Polytetrafluoroethyl- 0.1 μm and 5 μm They are suited for Clarification of cor- Upto 120 °C Highly resistant to $ 79.97/10 ea ●
ene (PTFE) aggressive media, rosives, solvents, most acids, alco-
since they are and aggressive flu- hols, detergents,
chemically inert. ids. This includes and solvents but
The membrane is the important not compatible
laminated onto a requirement in with certain alkali
nonwoven poly- HPLC analysis for metals and fluori-
propylene support sample filtration nating agents such
web for improved where any solid as xenon difluoride
strength and han- particles can cause and cobalt(III)
dling permanent damage fluoride
to the column
*
Indicative cost per unit pack of the filter paper. Cost estimation based on international brands available in India
Water Air Soil Pollut
(2024) 235:189
Water Air Soil Pollut (2024) 235:189
cannot be recovered after the analysis, which results
in the loss of information about the morphology and
number of MP particles (Naji et al., 2019).
3.3.3 µ‑FT‑IR and µ‑Raman Spectroscopy
Micro-FT-IR spectroscopy (µ-FT-IR) is an ana-
lytical tool which combines FT-IR spectroscopy
with microscopy. The µ-FT-IR has high spatial
resolution; hence, infrared bands can be identified
and compared with smaller samples. The µ-FT-IR
includes an objective lens for viewing MP particles
and an infrared probe for identifying and quantify-
ing MPs (Birch et al., 2020; Harrison et al., 2012;
Zhou et al., 2018). The analysis conducted has
a spatial resolution that is limited by diffraction.
Theoretically, it is about 1.7 μm at 4000 ­cm–1 and
13 μm at 500 ­cm–1. The lower size range of parti-
cles that can be identified without ambiguity is
10–20 μm (Cabernard et al., 2018; Löder et al.,
2015; Mintenig et al., 2019; Primpke et al., 2020;
Simon et al., 2018). The sample preparation is
minimal and is useful for the direct identification
of MPs (< 500 μm) on membrane filters (Harrison
et al., 2012). The technique of μ-FT-IR can be car-
ried out using either reflectance or transmission
mode. The transmission mode yields spectra of high
quality; however, it necessitates the use of infrared-
transparent substrates. On the other hand, the reflec-
tance mode allows for the quick analysis of thick
and opaque samples and is particularly effective
in detecting MPs in environmental samples (Ojeda
et al., 2009; Wenning et al., 2002).
The μ-FT-IR is used widely to characterize MPs
in different matrices, for example, marine organisms
(Zhang et al., 2020), sediment (Harrison et al., 2012;
Peng et al., 2017), food (Li et al., 2018) and surface
water (Wu et al., 2020). This technique is valuable for
its ability to gather data with spatial resolution and
for its usefulness in analyzing intricate samples. For
example, in one study by Zhang et al., (2019) on MPs
pollution in surface sediments of Sishili Bay, eight
types of polymers such as PP, rayon, PE, PA, PMMA,
PET, PS, and PU were identified using μ-FT-IR
method.
Micro-Raman spectroscopy identifies diverse size
classes of plastic particles, including those smaller
than 1 µm (Cole et al., 2014). Combining Raman
microscopy with Raman spectral imaging makes
Page 25 of 42 189
it feasible to produce spatial chemical images of a
sample based on its Raman spectra. Theoretically,
µ-Raman imaging could enable a spectral analysis
of complete membrane filters at a spatial resolution
below 1 µm, enabling to detect NPs (nanoplastics) in
environmental samples. However, µ-Raman spectros-
copy is less widely used than FT-IR.
The spectroscopic methods used for analyzing
MPs have limited spatial resolution due to the dif-
fraction limit of light. For instance, μ-FT-IR spec-
troscopy is restricted to about 10 μm, while μ-Raman
spectroscopy is limited to about 300 nm. This enables
μ-Raman spectroscopy for the analysis of nearly all
sizes of MPs. However, combining confocal opti-
cal microscopy with Raman spectroscopy (known as
μ-Raman spectroscopy) and utilizing visible-range
excitation lasers can lead to a much better spatial res-
olution of 1 μm or even below ≈300 nm, compared
with µ-FT-IR spectroscopy. Therefore, μ-Raman
spectroscopy is best suited for the analysis of NPs
(Anger et al., 2018; Ivleva et al., (2017).
3.3.4 FT‑IR and Raman Spectroscopy
Spectroscopic identification of polymers is most
reliable as it identifies the chemical makeup of an
unknown polymer by comparing the spectra of known
polymers with that of unknowns (Naji et al., 2019).
Raman spectroscopy (Bläsing & Amelung, 2018) and
FT-IR are the two common vibrational spectroscopic
techniques employed for MP analysis (Hendrick-
son et al., 2018; Käppler et al., 2016; Zhang & Liu,
2018). Both procedures analyze MPs over the surface
of the filter paper; therefore, MPs must be cleaned
appropriately to avoid any adhering contaminants
interfering with the sample spectrum, which reduces
the sample amount that can be used per assay. Tra-
ditional FT-IR can be used to identify large plastic
particles, whereas ATR-FT-IR can be used to exam-
ine MPs of size greater than 500 μm (James et al.,
2022). The focal plane array (FPA) based micro-FT-
IR (Löder et al., 2015) best identifies MPs of size less
than 500 μm. Transmittance, reflectance, and ATR
modes are among the different FT-IR modes that can
be used for MP analysis. Transmission mode involves
sample preparation when using thick and opaque
MPs, and this is done to allow IR radiation to pass
through the sample. Samples with irregular surfaces
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 189 Page 26 of 42
produce an irregular spectrum in reflectance mode,
indicating deterioration.
FT-IR has proven to be a highly useful method
for examining the chemical changes in particle sur-
faces caused by weathering/aging. Typically, one can
observe the emergence of new absorption bands asso-
ciated with OH, C═O, and COOH groups. Molecular
mapping of MPs using FPA-based imaging is useful
for studying morphological characteristics where,
characteristic spectra of the sample will depend on
the type of bonds in the particles, which aids in differ-
entiating MPs from the rest of the sample. The extent
of weathering on the plastic can also be determined
based on changes in chemical bond structures. A
study by Fan et al., (2021) on MPs constituent iden-
tification from admixtures using FT-IR revealed that
the characteristic wavenumbers for common polymers
such as PET are 793 ­cm−1, PE are 1472 ­cm−1 and
1462 ­cm−1, PP 841 ­cm−1, PVC 712 ­cm−1, and nylon
3925 ­cm−1. Only a few wavelengths in the obtained
spectrum contain relevant information for the iden-
tification polymer type in MPs; hence, manual inter-
ventions are required to minimize error rates. To
overcome this limitation, the curve fitting approach
is used where only the most important bands in the
spectrum are used to find a match. This method
improved accuracy ranging from 60 to 99%.
Raman imaging takes longer than FT-IR imaging
as the sample run time is longer in the former; how-
ever, the result of µ-FT-IR imaging is reliant on the
size, shape, and thickness of the analyte particles,
whereas Raman imaging is independent of the mor-
phology of the particles. Fuller & Gautam, (2016)
employed a novel method viz. pressurized fluid
extraction (PFE) to isolate MPs from the soil matrix
through selective dissolution of MPs. This poly-
mer–solvent mixture was then vaporized and ana-
lyzed by ATR-FT-IR spectroscopy (Fuller & Gautam,
2016). The advantages of this method are its speed,
independent of particle size, and less sample prepara-
tion time.
Apart from spectroscopic techniques, another
method of MPs identification is differential scanning
calorimeter (DSC) (El-Sayed et al., 2022). Because
both Raman and FT-IR are very effective techniques
for analyzing MPs, the decision to use one over the
other is usually determined depending on the goal of
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Water Air Soil Pollut (2024) 235:189
the study rather than their performance (Möller et al.,
2020). Peez et al., (2019) have presented a new meth-
odology for size-independent MPs analysis, such as
model samples of PE particles, PS beads, and PET
fibers using quantitative Proton nuclear magnetic
resonance (1H NMR) spectroscopy. The approach
is said to be inexpensive and quick. Still, all organic
matter must be removed from the sample to prevent
signal overlays. The 1H NMR approach is considered
inadequate for MPs detection in soil samples because
removing 100% of organic matter from soil samples
is impossible without affecting and damaging MPs
(Möller et al., 2020).
3.3.5 Scanning Electron Microscopy
Scanning electron microscopy (SEM) is one of the
useful techniques for obtaining morphological char-
acteristics of MPs (Reddy et al., 2006; Wagner et al.,
2019). Generally, SEM is combined with energy-
dispersive X-ray (EDX) technology, which provides
information about the elemental composition of mate-
rials’ micro-areas (Wagner et al., 2014; Zhao et al.,
2017). The advantage of SEM–EDX is it gives both
the elemental composition and surface morphol-
ogy of MPs simultaneously (Eriksen et al., 2013,
Van Cauwenberghe et al., 2015, Fries et al., 2013).
Despite being commonly perceived as an expensive
method, SEM–EDX analysis requires little time for
analysis as compared to other microscopic techniques
(Table 6). When characterizing MPs, environmental
SEM mode can be used to avoid introducing nitro-
gen gas into the SEM chamber. Additionally, sputter-
ing carbon or gold on the sample surface is required
to obtain high-resolution images. Many studies have
utilized conventional SEM to observe MPs in various
matrices such as sand (Tiwari et al., 2019), mussels
(Li et al., 2018), sewage sludge (Mahon et al., 2017),
and sediments (Neto et al., 2019; Shruti et al., 2019;
Wang & Wang, 2018).
It is important to understand that SEM method
involves extensive time and effort in preparing sam-
ples, making them impractical for analyzing large
numbers of particles needed for comprehensive stud-
ies. Nevertheless, these techniques offer significant
insights into particle morphology and elemental com-
position, facilitating comprehensive analysis of MPs.
 Table 6  Summary of commonly used analytical techniques for analysis of microplastics
Method Analyzable sample size Advantages Limitations

Stereo- (optical) Microscopy Evaluate particles larger than 50 µm–5 mm Microscopic method helps in identification Microplastics’ composition cannot deter-
efficiently of microplastics, physical characteriza- mine with this technique
tion, and abundance of microplastics is
Water Air Soil Pollut

calculated
FT-IR ATR-FT-IR can evaluate particles larger FT-IR such as focal plane array FT-IR
than 500 mm, and microscope coupled (FPA-FT-IR), micro-FT-IR (μ-FTIR),
FTIR can study MPs smaller than 20 mm and attenuated total reflectance FTIR
(ATR-FTIR) allow detection limit down
to 5–10 μm. FPA-FTIR can automati-
cally scan sample filter and obtain the
FTIR has limitations to examine wet sam-
ples. ATR-FTIR needs the probe to make
contact and pressure with the target mate-
rial, which has the possibility to cause the
loss and damage the microplastics
(2024) 235:189

spectral information quickly. It has a

library or a comprehensive polymer
database
NIR spectroscopic NIR spectroscopy can analyze microplas- Fast sample analysis and no pretreatment The sensitivity and specificity experiments
tics with size range 1 mm to 500 µm required of combined NIR spectroscopic chemo-
metric approach have not been successful
so far
Raman Spectroscopy Microscopy coupled Raman Spectroscopy It can detect microplastics smaller than The automatic mapping of micro-RS is still
(RS) method can examine particles of 1 m in size and in some cases as low as under development and is time-consuming
size more than 1 μm 500 nm. It can Analyze the wet sample
and simultaneous identify fillers or pig-
ments. The fast chemical mapping can
be performed by RS method
Mass spectrometry analysis, such as Pyr- No effects of particle size Pretreatment is not required in this method Only one particle with certain weight can
GC–MS, TGA-MS, and TED-GC–MS be assessed per run
Hyperspectral imaging technique Not affected by particle size No pre-treatment required and fast sample The technique is only capable of scanning
analysis microplastics (0.5–5 mm) on the surface
of soils
Time-of-Flight Secondary Ion Mass Spec- TOF–SIMS can analyze microplastics to Fast sample analysis This technique is a destructive method and
trometry (TOF–SIMS) the size down to < 15 µm it can only be used to analyze microplas-
tics with known compositions
SP-ICP-MS size range from approximately 1 to SP-ICP-MS could provide information Single particle mode (SP-ICP-MS) can only
5 − 10 μm on both the size distribution and mass help in quantitation of microplastics and
concentration of MPs not characterization
UV/VIS spectroscopy - UV/VIS spectrophotometer does not It has low accuracy due to organic interfer-
require expensive apparatus with high ence other than microplastics
Page 27 of 42

maintenance. The instrument helped in

quantifying the organic contents of the
189

targeted microplastics

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 189 Page 28 of 42 Water Air Soil Pollut (2024) 235:189

3.3.6 Atomic Force Microscopy

required and this method cannot be used

derived. The contact could release frag-

Impurities in environmental samples may

tions; also, the tip can produce artifacts

ments, in case of adhesive polymers, to

AFM cannot prevent outside contamina-

interfere with the experimental results

the tip and could produce an incorrect

Complex pre-treatment procedures are

Atomic Force Microscopy (AFM), a less-commonly
employed technique for MP analysis, operates by

at one time, also has much higher resolu- to analyze color of microplastics
employing a thin probe (cantilever) to interact with
the surface of the sample and generates high-reso-
image of the sample lution images at the nanometer (nm) scale. AFM is
frequently coupled with either Raman spectroscopy
or FT-IR to obtain information about polymer type.
AFM probes are capable of both contact and non-
Limitations

contact modes when interacting with samples. A pie-

zoelectric mechanism moves the sample along three
Cartesian axes while the cantilever glides across its
allows more of a specimen to be in focus
direct 3D images of the surface structure

surface. The tip can be maintained under “constant

tion, so closely spaced specimens can be
non-conducting polymers, as in the case

are detailed, highly resolved, and highly

can be used to investigate the surface of

of MPs. Other than that, AFM provides

involves simple sample preparation, it
AFM preserves the sample surface as it

force,” where data regarding interaction strength

Experimental results for this method
SEM has a large depth of field, which

The technique is non-destructive and

critical samples can be recovered.

between the tip and the sample surface can be col-

magnified at much higher levels

lected, or “constant height,” where information on the

sample’s height fluctuations can be obtained.
The sample preparation for AFM involves making
a colloidal suspension of particles, diluting it with
of the polymers

ultrapure water and transferring an aliquot, typically

5 µL, to a clean glass slide. Standard silicon nitride
Advantages

precised

cantilevers ScanAsyst-Air (Bruker; nominal length

115 µm, tip radius 2 nm, spring constant 0.4 ­Nm−1)
are used for operating in PeakForce Tapping mode
(Cavallaro et al., 2020). The registration of the inter-
action force curve at each pixel is the foundation of
the PeakForce Tapping mode. The force curve shows
how the interaction force between the cantilever and
the specimen depends on their distance. AFM ena-
bles additional characterization compared to SEM
Analyzable sample size

analysis, such as hydrophobicity (Fu & Zhang, 2018),

stiffness (Zhang et al., 2012), magnetization (Middea
0.04–2000 μm

et al., 2015), or conductivity (Trotsenko et al., 2016).

1 nm to 8 μm

0.001–5 µm

Using AFM enables the examination of non-conduc-

tive polymers to analyze their surfaces. AFM offers
the advantage of avoiding radiation damage to the
sample, unlike SEM. Some of the important advan-
tages and disadvantages of AFM are given in Table 6.
Laser diffraction particle size analysis
Scanning electron microscope (SEM)
Atomic force microscopy (AFM)

3.3.7 Transmission Electron Microscopy

The observation of fine structures smaller than

0.2 μm, which are not visible through optical micros-
Table 6  (continued)

copy, can be achieved through the use of transmission

electron microscopy (TEM). High energy electrons
discharged either by a field emitter source or a thin fil-
Method

ament of thermoionic material ­(LaB6 or W) is trans-

mitted through MPs. This produces high-resolution

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Water Air Soil Pollut (2024) 235:189
images, typically about three orders of magnitude
compared to optical microscopes. Due to its high
resolution, TEM is most suited for the identification
of smaller MPs and NPs (Gigault et al., 2016; Song
et al., 2020).
According to GESAMP, there are five primary
morphological classifications for MPs: fragments,
pellets, films, lines, and foams. The “lines” category
considers the particles’ aspect ratio and covers fila-
ments and fibers (GESAMP, 2019). Identifying the
various morphologies of MPs present in the environ-
ment makes it possible to classify them according to
their properties without using advanced instruments.
Moreover, morphological identification can give val-
uable insights into the sources of plastic pollution and
the fate of a particular type of debris (López-Rosales
et al., 2021). The characterization of particle shape
has been done using a variety of quantitative descrip-
tors. The most basic dimensions, such as width,
length, and height, deliver the preliminary characteri-
zation of the shape of the particle, but other measures
like irregularity or roundness can be acquired through
image processing (Blott & Pye, 2008). Roundness
describes the presence of corners and edges, while
irregularity refers to the deviations from a regular
three-dimensional shape due to the presence of con-
cavities and convexities. While unevenness and sur-
face irregularities have a limited impact, the main
dimensions of particles dictate their behavior in the
aquatic environment (Khatmullina & Isachenko,
2017). Particle settling or buoyancy characteristics
are typically determined using correlations that were
developed for particles with regular or nearly regular
shapes. However, this poses a challenge in obtain-
ing accurate shape descriptors. These morphological
descriptors need standardization to minimize ambigu-
ity in the comparison data from various sources and
surveys. Nevertheless, morphological characteriza-
tion involves some amount of subjectivity (López-
Rosales et al., 2021).
In recent times, 3D laser range scanners and X-ray
microtomography (X-ray mCT) have emerged as tech-
niques that can provide information on the 3D shape
of particles in a relatively short time (Rosal, 2021).
The process of X-ray mCT involves creating a three-
dimensional representation of an object using a series
of 2D projections captured during tomographic scan-
ning (Bozzini et al., 2018). This results in the genera-
tion of digital units known as voxels, which can be
Page 29 of 42 189
used to calculate each particle’s volume and surface
area by adding the volumes of the individual voxels
and their external areas. To determine the particles’
length, width, and height, an eigenvalue problem for
the inertia matrix needs to be solved (Safonov et al.,
2018). An alternative method for obtaining analyti-
cal functions of the external surface of 3D particles
involves combining X-ray mCT with spherical har-
monic analysis. Although X-ray mCT is currently of
limited use, it has been applied to the study of MPs
(Sagawa et al., 2018; Tötzke et al., 2021).
3.4 Quality Assurance and Quality Control (QA/QC)
Given the complexity of sampling, sample prepara-
tion, and quantitation techniques, it is not surpris-
ing to note that the data reported so far on MPs is
either under or over-estimated (Hanvey et al., 2017).
However, data comparison between studies could be
improved to a certain extent by following strict qual-
ity control measures during sampling to analysis.
MPs pollution can arise from various sources, includ-
ing airborne deposition on equipment and samples,
plastic-based sampling apparatuses, water utilized for
sample processing and equipment cleaning, reagents,
working solutions, and synthetic garments worn by
laboratory personnel. For example, sodium chloride,
one of the cheapest salts used for density separation,
was reported to contain 50 to 280 MPs particles/kg
(Iñiguez et al., 2017).
Three approaches can be adopted to reduce the
risk of secondary contamination: (i) implement sound
field practices and adhere to good laboratory prac-
tices (GLPs) that reduce the introduction of MPs con-
taminants in the chemicals, air, surfaces, and equip-
ment; (ii) assess the extent of MPs contamination
introduced to samples through background checks,
field and procedural blanks, and subsequently apply
blank correction; (iii) apply limit of detection (LOD)
and limit of quantitation (LOQ), by utilizing proce-
dural blanks. Various approaches used to minimize
MPs contamination are given in Fig. 6.
After collecting and processing samples, it is cru-
cial to quantify and characterize blanks and conduct
background checks. If experimental samples contain
analogous MPs, these blanks can be omitted or, at the
very least, acknowledged with the data during pub-
lication (e.g., Vandermeersch et al., 2015). Another
option, as examined by Kroon et al., (2018), is to
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 189 Page 30 of 42
Fig. 6  Recommended procedure to mitigate air contamination, cross-contamination, and ensure control over contamination through-
out the stages of microplastic sampling, processing, and identification
gather items that have the potential to contribute to
secondary contamination, such as neuston nets, paint
chips from remotely operated vehicles (ROVs), coral
skeletons, human hair, clothing, gloves, rubber bands,
and lab coats. These items can then be analyzed using
ATR FT-IR to construct a tailored library of spectra.
MPs present in the samples that display > 90% spec-
tral match to the tailored library can be excluded from
the final tally.
4 Models for Accumulation, Contamination,
and Pollution Assessment for Soil
and Sediments
It is commonly believed that plastic particles exhibit
biochemical inertness as a result of their large suba-
tomic scale; hence, it appears that plastics are less
hazardous and non-toxic. However, the slow degrada-
bility, combined with the cocktail of chemical addi-
tives, makes plastics the most notorious pollutant
humans have ever made (Campanale et al., 2020). In
addition, polymerization reactions are hardly com-
plete, and unreacted residual monomers may be found
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Water Air Soil Pollut (2024) 235:189
in the polymeric material, which can harm the envi-
ronment and human health or may impact the proper-
ties of the polymer (Campanale et al., 2020). Other
than residual monomers, plastics have various types
of additives, such as plasticizers, UV-stabilizers,
flame retardants, processing aids, and low-atomic-
weight polymer segments as well as oligomers,
polymerization solvents, and catalyst residues (Wies-
inger et al., 2021). Most non-polymeric segments
have low atomic weights, meaning they could migrate
from the plastic object into the environment.
Furthermore, MPs accumulate several contami-
nants from the surrounding environment, like heavy
metals and organic contaminants (Chakraborty et al.,
2022). Hence, MPs pose risks due to particle toxic-
ity, additives, and accumulated contaminants. Several
model equations are proposed for the risk assessment
of MPs, which are discussed below.
4.1 Polymer Hazard Index and Pollution Load Index
The application of index models for evaluating MP
pollution load as well as risks is important as it help
to quickly assess the risk and make a decision. The
Water Air Soil Pollut (2024) 235:189
index is an algorithm that computes the final result as
a single number from the measured variables, thereby
expressing a measure of the qualitative indicator of
MP’s pollution. For example, the polymer hazard
index (PHI) is calculated using Eq. 1, using the MPs’
concentration and polymer type.
∑ pRoverall = pR1 × pR2 × pR3 … … … pRn n
PHI = Pn × Sn (1)
The representation of the percentage of specific
polymer types sampled and collected at each location
is represented by Pn and Sn and the total hazard is rep-
resented as the sum of different individual polymer
hazards (Lithner et al., 2011).
The pollution load index (PLI) is used to evaluate
the degree/extent of MP pollution in surface sedi-
ments (Ranjani et al., 2021). Here PLI at every loca-
tion is associated to MP concentration factor (CF i ), as
given in Eqs. 2 and 3.
Ci
CF i = (2)
Coi
(3)
√
PLI = CF i
CF i is the quotient of the MP concentration at each
location (Ci ) to the background MP concentration
(Coi ). The lowest MPs concentration found in sedi-
ments is denoted as the background value. PLI has
been categorized as low or “risk category I” if the
value is below 10, medium or “risk category II”, if
they fall between 10 and 20, significant or under “risk
category III” if they range from 20 to 30, and high or
under “risk category IV” if they exceed 30.
4.2 Polymer Risk Indices and Potential Ecological
Risk Index
There is no standard approach for assessing the MPs
risk. To assess the ecological hazards of MPs/NPs,
one can consider the polymer composition and the
associated chemical toxicity coefficient. The equa-
tions for determining the polymer risks indices
("pRi") and the overall polymer risks indices for a
given sample (­pRoverall) are provided in Eqs. 4 and 5
(Lithner et al., 2011). The “pRi” is used to evaluate
the potential environmental hazard associated with
the MPs/NPs. On the other hand, “pRoverall” measures
the overall polymeric risks across all samples, which
Page 31 of 42 189
is calculated as the ­nth root of the product of the poly-
mer risks indices and the number of samples.
∑ Pmi
pRi = ( × Sj ) (4)
pT
)1
(5)
(
where “Pmi” represents the number of individual
MPs/NPs polymers discovered in sample i, and
“pT” indicates the total number of MPs/NPs poly-
mers identified in sample i. The chemical toxicity
coefficient derived from hazard ratings of several
polymers is represented by “Sj.” The polymeric risk
indices ­(pRi) have been categorized as low if they
are below 150, medium if they fall between 150 and
300, significant if they range from 300 to 600, high
if they exceed 600, and very high if they are greater
than 1200.
The polymer ecological risk index (pERI) esti-
mates the degree of risk of MPs/NPs to the ecologi-
cal system, including sediments and biota. pERI is
provided in Eqs. 6, 7, and 8.
Ci
Cfi = (6)
Cni
∑n Pn
Tri = × Sn (7)
n=1 C i
Eri = Tri × Cfi (8)
where Ci and Cni are concentrations of pollutant i
(microplastics) in polluted and unpolluted samples,
respectively. Tri is represented as the toxicity coeffi-
cient introduced by Håkanson (1980), indicating bio-
logical sensitivity and toxicity level. Pn refers to the
concentration of a particular polymer, whereas Sn rep-
resents the hazard score assigned to plastic polymers.
The pERI for MPs/NPs is classified into five catego-
ries. Class I is assigned when the pERI is < 10, Class
II is assigned when the pERI ranges from 10 to 100,
Class III is assigned when the pERI ranges from 101
to 1,000, Class IV is assigned when the pERI ranges
from 1000 to 10,000, and Class V is assigned when
the pERI is > 10,000. These categories correspond
to the degree of risk that polymeric pollutants pose
to ecological systems, ranging from low, moderate,
Vol.: (0123456789)
13
 189

Table 7  Overview of the risk assessment index models for environmental MPs and NPs
Type/purpose Risk type/matrix Model name Formulae Classification References

13
Vol:. (1234567890)
Health risk assessment Cancer risks pCR (plastic Carcino- pCRoralordermalorinhalation = EDI oralordermalorinhalation For pEDI, when > 1, it Christian
genic Risks) × CSF oralordermalorinhalation indicates high intake of et al., 2022
pCRt = pCRoral + pCRdermal + pCRinhalation MPs or NPs
low when < 1
Page 32 of 42

plastic Estimated Exposure from oral Pi orPmi ×RI

pEDIoral = Bw
Daily Intake ingestion
(pEDI) Exposure from dermal Pmi ×SA×dp ×ABS×ET×FE×DE×CF
pEDIdermal = Bw×AT
routes
Exposure from inhala- Pi ×PM 10 ×DAIR×PIAF×ET×FSPO×CF×ED×EF
pEDIinhalation = Bw×AT
tion routes
Contamination or accu- Marine organism plastic-Bioconcentration Pi−organismorbiota pBCf/pBSAf/ppBCf/ppB-
pBCfi = Pb−water
mulation and pollution or Accumulation fac- SAf < 1: low accumulation
load assessment tors (pBCf or pBAf) 1 ≤ pBCf/pBSAf/ppBCf/
plastic-Biota-Sediment Pi−organismorbiota ppBSAf < 3: moderate
pBSAfi = Pb−sediment accumulation
Accumulation factor
(pBSAf) 3 ≤ pBCf/pBSAf/ppBCf/
Pi−organismorbiota
ppBSAf ≤ 6: considerable
plastic polymer biota- ppBCfi = pBCf/pBSAf/ppBCf/
Bioconcentration or Pb−water
ppBSAf > 6: very highly
Accumulation factors accumulated
(ppBCf)
plastic polymer biota- Pi−organismorbiota
ppBSAfi = Pb−sediment
Sediment Accumula-
tion factor (ppBSAf)
Biota Accumulation ( )1 BALI > 1: polluted
Load Index (BALI) BALI < 1: Not polluted
BALI = ppBSAf 1 × ppBSAf 2 × ppBSAf 3 … … … ppBSAfn n
BALI = (ppBCf 1 × ppBCf 2 × ppBCf 3 … … … ppBCfn n ) 1

Exposure assessment Marine sediments Microplastics concentra- MPmass,t = MPmass,t−1 + (PLmass,t × fML × f(float,aashore,seabed) ) × (1 − weightloss) Assumptions
[ ]

tion in environmental fML around 1.75 to 4.62%

compartments PLmass,t assumed to be 4.5%
Microplastics mass MPmass,t
f
= MPmass,t−1 + (1.045 × PLmass,t × fML × f(float,aashore,seabed) ) × (1 − weightloss) Seabed
[ ] assumed to be 94%
in compartments fashore assumed to be 5%
(2017–2100) ffloat assumed to be 1%
Water Air Soil Pollut

Weight loss can vary

between 0.65 and 5%
*
pCR, plastic carcinogenic risks; EDI Estimated daily intake; PEDI Plastic-estimated daily intake; CSF Cancer slope factor; CR Cancer risk; Pmi , number of distinct MPs/NPs
polymers identified in sample i; Pi , quantity of MPs/NPs in the studied matrix (water, soil, air, food); RI, ingestion rate for water or soil; BW, average body weight; SA, skin area
available for contact; dp, pore diffusion coefficient; ABS, dermal absorption factor; ET Exposure time; CF Conversion factor; FE Frequency of exposure; DE Duration of expo-
sure; AT Averaging time; PM10, particulate matter; DAIR Daily air inhalation rate; PIAF Retention fraction of inhaled particulates in body; FSPO, fraction of soil-borne particu-
lates in air; Pb, quantity of MPs/NPs in background or reference matrix; pBCfi, plastic, bio concentration factors; pBSAfi, plastic-biota-sediment accumulation factor; ppBCfi, plas-
(2024) 235:189

tic polymer biota-bioconcentration or accumulation factors; ppBSAfi, plastic polymer biota-sediment accumulation factor; BALI, biota accumulation load index; fML , mass of the
total yearly marine litter; MPmass,t−1, mass of microplastics in compartments; PLmass,t , plastic production; fSeabed , marine litter ending up in seabed; fashore, marine litter washing up
on ashore; ffloat , free floating microplastics in water body
Water Air Soil Pollut (2024) 235:189
substantial, high, to very high. Some of the important
risk assessment models are summarized in Table 7.
Moreover, the most common ecological risk assess-
ment methods for MPs use the pollution load index
(PLI) and pollution hazard index (PHI) to assess MP
pollution levels in different regions, considering MP
abundance and polymer chemical toxicity.
Moreover, MP pollution is influenced by human
activity, and the ecological risk assessment frame-
work for MPs should take socio-economic factors into
account (Zhang et al., 2022). Pollution and risk indi-
ces are essential for assessing the contamination of
various media by MPs/NPs accurately; hence, an eco-
logical risk assessment of MPs for different environ-
mental media is the foundation for controlling plastic
pollution in the future. Model-generated data are sim-
plified representations of environmental issues, which
help policymakers comprehend environmental chal-
lenges and make more prompt and effective environ-
mental decisions. However, plastic polymers vary in
toxicity and distribution in the environmental matrix;
thus, models should be used carefully and only when
all the parameters and factors are known.
5 Future Perspectives
MPs in soil and sediments have only recently cap-
tured the attention of researchers. It is evident that
the concentration of MPs in soil, sediments, and
other matrices is poised to increase in the future as
the demand for plastics is ever-growing. Correspond-
ingly, countries are focusing on managing plastic
waste, but it is slow compared to the production rate
of plastics. Therefore, extensive studies are required
in this area to determine the scale of MPs contamina-
tion in various matrices. Several analytical techniques
are published for the assessment of MPs, but these are
non-standard methods that lack uniformity in sample
collection, extraction, and quantitation.
The disparity starts right from reporting the size
range of MPs. In many studies, the information
regarding sampling units, density separation, the type
and pore size of filter paper used, and unit of the MPs
abundance is ambiguous. These shortcomings make
comparison of the published data difficult. There-
fore, standard operating procedures (SOPs) must be
developed to bring consistency in the procedures and
to reduce the disparities while reporting the data.
Page 33 of 42 189
Stringent QA/QC measures must be implemented
during the analysis as these aid in reducing the con-
tamination of the samples, and ensuring reproducible
results. The recent development of reference materials
and inter-laboratory comparison (ILC) exercises on
MPs analysis will pave the way for developing stand-
ard methodologies and shall improve the comparabil-
ity of data (Martínez-Francés et al., 2023). It is desired
that all laboratories working in the area of MPs should
participate in ILC programs to improve data quality.
Nevertheless, this review has demonstrated that vari-
ous analytical methodologies are available and can be
used for MPs detection and quantitation. This review
has also focused on various models which would help
to estimate the ecological risks, human health risk, and
various other exposure risk assessments.
Finding solutions to limit the number of MPs and
plastics entering into the environment in the initial
place may be made possible by examining the mag-
nitude of MPs input into soils through pathways such
as compost, road runoff, and sewage sludge and MPs
input into sediments, through biofilms and gravity dep-
osition. MPs contamination in the soils and sediments
may pose environmental risk leading to public pres-
sure on decision-makers, consumers, and businesses to
take appropriate actions. Collaboration among research
institutions is paramount for developing standard meth-
ods, ILC and establishing quality control standards to
improve MPs data quality.
Acknowledgements The authors thank CSIR-National Envi-
ronmental Engineering Research Institute, Nagpur, India, for
financial assistance through intramural funding MLP-199(07).
Author Contribution Designing, conceptualization, data
collection, and data analysis were performed by AP, AD.
Review, editing, and overall supervision done by ARK. All
authors read and approved the final version of the manuscript.
Funding This work was supported by the CSIR-National
Environmental Engineering Research Institute, Nagpur, under
Grant [MLP-199].
Declarations
Ethics Approval and Consent to Participate Not applicable.
Consent for Publication Not applicable.
Competing Interests The authors declare no competing
interests.
Vol.: (0123456789)
13
 189 Page 34 of 42
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