MPs in Soil and Sediment - Paper

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 will improve the reproducibility and comparability of
review of the characterization, quantification, and results. This review calls for further research on MPs’
ecological risk assessment of microplastics (MPs) in effects on soil and sediment environments to inform
soils and sediments. MPs, defined as plastic particles standardization efforts and improve our understand-
of size smaller than 5 mm, have been less studied in ing of MPs pollution.
these environments compared to aquatic ecosystems.
Broadly, all analytical methods include the follow- Keywords Extraction · FT-IR · Microplastics ·
ing steps: sampling, extraction, polymer identifica- Raman spectroscopy · Sediment · Soil
tion, and quantitation/particle counting. This review
highlights the variation in current methodologies
for sampling, extraction, and quantification of MPs, 1 Introduction
which hinders data comparison across studies. This
poses a real challenge to compare the data of vari- Since the commercialization of plastics in the 1950s,
ous studies. Hence, there is an urgency to develop global plastic production has only grown exponentially,
standardized methodologies for analyzing MPs in and over the years, plastics have become an inevitable
different environmental matrices. Spectroscopic tech- material for humans. It is estimated that, in 2022, 21
niques such as FT-IR and Raman are the most widely million tonnes (Mt) of macroplastics (plastics larger
used techniques for polymer identification. Adopting than 5 mm) leaked into the environment globally
proper quality control and quality assurance measures 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
A. Prajapati · A. Dehal · A. R. Kumar (*)
contribution to total global greenhouse gas emissions
Chemical and Hazardous Waste Management Division,
CSIR-National Environmental Engineering Research (1.9 GtCO2 e in 2022) (OECD, 2023). Apart from
Institute, Nagpur 440020, India being cheap, plastic became widely popular due to its
e-mail: [email protected] properties such as durability, corrosion resistance, low
thermal conductivity, and lightweight (Andrady, 2011;
A. Prajapati
Rashtrasant Tukadoji Maharaj Nagpur University, Andrady and Neal, 2009; Imhof et al., 2012). A sig-
Nagpur 440033, India nificant quantity of processed and manufactured plastic
is meant for single use. In most developing countries,
A. Dehal · A. R. Kumar
these single-use plastics (SUPs) are disposed off with-
Academy of Scientific and Innovative Research (AcSIR),
Ghaziabad 201002, India out proper segregation and treatment, making SUPs
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189 Page 2 of 42 Water Air Soil Pollut (2024) 235:189
the major contributor to the municipal solid waste. Environmental Protection (GESAMP), considered
The natural degradation of plastic is very slow, and it the nano-sized particles (1 mm to 1 µm) to be MPs
takes decades to completely decompose plastic mate- (Möller et al., 2020). There is no universally accepted
rial in the environment (Hidalgo-Ruz et al., 2012). and unequivocally defined size range for MPs. The
Consequently, discarded plastics get collected in the dispersion and bioavailability of MPs in the environ-
environment over time and transported to other regions ment depend on their shape, size, density, color, and
through air, water, and wind, eventually ending up in chemical makeup. Since most plastic debris makes its
the seas (Thompson et al., 2004). Thus, plastic is omni- way from land to water bodies and eventually to sea,
present, regardless of how heavily inhabited or isolated the accumulated plastics in the ocean cause death of
a location is (Möller et al., 2020). many aquatic organisms that mistake MPs for food.
The first report to establish the evidence on marine The initial research on MPs in aquatic or marine
plastic pollution dates back to the 1970s (Carpen- environments aimed to understand MP’s occurrence,
ter and Smith, 1972). Since then, more and more abundance, fate, and impact on aquatic/marine organ-
studies have documented the widespread plastic isms. Because contamination control must happen at
contamination in different environmental matrices the source, studies on MPs got expanded to terrestrial
(Campanale et al., 2022). The most used polymers for ecosystems (Campanale et al., 2022). This is evident
plastic manufacturing and packaging are polyethylene from Fig. 2, which indicates that the number of arti-
(PE), polypropylene (PP), polystyrene (PS), poly- cles on MPs in soil and sediments increased from the
ethylene terephthalate (PET), and polyvinylchloride year 2015 onwards (Web of Science database). Plastic
(PVC) (Thompson et al., 2004). Table 1 lists the most garbage generated on land is primarily disposed of in
commonly used polymers, their properties, applica- soil or aquatic ecosystems. In the terrestrial ecosys-
tions, and hazard statement. tem, littering, surface runoff, application of biosolids,
Due to biotic and abiotic processes, discarded compost on agricultural soil, and farming methods
plastics disintegrate into diverse shapes and sizes utilizing plastics, such as mulching, expose urban and
ranging from meters to micrometers (Barnes et al., agricultural soil to MPs contamination (De Souza
2009), which can vary from > 20 mm for macroplas- Machado et al., 2018; Li et al., 2018; Liu et al., 2018).
tics, 20–5 mm for mesoplastics, < 5 mm for MPs, Due to biofouling and weathering, the density of
and < 1 µm for nanoplastics. Microplastics (MPs) MPs fluctuates over time and eventually, soil and
are plastic particles of size < 5 mm. MPs are classi- sediments become the sink for MPs (Bläsing &
fied into (1) primary MPs, which are produced for Amelung, 2018; Cunningham et al., 2020; Katare
that size as beads or pellets. They are used in per- et al., 2022). Higher-density MPs sink and accumulate
sonal care products, sand blasting (as abrasives), and in sediments, while beach sand can amass floating,
domestic cleaning agents. (2) Secondary MPs are partly buoyant, and sink plastics. MPs can also sorb
formed from the disintegration of discarded plastics and transport heavy metals, organic contaminants, and
(De Souza Machado et al., 2018). The disintegra- pathogens, making them a cocktail of contaminants
tion is induced by biological, physical, or chemical (Bayo et al., 2018; Bhagat et al., 2022). The presence
factors (Andrady, 2011). Figure 1 depicts the lifecy- of MPs can alter the chemical and physical properties
cle of plastics and MPs in soil and sediments. MPs of soil and sediments, ensuing disturbances in the
are observed in numerous shapes, for example, bead, food chain. Due to biomagnification, MPs ascend
pellet, foam, film, fragments, and fiber/filament. The along different trophic levels, causing organisms of
term MP was first introduced by Richard Thompson all the trophic levels exposed to MPs, raising food
in 2004 to refer to the microscopic plastic particles safety concerns (Rainieri & Barranco, 2019). Soil and
of size 20–2000 μm found in British beach water col- sediments are non-homogenous, hence pose challenges
umns and sediments (Thompson et al., 2004). Later, to MPs analysis. So far, no standard analytical method
the MPs size range was extended to include plastic is available to study MPs in soil or sediments. Thus,
particles of size up to 5 mm, such as pellets (Arthur the reported data on MPs in various matrices are
et al., 2009). associated with different levels of inaccuracies
Professional bodies, such as the Joint Group (Hidalgo-Ruz et al., 2012; Zhang & Liu, 2018).
of Experts on Scientific Aspects of Marine
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Table 1 List of commonly used polymers with their properties, applications, and hazard statement
Sl. no Polymer type Density (g/cm3) Crystallinity Polarity Uses Hazard statement
Water Air Soil Pollut
1 High-density polyethylene 0.94–0.97 70–95% Non-polar Plastic bottles, toys, chemical containers, Extremely flammable gas
pipes May cause drowsiness or dizziness
2 Low-density polyethylene 0.91–0.93 45–60% Non-polar Milk cartons, utensils, plastic bags, wire Extremely flammable gas
insulation May cause drowsiness or dizziness
3 Polyvinyl chloride 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
4 Polypropylene 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
5 Polyethylene terephthalate 1.34–1.39 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
6 Polystyrene 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
7 Polycarbonate 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
8 Polyurethane 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
9 Polyamide 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
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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 on water holding capacity and soil porosity (Wang et al.,
Environment 2023); hydraulic conductivity, and soil particle size dis-
tribution (Jing et al., 2023). MPs also tend to reduce the
MPs in soils affect soil structure and reduce infiltra- concentrations of PO43– and NH4+ in leachate water
tion rate of soils; besides, they cause a negative impact posing a serious threat to soil biota (Guo et al., 2023;
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Water Air Soil Pollut (2024) 235:189 Page 5 of 42 189
Kiran et al., 2022). MPs run off in the soil causes bio- plastic residues, which are transformed into MPs over
turbation (Hurley & Nizzetto, 2018). If MPs are present time and through environmental factors. These MPs
in high quantities, they clog and obstruct soil pores, thus scatter in the soil and adhere to other pollutants such
reducing soil infiltration capacity. This will disrupt the as persistent organic pollutants (POPs), heavy metals,
nutrient cycles in the soil, change the microbial com- and pesticides.
munity, and eventually negatively impact plant growth According to Li et al., (2023) and Rochman,
(Dong et al., 2021; Lwanga et al., 2022). Soils also (2018), sediments appear to be a long-term sink for
functions as a sink for MPs, and recent researches are MPs. The phenomenon of biofouling involves organ-
focused on how MPs affect the soil ecosystem (Wang isms colonizing on the surface of plastic particles by
et al., 2023; Jing et al., 2023). Figure 3 shows typical MP secreting organic matrices, which is facilitated by the
particles found in soil samples (Unpublished results). hydrophobic nature of the plastic. The swift absorp-
Several studies (Chua et al., 2014; Avio et al., tion of organic compounds leads to the formation of
2015) have revealed the vector property of MPs, a "conditioning film," enabling the beginning of a
i.e., carriers of harmful chemical pollutants in the biological process. It begins with the colonization of
soil matrix. Some of the commonly used additives/ bacteria and progresses to the attachment of micro-
chemical pollutants in plastics include polychlorin- algae and, potentially, various invertebrate groups
ated biphenyls (PCBs), phthalates, nonylphenol, poly- (Artham et al., 2009; Fazey & Ryan, 2016). Several
fluorinated alkyl substances (PFAS), Polyaromatic other studies also highlighted the emergence of MPs
hydrocarbons (PAHs), UV-stabilizers, and bromi- in sediments, the buildup of biofilms, and the accu-
nated flame retardants such as polybrominated diphe- mulation and adsorption of pollutants (Kooi et al.,
nyl ethers (PBDEs) (Chakraborty et al., 2022; Praja- 2017; Xiong et al., 2022).
pati et al., 2022). The important reservoirs for MPs From the MPs analytical perspective, soils and
are thought to be urban and agricultural soils (Hurley sediments are complex matrices. The specific fac-
& Nizzetto, 2018). Mulching processes leave behind tors that influence these complexities have not
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)
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been discussed in detail (Campanale et al., 2022; appropriate sample location can significantly influ-
Cao et al., 2021; Dong et al., 2021). However, few ence the total MPs content in a particular location;
reviews report the MPs pollution in beach sand and hence this is a crucial step in the overall analytical
sediments and focus on particular geographic areas method (Liu et al., 2018). According to the European
such as Latin America and the Caribbean, the Asian Commission’s Marine Strategy Framework Directive
coast and the Mediterranean region (Curren et al., (MSFD) guidelines, the number of sampling sites
2021; Grillo et al., 2022). These reviews mainly that must be used to represent a particular region is
concentrate on the quantification, the available ana- unrestricted, but enough replicas must be collected
lytical standards and the guidelines for MP analysis, to address the non-uniformity of the chosen region
rather than the analytical methods employed. Other to generate representative samples. The survey area
review articles examine the migration and the behav- should be appropriately defined as this determines
ior of MPs and MP additives (Li et al., 2023; Luo how many samples must be collected to obtain useful
et al., 2022b), and others evaluate the effect of the information regarding the sampling site.
extraction methods used, sometimes even highlight-
ing one specific protocol such as density separation 3.1.1 Soil Sampling
and the use of different salts (Cutroneo et al., 2021)
or the assessment and the degradation of MPs in the Single-site/grab sampling or composite sampling
environment to determine if these methods are eco- may be adopted depending on the sampling site and
friendly or not (Kasmuri et al. 2021). Moreover, no objectives of the investigation (Möller et al., 2020;
review has been published since 2017 that exclu- Zhou et al., 2018). Composite sampling is preferred
sively focuses on the state-of-the-art in the analysis for agricultural soil sampling, as this soil undergoes
of MPs in soils and sediments, especially matrix spe- regular alterations due to farming and soil condition-
cific challenges and guidance on how to deal with ing. Single-site sampling is appropriate for soil that
them. is exposed to fewer human activities. Sampling tools
This review discusses the analytical methods for used include stainless steel spade, soil auger (Corra-
the determination of MPs in soils and sediments. dini et al., 2021; van den Berg et al., 2020), shovel
We cover the latest developments in the methodolo- (Liu et al., 2018; Zhou et al., 2018), corer (Crossman
gies (during the last 5 years) for the separation and et al., 2020; Helcoski et al., 2020), and lenz sam-
the extraction of MPs, as well as the innovative ana- pler (Lv et al., 2019). Handpicking using a tweezer/
lytical tools that are used for their identification and forceps can also be used in cases where the MPs are
quantification with the emphasis on standardization distinguishable from the rest of the matrix (Gwin-
of analytical protocols and results reporting. Table 2 nett et al., 2021). Soil samples can be collected from
summarizes typical studies on MPs abundance in dif- small sampling units called quadrats of dimensions of
ferent soil and sediment samples. 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
3 Analytical Methods happening in an area can be used to determine sam-
pling depth. According to various studies, the sam-
The general analytical scheme followed for MPs anal- pling depth may range between 0 and 30 cm (depend-
ysis in soil and sediment samples is given in Fig. 4. ing on tilling depth) (Cooper & Corcoran, 2010;
Often, the complexity of samples and the objectives Browne et al., 2011 Yang et al., 2018). Non-agri-
of the study necessitates additional steps for the cultural soil will have a relatively shallow sampling
extraction and purification of MPs. depth than agricultural soil, typically 5 cm. Other
soils are sampled at a shallower depth of less than
3.1 Soil and Sediment Sample Collection 5 cm. Stratified sampling is preferred to determine the
depth of pollution within the soil profile. If the ver-
The acquisition of the environmental sample is tical distribution of MPs needs to be examined after
the first step in the analytical procedure. A suit- cultivation, sampling depth should be varied depend-
able sample site must be chosen, as the choice of an ing on the type of cultivation (Bläsing & Amelung,
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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
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
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microplas-
tics in the
soils
189
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Table 2 (continued)
189
method
13
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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-
tigate the
potential
effects of
microplas-
tics on crop
growth or
soil health
(2024) 235:189
Table 2 (continued)
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
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
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locations or
methods
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Table 2 (continued)
189
method
13
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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
(2024) 235:189
Table 2 (continued)
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.,
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
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Table 2 (continued)
189
method
13
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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
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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
insights into
microplastic
pollution in
freshwater
systems,
which is
less studied
compared to
marine envi-
(2024) 235:189
ronments
Table 2 (continued)
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.,
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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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 properties (Möller et al., 2020). Collected samples
should always be higher than required for the analy- should be stored in stainless steel containers or glass
sis, as these samples can be used as laboratory control bottles. Care must be taken to avoid the interaction of
samples or for repetition and determination of soil the sample with any plastic tool or surroundings that
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Table 3 Sampling methods for soils and sediments
Soil sampling Sediment sampling
Type of method Description Type of method Description
Simple random sampling The sampling points are chosen randomly under the Shore sediment sampling Multiple transects at a right angle from the water line and
premise that each point has an equal chance of being the placement of quadrats along the transects. Transects
selected. The method is feasible to implement, and may be visually scanned for bigger microplastics in the
focuses on specific sampling zones field. The surface layer can be removed to a proximate
depth and sieved or transferred to the laboratory for
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subsequent steps
Systematic grid sampling It is the distribution of sampling points along the nodes Sediment manual grab methods Utilize tools such as hand spades and stainless steel spoon
of a regular pattern. First point is selected at random for littoral and beach environments
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 Deeper sediment sampling Deep sediment sampling provides data on the change of
method. Points are chosen on regular intervals along MP’s abundance and other characteristics spanning a
one or more straight lines century to present day. Some examples are Ekman and
Van Veen grab samplers
Unaligned grid sampling This sampling technique combines the benefits of ran- Point integration method A sampler is lowered to stream at a specific point where
dom sampling and systematic grid sampling. Sampling the sediment should be collected
points are situated randomly within the grid compart-
ments
Stratified sampling In this sampling method, the sampling area is divide into Depth integration method In this method, suspended sediment is iso-kinetically
smaller compartments known as strata. The contamina- collected by lowering and raising a sampler in a constant
tion within each stratum is homogeneously distributed transit rate in a stream. Depth integration is done either
than in the sampling site as whole by Equal Discharge Integration (EDI) method or by
Equal Width Increment (EWI) method
Judgmental sampling Judgemental sampling is based on the expert information Bed materials sampling Most commonly used methods for bed material sampling
for example historical utilization, visual inspection. It are grab sampling, dredge sampling, and core sampling
is simple to implement but is biased and may only be for example Van Veen, Smith-Mclntyre, Ponar, Peterson,
suitable for studies which focuses on sampling zones orange peel bucket, Birge-Ekman, and Shipek are most
like hollows 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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◂Fig. 5 Sampling techniques, density separation, extraction, bias and misidentification; hence warrants care while
and analysis methods for microplastics found in a soils and b sampling.
sediment sample (2018–2022) (n = 25)
Sieving is commonly used for volume reduction.
Sediments present on the river bank can be sampled
are exposed to plastic contamination. Table 3 shows with the help of shovels, spoons, trowels, spatula etc.
various sampling techniques for soil samples. Obtain- (Eo et al., 2019; Horton et al., 2017; Lenaker et al.,
ing a representative soil sample is always challenging 2019; Sarkar et al., 2019). In contrast, sediments from
due to the heterogeneous nature of soil MPs distribu- the riverbed can be collected using Van Veen grab
tion; hence, a sufficiently large quantity of samples is sampler, drill corers, sediments corer, Petite Ponar
required (Corradini et al., 2021). Various sampling, Grab, peterson grab, Ekman dredge sampler etc.
extraction, and identifications used for MPs are given (Castañeda et al., 2014; Crew et al., 2020; He et al.,
in Fig. 5. 2020; Rao et al., 2020). Two recent approaches for
collecting undisturbed sediment sampling include
“diving bell vessel” of Mani et al., (2019), and “freeze
3.1.2 Sediment Sampling core sampling” of Frei et al., (2019). However, these
procedures are feasible for research but may pose
The first step in sediment sampling is to identify a challenges for monitoring programs. Generally, sam-
suitable sampling location based on which the samples are kept in glass or stainless-steel containers to
pling approach is decided. When sampling a beach evade plastic contamination. Table 3 shows various
site, transects are commonly used, with quadrats of sampling methods adopted for sediment samples.
variable dimensions. At least two transects (50 m
apart) should be defined in each sampling area, and 3.2 Extraction of MPs from the Sample
their placement should be set to reflect the whole
site. It is a widely observed practice to place the Once the samples are brought to the laboratory, pre-
transects along the strandline as this region contains liminary sample processing, such as sieving or hand-
more MPs. However, this approach is likely to pro- picking, is adopted to remove larger particles. Fol-
duce biased results (Mendoza et al., 2021). The quad- lowing sieving, the required quantity of samples is
rats are assigned inside the transects, and the repli- weighed accurately and dried in an oven at < 70 ◦ C
cate samples are taken (at least 5 m apart). In beach to remove moisture. However, the drying tempera-
sediments, MP’s vertical distribution is influenced ture and duration depend on the moisture content and
by the movement of air and water or physical activi- sample characteristics, for example, reported temper-
ties; hence, samples must be collected from different ature for drying ranged from 50 to 90 ℃ for 24 h or
depths (Browne et al., 2011; Cooper & Corcoran, overnight (Hossain et al., 2021; Liu et al., 2018; Paes
2010). Studies given in Table 3 have employed differ- et al., 2022). In some cases, air drying method have
ent sampling depths, ranging from 0 to 32 cm. been used to reduce moisture (Fakour et al., 2021;
Bulk, selective, and volume-reduced sampling Weber et al., 2023). But, drying temperatures > 70 ℃
are different types of sampling procedures. Bulk for longer time periods may result in surface modi-
sampling is the collection of the entire sample vol- fication of MPs (Munno et al., 2018), which is rec-
ume without any previous reduction. Bulk samples ommended by authors too. The next step is the sepa-
are the preferred choice when visual identification ration of MPs from the bulk matrix, which includes
of MPs becomes challenging due to low abundance density separation, filtration, sieving, and visual sort-
requiring large volumes of water or sediments or ing. Because of the complexity of soil and sediment
their small size making them tough to detect with the samples, selecting a suitable separation procedure is
naked eye. Selective sampling is considered when challenging, especially when the particle size of the
MPs can be identified with the naked eye, and this soil/sediment and the MPs decreases (Peng et al.,
strategy is more prominent with sediment surfaces. 2017). Both soil and sediments generate aggregates
This method is only suitable for particles of size that could trap MPs; hence, the approach chosen
1–5 mm and is not preferred when additional debris must effectively disperse the aggregates without trig-
adheres to MPs. Therefore, this approach is prone to gering the fragmentation of MPs (Fries et al., 2013;
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Li et al., 2018). The Munich Plastic Sediment Sepa- (KOH, 10% 60 °C, 24 h) has yielded better recover-
rator (MPSS), developed by Imhof et al., (2012), is ies of MPs from biological matrices. (Dehaut et al.,
a highly efficient tool for extracting MPs from sedi- 2016; Zou et al., 2019). However, it is important to
ments based on density separation (Rocha-Santos & note that strong acids or alkaline digestion solutions
Duarte, 2015; Löder et al., 2015). The extraction effi- may lead to varying degrees of MPs degradation
ciency of MPSS for larger MP particles (1 to 5 mm) (Enders et al., 2019; Munno et al., 2018). Zou et al.,
and smaller particles (< 1 mm) were 100 and 95.5%, (2019) compared the extraction efficiencies of the six
respectively. Additionally, the MPSS demonstrates most commonly used digestion reagents to extract
the capability to extract MPs from large volume of PS-MPs from biological samples and found that KOH
sediment samples, i.e., 5–6 kg of sediment in a single digestion did not affect the surface morphology and
operation. Furthermore, the Sediment-Microplastic had the least impact on PS’s fluorescence intensity.
Isolation (SMI) unit offers a convenient and portable However, all other digestion procedures ( HNO3: HCl,
solution for extracting MPs from diverse sediment NaOH, HNO3, H2O2, and H NO3:HClO4) caused PS’s
types with a recovery rate of 95.8% in a single step surface to aggregate, bubble, scratch, and depressed,
(Coppock et al., 2017). as well as to diminish its fluorescence intensity to
Another recently designed technique is the com- varying degrees (Zou et al., 2019).
pact glass, Japan agency microplastic-sediment sepa- Several researchers have used hydrogen perox-
rator (JAMSS). The JAMSS comprises two parts: ide oxidation (HPO) to remove organic matter from
a lower and upper modified glass plate. When the different types of samples, such as water (Wang
two plates are used together, the lower container and et al., 2017a, b), soil (Wang et al., 2021), sediment
upper tube form a single, cylindrical container into (Ding et al., 2019), sludge (Li et al., 2018), and ani-
which the sample can be poured. The plates can then mal tissues (Lv et al., 2019). However, the reaction
be slid against each other to separate the lower and time, reaction temperature, and H 2O2 concentration
upper halves of the sample by introducing a lid and employed in the digestion procedures varied widely.
bottom (the glass plate) to each half. The recovery For example, Liu et al., (2018) utilized 30% H2O2 for
rates for MPs < 1000 µm size are 94.0–97.8% (Naka- 24 h at 70 °C to remove soil organic matter, whereas
jima et al., 2019), which is close to the previously Ding et al., (2020) used the same concentration of
developed separators such as MPSS (Imhof et al., H2O2 at 65 °C for 72 h. Different reaction conditions
2012) and SMI (Coppock et al., 2017). All the units may be required depending on factors such as sam-
were tested with actual field sediment samples to pling site, soil type, and organic matter concentration;
understand the recovery rates. JAMSS can be proven however, strong reaction conditions may cause par-
to one of efficient system to separate MPs from soils ticular types of MPs to degrade or even discolor or
and sediments. fragment (Prata et al., 2019). It has been demonstrated
that when 70% H 2O2 is used at 70 °C, 96–108% of
3.2.1 Digestion the organic matter in loamy-sandy soil is destroyed,
with the concomitant degradation of Polyamide (PA)
Alkali and Acid Strong acids, e.g., perchloric acid, and PS MPs (Hurley et al., 2018). Temperature plays
nitric acid, and hydrochloric acid, and strong bases, a significant role in the degradation of polymers
e.g., potassium hydroxide and sodium hydroxide, (Luo et al., 2022a). Tang et al., (2018) demonstrated
have been employed for digestion to remove organic that PVC placed in an oven at 50 °C did not show
matter from MPs (Zou et al., 2019; Scheurer and any changes in FT-IR spectra, whereas PVC kept at
Bigalke, 2018; Munno et al., 2018). However, the 100 °C showed new absorption peaks after 9, 25, 45,
analytical results may show wide variation depending and 83 days. Treatment of PE and PP with 30–35%
on the rigor of the digestion procedure. For example, H2O2 at room temperature for 7 days decreased the
Cole et al., (2014) examined the usage of NaOH and MPs by about 17% (Nuelle et al., 2014). Therefore,
HCl for separation MPs from organic-rich marine the digestion conditions must be selected carefully. It
species and seawater samples and observed that 1 M is suggested that Fenton’s reagent, rather than H2O2
NaOH provided better recovery (90.0 ± 2.9%) than alone, below 40 °C is more efficient in organic matter
2 M HCl (72.1 ± 9.2%). Similarly, alkaline digestion removal from MPs in soil samples (Cao et al., 2021;
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Hurley et al., 2018). Table 2 provides more details on 3.2.2 Separation of Microplastics from Matrix
different digestion methods, nature of soil samples,
polumer types, and other details. Density Separation An aliquot of soil/sediment is
added to high-density salt solutions; thereby, MPs are
Enzymatic Digestion Enzymatic digestion gener- made to float, i.e., density separation. This step helps
ally destroys organic matter in soil, biological and to separate MPs from the matrix; however, some non-
wastewater samples (Löder et al., 2017; Mbachu plastic particles are also likely to float if present in the
et al., 2021). Löder et al., (2017) reported the basic sample. In the beginning of MPs research, a saturated
enzymatic purification protocol (BEPP) to remove NaCl solution (0.8–1.4 g/mL) was used (Möller et al.,
organic substances from various environmental sam- 2022). Whereas high-density polymers such as PLA
ples, such as water, biota, sediment, and food. The (1.32 g/mL), PBT (polybutylene terephthalate) (1.34–
BEPP procedure focuses on three specific enzymatic 1.39 g/mL), PET (1.5 g/mL), PVC ( 1.58 g/mL)
reactions: protease, cellulase, and chitinase. An ini- require salt solutions such as NaI (ρ = 1.8 g cm–3)
tial incubation with sodium dodecyl sulfate (SDS) (Coppock et al., 2017; Stock et al., 2019), Na2WO4
and H2O2 treatment is employed to extract MPs from (ρ = 1.4 g cm–3) (Frias et al., 2018), ZnCl2 (ρ = 1.6–
environmental samples. Similarly, Mintenig et al., 1.7 g cm–3) (Coppock et al., 2017; Masura et al.,
(2017) successfully extracted and purified MPs from 2015a, b), and NaBr (ρ = 1.55 g cm–3) (Frias et al.,
treated wastewater using enzymatic reactions, includ- 2018; Kedzierski et al., 2017). For extraction of MPs
ing lipase, protease, and cellulose. Enzymatic diges- from soil, CaCl2 solution has been used by Li et al.,
tion has proven to be an effective, selective, and mild (2019) as Ca2+ act as a bridge between organic mol-
method, making it a potentially useful technique for ecules’ positive and negative charges, making it eas-
removing soil organic matter and extracting MPs ier to separate soil organic material. Table 4 lists the
(Railo et al., 2018; von Friesen et al., 2019). Cao commonly used salts for the density separation pro-
et al., (2021) demonstrated that combining proteases, cess with their merits and demerits. Almost all studies
lipases, cellulases, hemi-cellulases, oxidant sample employ density separation as a simple way to separate
pretreatment, and density separation could efficiently MPs, either in a single step or a double-step utilizing
reduce up to 90% of the organic matter in soil sam- low-density and high-density solutions consecutively.
ples. Möller et al., (2022) studied the effect of enzy- Although the two-step extraction is reported to yield
matic oxidative digestion methods (protease, pecti- higher recoveries, most studies employ a single-step
nase, viscozyme L, and cellulase) with various MPs extraction using a salt solution of density > 1.4 (Zhao
such as polylactic acid (PLA), PE, PVC, PET. Except et al., 2017 and Nuelle et al., 2014). Even though NaI
for PLA, the remaining MPs were unaffected by and ZnCl2 solutions have high density, the recovery
enzymatic digestion, and the organic matter removal and recycling of these solutions are difficult due to
efficiency was 77%. PLA showed evidence of deg- their toxic and corrosive nature. However, most of
radation and a decreased molecular weight distribu- the studies reported only one-step density separation
tion after protease treatment (Möller et al., 2022). method, i.e., after digestion as reported by Paes et al.,
López-Rosales et al., (2021) analyzed MPs recoveries (2022) and Rezaei et al., (2022) which is recom-
with various methods of digestion and found that the mended by the authors too.
enzymatic treatment showed unaltered plastics parti-
cles and good recoveries for tested polymers (> 81%), 3.2.3 Filtration
which is comparable to the oxidation approach
(recovery > 83%). Despite these merits, enzymatic Sieving can be repeated after density separation to
digestion for soils and sediments has received rela- separate bigger plastic particles if necessary. Based
tively little attention since it requires more time and/ on the mesh size employed, sieving also aids in deter-
or is costlier than other digestion techniques (Cao mining the particle size. Following sieving, vacuum
et al., 2021; Tirkey and Upadhyay, 2021). In case of filtration isolates the MPs from the supernatant solu-
extraction process, authors suggest using H 2O2 and tion. The filtration is carried out using a filter paper of
fentons reagent together for better recovery. 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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189
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

levels can inhibit growth of
aquatic species
2 Calcium chloride (CaCl2) 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
3 Sodium bromide (NaBr) 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
4 Sodium tungstate dihydrate 1.4 Minor severity of hazard Low potential to affect aquatic $ 223.16/500 g Pagter et al., 2020
(Na2WO4.2H2O) life as it has no BOD
5 Monosodium phosphate 1.4–1.45 May cause skin and serious eye Reacts slowly on exposure $ 91.75/500 g Zhang et al., 2018
(NaH2PO4) irritation to (moisture) with (some)
metals. On burning: release
of toxic and corrosive gases/
vapors (phosphorus oxides)
6 Sodium polytungstate 1.4–1.65 Expensive, hazardous Causes harmful effect on $ 233.43/100 g Cunningham et al., 2020
3Na2WO4.9WO3.H2O aquatic life, fire, and spillage
in water can also cause pollu-
tion of watercourses
7 Lithium metatungstate 1.62 Non-hazardous It is not toxic to the aquatic $ 115.59/25 g Masura et al., 2015a, b; Quinn
(Li2WO4) environment et al., 2017
8 Zinc bromide ( ZnBr2) 1.7 Higher recovery rate, hazardous Chronic aquatic toxicity $ 164.70/500 g Quinn et al., 2017
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
paper (Sørensen et al., 2021). A wide range of diam- Another way for visual identification using the
eters (25 to 125 mm) and pore sizes (0.2 to 5 µm) of stereomicroscope is to stain the sample, in which a
filter papers have been reported for MPs filtration lipophilic dye (e.g., Nile Red) selectively stains the
(Hidalgo-Ruz et al., 2012; Maes et al., 2017; Claes- MP particles, which can then be analyzed based on
sens et al., 2011; Frias et al., 2010; Crichton et al., their fluorescence (Maes et al., 2017). However, the
2017). Filter papers that are commonly used include efficiency of this approach for soil and sediment sam-
silicon membrane, glass fiber (GF), nitrocellulose and ples is debatable because, given the complexity of the
polytetrafluoroethylene (PTFE) filters. The type of matrix, other lipophilic detritus present in the sam-
filter paper used for MPs characterization may vary ple has the probability of absorbing the dye, adding
based on the instrumental technique used. For exam- difficulty to the identification of MPs (Möller et al.,
ple, optical microscopy-based techniques employ GF 2020). Quantitation is done by manually counting
or nitrocellulose filters, whereas for automated imag- the MPs in a unit area (1 × 1 cm) of the filter paper
ing with IR spectroscopy, reflective or IR transparent and then extrapolating it to the entire area. The dis-
filter papers such as silica, alumina, silver oxide are advantage of this method is that it is very susceptible
used. In the case of mass spectroscopy approaches, to error and false identifications, leading to inaccurate
the filter paper should not interfere with the plastic observations. Integrating microscopy with spectros-
signal; therefore, glass fiber filter paper is suitable for copy is useful in confirming the presence of MPs, as
pyrolysis gas chromatography/mass spectroscopy (pyr in the latter, identification is based on the polymer
GC–MS). Table 5 gives details of the various types of type.
filter papers, pore sizes, characteristics, specific appli-
cations, and approximate cost. 3.3.2 Chromatography
When combined with additional approaches, chro-

3.3 Identification and Quantitation
matographic techniques can provide quantitative
and qualitative identification of different polymers.
Various analytical methods are used to identify poly-
Several studies have utilized methods such as sol-
mer types, including visual sorting with the help of
vent extraction with size exclusion chromatography
the naked eye or microscope, pyr-GC–MS, and ther-
(SEC), Pyr GC–MS (Dekiff et al., 2014; Fries et al.,
mogravimetric and spectroscopic techniques such
2013; Hendrickson et al., 2018), and Pyr GC–MS
as Raman or Fourier transform infrared (FT-IR)
with attenuated total reflectance-Fourier transform-
spectroscopy.
infrared (ATR-FT-IR) spectroscopy (Dümichen et al.,
2017; Fischer & Scholz-Böttcher, 2017; Löder et al.,
3.3.1 Visual Identification and Counting 2015). However, the practical efficiency of these
approaches is limited due to the small pyrolysis cap-
An optical microscope or stereomicroscope is the sule size and sample amount per run, in addition
most common technique used for MP’s identifica- to the extensive sample clean-up required in the case
tion and quantitation. This method is reported to of high-volume samples (Peñalver et al., 2020). This
have error rates ranging from 20 to 70% (Song et al., renders the procedure to be extremely time-consum-
2015). This could be overcome by using a stereomi- ing and ineffective for bulk samples. These drawbacks
croscope in conjunction with spectroscopic tech- are overcome in the technique thermal extraction
niques that are capable of distinguishing MPs from desorption-gas chromatography-mass spectrometry
the rest of the sample. These include the “hot needle (TED-GC–MS) in which the gaseous degradation
test,” or comparing microscopic images of the sample products are trapped in a solid phase and analyzed by
before and after heating. This procedure leads to the GC–MS. Apart from sample grinding and mixing to
disintegration of MPs and hence helps in the identifi- achieve homogeneity, this procedure does not require
cation of MPs. However, these techniques are also not much sample pre-treatment. Compared to other meth-
error-free and come under destructive analytical tech- ods, TED-GC–MS can handle more samples and
niques where the sample cannot be recovered after- takes less run time. However, the drawback is that it
wards for further analysis. 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
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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,
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)
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,
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
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13
Table 5 (continued)
189
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
(2024) 235:189
cannot be recovered after the analysis, which results it feasible to produce spatial chemical images of a
in the loss of information about the morphology and sample based on its Raman spectra. Theoretically,
number of MP particles (Naji et al., 2019). µ-Raman imaging could enable a spectral analysis
of complete membrane filters at a spatial resolution
3.3.3 µ‑FT‑IR and µ‑Raman Spectroscopy below 1 µm, enabling to detect NPs (nanoplastics) in
environmental samples. However, µ-Raman spectros-
Micro-FT-IR spectroscopy (µ-FT-IR) is an ana- copy is less widely used than FT-IR.
lytical tool which combines FT-IR spectroscopy The spectroscopic methods used for analyzing
with microscopy. The µ-FT-IR has high spatial MPs have limited spatial resolution due to the dif-
resolution; hence, infrared bands can be identified fraction limit of light. For instance, μ-FT-IR spec-
and compared with smaller samples. The µ-FT-IR troscopy is restricted to about 10 μm, while μ-Raman
includes an objective lens for viewing MP particles spectroscopy is limited to about 300 nm. This enables
and an infrared probe for identifying and quantify- μ-Raman spectroscopy for the analysis of nearly all
ing MPs (Birch et al., 2020; Harrison et al., 2012; sizes of MPs. However, combining confocal opti-
Zhou et al., 2018). The analysis conducted has cal microscopy with Raman spectroscopy (known as
a spatial resolution that is limited by diffraction. μ-Raman spectroscopy) and utilizing visible-range
Theoretically, it is about 1.7 μm at 4000 cm–1 and excitation lasers can lead to a much better spatial res-
13 μm at 500 cm–1. The lower size range of parti- olution of 1 μm or even below ≈300 nm, compared
cles that can be identified without ambiguity is with µ-FT-IR spectroscopy. Therefore, μ-Raman
10–20 μm (Cabernard et al., 2018; Löder et al., spectroscopy is best suited for the analysis of NPs
2015; Mintenig et al., 2019; Primpke et al., 2020; (Anger et al., 2018; Ivleva et al., (2017).
Simon et al., 2018). The sample preparation is
minimal and is useful for the direct identification 3.3.4 FT‑IR and Raman Spectroscopy
of MPs (< 500 μm) on membrane filters (Harrison
et al., 2012). The technique of μ-FT-IR can be car- Spectroscopic identification of polymers is most
ried out using either reflectance or transmission reliable as it identifies the chemical makeup of an
mode. The transmission mode yields spectra of high unknown polymer by comparing the spectra of known
quality; however, it necessitates the use of infrared- polymers with that of unknowns (Naji et al., 2019).
transparent substrates. On the other hand, the reflec- Raman spectroscopy (Bläsing & Amelung, 2018) and
tance mode allows for the quick analysis of thick FT-IR are the two common vibrational spectroscopic
and opaque samples and is particularly effective techniques employed for MP analysis (Hendrick-
in detecting MPs in environmental samples (Ojeda son et al., 2018; Käppler et al., 2016; Zhang & Liu,
et al., 2009; Wenning et al., 2002). 2018). Both procedures analyze MPs over the surface
The μ-FT-IR is used widely to characterize MPs of the filter paper; therefore, MPs must be cleaned
in different matrices, for example, marine organisms appropriately to avoid any adhering contaminants
(Zhang et al., 2020), sediment (Harrison et al., 2012; interfering with the sample spectrum, which reduces
Peng et al., 2017), food (Li et al., 2018) and surface the sample amount that can be used per assay. Tra-
water (Wu et al., 2020). This technique is valuable for ditional FT-IR can be used to identify large plastic
its ability to gather data with spatial resolution and particles, whereas ATR-FT-IR can be used to exam-
for its usefulness in analyzing intricate samples. For ine MPs of size greater than 500 μm (James et al.,
example, in one study by Zhang et al., (2019) on MPs 2022). The focal plane array (FPA) based micro-FT-
pollution in surface sediments of Sishili Bay, eight IR (Löder et al., 2015) best identifies MPs of size less
types of polymers such as PP, rayon, PE, PA, PMMA, than 500 μm. Transmittance, reflectance, and ATR
PET, PS, and PU were identified using μ-FT-IR modes are among the different FT-IR modes that can
method. be used for MP analysis. Transmission mode involves
Micro-Raman spectroscopy identifies diverse size sample preparation when using thick and opaque
classes of plastic particles, including those smaller MPs, and this is done to allow IR radiation to pass
than 1 µm (Cole et al., 2014). Combining Raman through the sample. Samples with irregular surfaces
microscopy with Raman spectral imaging makes
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produce an irregular spectrum in reflectance mode, the study rather than their performance (Möller et al.,
indicating deterioration. 2020). Peez et al., (2019) have presented a new meth-
FT-IR has proven to be a highly useful method odology for size-independent MPs analysis, such as
for examining the chemical changes in particle sur- model samples of PE particles, PS beads, and PET
faces caused by weathering/aging. Typically, one can fibers using quantitative Proton nuclear magnetic
observe the emergence of new absorption bands asso- resonance (1H NMR) spectroscopy. The approach
ciated with OH, C═O, and COOH groups. Molecular is said to be inexpensive and quick. Still, all organic
mapping of MPs using FPA-based imaging is useful matter must be removed from the sample to prevent
for studying morphological characteristics where, signal overlays. The 1H NMR approach is considered
characteristic spectra of the sample will depend on inadequate for MPs detection in soil samples because
the type of bonds in the particles, which aids in differ- removing 100% of organic matter from soil samples
entiating MPs from the rest of the sample. The extent is impossible without affecting and damaging MPs
of weathering on the plastic can also be determined (Möller et al., 2020).
based on changes in chemical bond structures. A
study by Fan et al., (2021) on MPs constituent iden- 3.3.5 Scanning Electron Microscopy
tification from admixtures using FT-IR revealed that
the characteristic wavenumbers for common polymers Scanning electron microscopy (SEM) is one of the
such as PET are 793 cm−1, PE are 1472 cm−1 and useful techniques for obtaining morphological char-
1462 cm−1, PP 841 cm−1, PVC 712 cm−1, and nylon acteristics of MPs (Reddy et al., 2006; Wagner et al.,
3925 cm−1. Only a few wavelengths in the obtained 2019). Generally, SEM is combined with energy-
spectrum contain relevant information for the iden- dispersive X-ray (EDX) technology, which provides
tification polymer type in MPs; hence, manual inter- information about the elemental composition of mate-
ventions are required to minimize error rates. To rials’ micro-areas (Wagner et al., 2014; Zhao et al.,
overcome this limitation, the curve fitting approach 2017). The advantage of SEM–EDX is it gives both
is used where only the most important bands in the the elemental composition and surface morphol-
spectrum are used to find a match. This method ogy of MPs simultaneously (Eriksen et al., 2013,
improved accuracy ranging from 60 to 99%. Van Cauwenberghe et al., 2015, Fries et al., 2013).
Raman imaging takes longer than FT-IR imaging Despite being commonly perceived as an expensive
as the sample run time is longer in the former; how- method, SEM–EDX analysis requires little time for
ever, the result of µ-FT-IR imaging is reliant on the analysis as compared to other microscopic techniques
size, shape, and thickness of the analyte particles, (Table 6). When characterizing MPs, environmental
whereas Raman imaging is independent of the mor- SEM mode can be used to avoid introducing nitro-
phology of the particles. Fuller & Gautam, (2016) gen gas into the SEM chamber. Additionally, sputter-
employed a novel method viz. pressurized fluid ing carbon or gold on the sample surface is required
extraction (PFE) to isolate MPs from the soil matrix to obtain high-resolution images. Many studies have
through selective dissolution of MPs. This poly- utilized conventional SEM to observe MPs in various
mer–solvent mixture was then vaporized and ana- matrices such as sand (Tiwari et al., 2019), mussels
lyzed by ATR-FT-IR spectroscopy (Fuller & Gautam, (Li et al., 2018), sewage sludge (Mahon et al., 2017),
2016). The advantages of this method are its speed, and sediments (Neto et al., 2019; Shruti et al., 2019;
independent of particle size, and less sample prepara- Wang & Wang, 2018).
tion time. It is important to understand that SEM method
Apart from spectroscopic techniques, another involves extensive time and effort in preparing sam-
method of MPs identification is differential scanning ples, making them impractical for analyzing large
calorimeter (DSC) (El-Sayed et al., 2022). Because numbers of particles needed for comprehensive stud-
both Raman and FT-IR are very effective techniques ies. Nevertheless, these techniques offer significant
for analyzing MPs, the decision to use one over the insights into particle morphology and elemental com-
other is usually determined depending on the goal of position, facilitating comprehensive analysis of MPs.
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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
calculated
FT-IR ATR-FT-IR can evaluate particles larger FT-IR such as focal plane array FT-IR FTIR has limitations to examine wet sam-
than 500 mm, and microscope coupled (FPA-FT-IR), micro-FT-IR (μ-FTIR), ples. ATR-FTIR needs the probe to make
FTIR can study MPs smaller than 20 mm and attenuated total reflectance FTIR contact and pressure with the target mate-
(ATR-FTIR) allow detection limit down rial, which has the possibility to cause the
to 5–10 μm. FPA-FTIR can automati- loss and damage the microplastics
cally scan sample filter and obtain the
(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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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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images, typically about three orders of magnitude used to calculate each particle’s volume and surface
compared to optical microscopes. Due to its high area by adding the volumes of the individual voxels
resolution, TEM is most suited for the identification and their external areas. To determine the particles’
of smaller MPs and NPs (Gigault et al., 2016; Song length, width, and height, an eigenvalue problem for
et al., 2020). the inertia matrix needs to be solved (Safonov et al.,
According to GESAMP, there are five primary 2018). An alternative method for obtaining analyti-
morphological classifications for MPs: fragments, cal functions of the external surface of 3D particles
pellets, films, lines, and foams. The “lines” category involves combining X-ray mCT with spherical har-
considers the particles’ aspect ratio and covers fila- monic analysis. Although X-ray mCT is currently of
ments and fibers (GESAMP, 2019). Identifying the limited use, it has been applied to the study of MPs
various morphologies of MPs present in the environ- (Sagawa et al., 2018; Tötzke et al., 2021).
ment makes it possible to classify them according to
their properties without using advanced instruments. 3.4 Quality Assurance and Quality Control (QA/QC)
Moreover, morphological identification can give val-
uable insights into the sources of plastic pollution and Given the complexity of sampling, sample prepara-
the fate of a particular type of debris (López-Rosales tion, and quantitation techniques, it is not surpris-
et al., 2021). The characterization of particle shape ing to note that the data reported so far on MPs is
has been done using a variety of quantitative descrip- either under or over-estimated (Hanvey et al., 2017).
tors. The most basic dimensions, such as width, However, data comparison between studies could be
length, and height, deliver the preliminary characteri- improved to a certain extent by following strict qual-
zation of the shape of the particle, but other measures ity control measures during sampling to analysis.
like irregularity or roundness can be acquired through MPs pollution can arise from various sources, includ-
image processing (Blott & Pye, 2008). Roundness ing airborne deposition on equipment and samples,
describes the presence of corners and edges, while plastic-based sampling apparatuses, water utilized for
irregularity refers to the deviations from a regular sample processing and equipment cleaning, reagents,
three-dimensional shape due to the presence of con- working solutions, and synthetic garments worn by
cavities and convexities. While unevenness and sur- laboratory personnel. For example, sodium chloride,
face irregularities have a limited impact, the main one of the cheapest salts used for density separation,
dimensions of particles dictate their behavior in the was reported to contain 50 to 280 MPs particles/kg
aquatic environment (Khatmullina & Isachenko, (Iñiguez et al., 2017).
2017). Particle settling or buoyancy characteristics Three approaches can be adopted to reduce the
are typically determined using correlations that were risk of secondary contamination: (i) implement sound
developed for particles with regular or nearly regular field practices and adhere to good laboratory prac-
shapes. However, this poses a challenge in obtain- tices (GLPs) that reduce the introduction of MPs con-
ing accurate shape descriptors. These morphological taminants in the chemicals, air, surfaces, and equip-
descriptors need standardization to minimize ambigu- ment; (ii) assess the extent of MPs contamination
ity in the comparison data from various sources and introduced to samples through background checks,
surveys. Nevertheless, morphological characteriza- field and procedural blanks, and subsequently apply
tion involves some amount of subjectivity (López- blank correction; (iii) apply limit of detection (LOD)
Rosales et al., 2021). and limit of quantitation (LOQ), by utilizing proce-
In recent times, 3D laser range scanners and X-ray dural blanks. Various approaches used to minimize
microtomography (X-ray mCT) have emerged as tech- MPs contamination are given in Fig. 6.
niques that can provide information on the 3D shape After collecting and processing samples, it is cru-
of particles in a relatively short time (Rosal, 2021). cial to quantify and characterize blanks and conduct
The process of X-ray mCT involves creating a three- background checks. If experimental samples contain
dimensional representation of an object using a series analogous MPs, these blanks can be omitted or, at the
of 2D projections captured during tomographic scan- very least, acknowledged with the data during pub-
ning (Bozzini et al., 2018). This results in the genera- lication (e.g., Vandermeersch et al., 2015). Another
tion of digital units known as voxels, which can be option, as examined by Kroon et al., (2018), is to
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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 in the polymeric material, which can harm the envi-
secondary contamination, such as neuston nets, paint ronment and human health or may impact the proper-
chips from remotely operated vehicles (ROVs), coral ties of the polymer (Campanale et al., 2020). Other
skeletons, human hair, clothing, gloves, rubber bands, than residual monomers, plastics have various types
and lab coats. These items can then be analyzed using of additives, such as plasticizers, UV-stabilizers,
ATR FT-IR to construct a tailored library of spectra. flame retardants, processing aids, and low-atomic-
MPs present in the samples that display > 90% spec- weight polymer segments as well as oligomers,
tral match to the tailored library can be excluded from polymerization solvents, and catalyst residues (Wies-
the final tally. 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-
4 Models for Accumulation, Contamination,
nants from the surrounding environment, like heavy
and Pollution Assessment for Soil
metals and organic contaminants (Chakraborty et al.,
and Sediments
2022). Hence, MPs pose risks due to particle toxic-
ity, additives, and accumulated contaminants. Several
It is commonly believed that plastic particles exhibit
model equations are proposed for the risk assessment
biochemical inertness as a result of their large suba-
of MPs, which are discussed below.
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- 4.1 Polymer Hazard Index and Pollution Load Index
tives, makes plastics the most notorious pollutant
humans have ever made (Campanale et al., 2020). In The application of index models for evaluating MP
addition, polymerization reactions are hardly com- pollution load as well as risks is important as it help
plete, and unreacted residual monomers may be found to quickly assess the risk and make a decision. The
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index is an algorithm that computes the final result as is calculated as the nth root of the product of the poly-
a single number from the measured variables, thereby mer risks indices and the number of samples.
expressing a measure of the qualitative indicator of ∑ Pmi
MP’s pollution. For example, the polymer hazard pRi = ( × Sj ) (4)
index (PHI) is calculated using Eq. 1, using the MPs’ pT
concentration and polymer type.
)1
(5)
(
∑ pRoverall = pR1 × pR2 × pR3 … … … pRn n
PHI = Pn × Sn (1)
where “Pmi” represents the number of individual
The representation of the percentage of specific
MPs/NPs polymers discovered in sample i, and
polymer types sampled and collected at each location
“pT” indicates the total number of MPs/NPs poly-
is represented by Pn and Sn and the total hazard is rep-
mers identified in sample i. The chemical toxicity
resented as the sum of different individual polymer
coefficient derived from hazard ratings of several
hazards (Lithner et al., 2011).
polymers is represented by “Sj.” The polymeric risk
The pollution load index (PLI) is used to evaluate
indices (pRi) have been categorized as low if they
the degree/extent of MP pollution in surface sedi-
are below 150, medium if they fall between 150 and
ments (Ranjani et al., 2021). Here PLI at every loca-
300, significant if they range from 300 to 600, high
tion is associated to MP concentration factor (CF i ), as
if they exceed 600, and very high if they are greater
given in Eqs. 2 and 3.
than 1200.
Ci The polymer ecological risk index (pERI) esti-
CF i = (2) mates the degree of risk of MPs/NPs to the ecologi-
Coi
cal system, including sediments and biota. pERI is
provided in Eqs. 6, 7, and 8.
(3)
√
PLI = CF i
Ci
CF i is the quotient of the MP concentration at each Cfi = (6)
Cni
location (Ci ) to the background MP concentration
(Coi ). The lowest MPs concentration found in sedi-
∑n Pn
ments is denoted as the background value. PLI has Tri = × Sn (7)
been categorized as low or “risk category I” if the n=1 C i
value is below 10, medium or “risk category II”, if

they fall between 10 and 20, significant or under “risk Eri = Tri × Cfi (8)
category III” if they range from 20 to 30, and high or
under “risk category IV” if they exceed 30. where Ci and Cni are concentrations of pollutant i
(microplastics) in polluted and unpolluted samples,
4.2 Polymer Risk Indices and Potential Ecological respectively. Tri is represented as the toxicity coeffi-
Risk Index cient introduced by Håkanson (1980), indicating bio-
logical sensitivity and toxicity level. Pn refers to the
There is no standard approach for assessing the MPs concentration of a particular polymer, whereas Sn rep-
risk. To assess the ecological hazards of MPs/NPs, resents the hazard score assigned to plastic polymers.
one can consider the polymer composition and the The pERI for MPs/NPs is classified into five catego-
associated chemical toxicity coefficient. The equa- ries. Class I is assigned when the pERI is < 10, Class
tions for determining the polymer risks indices II is assigned when the pERI ranges from 10 to 100,
("pRi") and the overall polymer risks indices for a Class III is assigned when the pERI ranges from 101
given sample (pRoverall) are provided in Eqs. 4 and 5 to 1,000, Class IV is assigned when the pERI ranges
(Lithner et al., 2011). The “pRi” is used to evaluate from 1000 to 10,000, and Class V is assigned when
the potential environmental hazard associated with the pERI is > 10,000. These categories correspond
the MPs/NPs. On the other hand, “pRoverall” measures to the degree of risk that polymeric pollutants pose
the overall polymeric risks across all samples, which to ecological systems, ranging from low, moderate,
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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
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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%
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
substantial, high, to very high. Some of the important Stringent QA/QC measures must be implemented
risk assessment models are summarized in Table 7. during the analysis as these aid in reducing the con-
Moreover, the most common ecological risk assess- tamination of the samples, and ensuring reproducible
ment methods for MPs use the pollution load index results. The recent development of reference materials
(PLI) and pollution hazard index (PHI) to assess MP and inter-laboratory comparison (ILC) exercises on
pollution levels in different regions, considering MP MPs analysis will pave the way for developing stand-
abundance and polymer chemical toxicity. ard methodologies and shall improve the comparabil-
Moreover, MP pollution is influenced by human ity of data (Martínez-Francés et al., 2023). It is desired
activity, and the ecological risk assessment frame- that all laboratories working in the area of MPs should
work for MPs should take socio-economic factors into participate in ILC programs to improve data quality.
account (Zhang et al., 2022). Pollution and risk indi- Nevertheless, this review has demonstrated that vari-
ces are essential for assessing the contamination of ous analytical methodologies are available and can be
various media by MPs/NPs accurately; hence, an eco- used for MPs detection and quantitation. This review
logical risk assessment of MPs for different environ- has also focused on various models which would help
mental media is the foundation for controlling plastic to estimate the ecological risks, human health risk, and
pollution in the future. Model-generated data are sim- various other exposure risk assessments.
plified representations of environmental issues, which Finding solutions to limit the number of MPs and
help policymakers comprehend environmental chal- plastics entering into the environment in the initial
lenges and make more prompt and effective environ- place may be made possible by examining the mag-
mental decisions. However, plastic polymers vary in nitude of MPs input into soils through pathways such
toxicity and distribution in the environmental matrix; as compost, road runoff, and sewage sludge and MPs
thus, models should be used carefully and only when input into sediments, through biofilms and gravity dep-
all the parameters and factors are known. osition. MPs contamination in the soils and sediments
may pose environmental risk leading to public pres-
sure on decision-makers, consumers, and businesses to
5 Future Perspectives take appropriate actions. Collaboration among research
institutions is paramount for developing standard meth-
MPs in soil and sediments have only recently cap- ods, ILC and establishing quality control standards to
tured the attention of researchers. It is evident that improve MPs data quality.
the concentration of MPs in soil, sediments, and
other matrices is poised to increase in the future as Acknowledgements The authors thank CSIR-National Envi-
ronmental Engineering Research Institute, Nagpur, India, for
the demand for plastics is ever-growing. Correspond- financial assistance through intramural funding MLP-199(07).
ingly, countries are focusing on managing plastic
waste, but it is slow compared to the production rate Author Contribution Designing, conceptualization, data
of plastics. Therefore, extensive studies are required collection, and data analysis were performed by AP, AD.
in this area to determine the scale of MPs contamina- Review, editing, and overall supervision done by ARK. All
authors read and approved the final version of the manuscript.
tion in various matrices. Several analytical techniques
are published for the assessment of MPs, but these are Funding This work was supported by the CSIR-National
non-standard methods that lack uniformity in sample Environmental Engineering Research Institute, Nagpur, under
collection, extraction, and quantitation. Grant [MLP-199].
The disparity starts right from reporting the size
Declarations
range of MPs. In many studies, the information
regarding sampling units, density separation, the type
Ethics Approval and Consent to Participate Not applicable.
and pore size of filter paper used, and unit of the MPs
abundance is ambiguous. These shortcomings make
Consent for Publication Not applicable.
comparison of the published data difficult. There-
fore, standard operating procedures (SOPs) must be
Competing Interests The authors declare no competing
developed to bring consistency in the procedures and interests.
to reduce the disparities while reporting the data.
Vol.: (0123456789)
13
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Water Air Soil Pollut (2024) 235:189

Microplastics in Soils and Sediments: a Review

Received: 4 September 2023 / Accepted: 30 January 2024

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

Fig. 2 a Number of 750

Stereomicro- ing on microplastics on six

scope Polymer Meas- PMMA as river and sewage ecological

styrene tion, identification, and plastics in Bigalke,

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

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

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

Type of method Description Type of method Description

not separate denser polymers friendly but high chloride

When combined with additional approaches, chro-

and do not contain and particulate Autoclave friendly

contains no support Filtration of aqueous chloroform, cresol,

and lo w absorp- studies most alcohols,

cially when fine air pollution hydrofluoric acid)

structures that con- done. Filtration of

spectral information quickly. It has a

maintenance. The instrument helped in

3.3.6 Atomic Force Microscopy

required and this method cannot be used

Impurities in environmental samples may

ments, in case of adhesive polymers, to

interfere with the experimental results

Complex pre-treatment procedures are

contact modes when interacting with samples. A pie-

surface. The tip can be maintained under “constant

are detailed, highly resolved, and highly

of MPs. Other than that, AFM provides

force,” where data regarding interaction strength

The technique is non-destructive and

between the tip and the sample surface can be col-

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

ultrapure water and transferring an aliquot, typically

cantilevers ScanAsyst-Air (Bruker; nominal length

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

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

Using AFM enables the examination of non-conduc-

3.3.7 Transmission Electron Microscopy

The observation of fine structures smaller than

copy, can be achieved through the use of transmission

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

value is below 10, medium or “risk category II”, if

plastic Estimated Exposure from oral Pi orPmi ×RI

tion in environmental fML around 1.75 to 4.62%

Weight loss can vary

References organic contaminants. Chemosphere, 298, 134238.

Dümichen, E., Eisentraut, P., Bannick, C. G., Barthel, A. K., itory.​ocean​bestp​racti​ces.​org/​bitst​ream/​handle/​11329/​

Polymer, 102, 396–403. https://​doi.​org/​10.​1016/j.​polym​ in Analytical Chemistry, 108, 195–202. https://​doi.​org/​

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3.3.6 Atomic Force Microscopy

3.3.7 Transmission Electron Microscopy

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

Dümichen, E., Eisentraut, P., Bannick, C. G., Barthel, A. K., itory.oceanbestpractices.org/bitstream/handle/11329/

Polymer, 102, 396–403. https://doi.org/10.1016/j.polym in Analytical Chemistry, 108, 195–202. https://doi.org/