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. Author manuscript; available in PMC: 2023 Jun 7.
Published in final edited form as: Sci Total Environ. 2023 Jan 26;871:161718. doi: 10.1016/j.scitotenv.2023.161718

Table 4.

Density separation and organic removal for MPs analysis in soil.

No. Order Extraction (density separation; DS) Organic removal (OR) Filtration Ref.
Solution Procedure Filter type Drying conditions
1 DS → OR NaCl (1.19 g/cm3) Add NaCl solution
Ultrasonication for 2 min
Stir for 30 min
Settle for 24 h
Repeat three times
WPO (30% H2O2) at 50 °C for 72 h 20 μm nylon net filter Room temperature (Liu et al., 2018)
2 DS → OR NaCl (1.20 g/cm3) 1. Add 160 mL of 27% NaCl solution
Stir for 10 min
Centrifuge at 3450 G for 30 min

Filter supernatant using 0.45 μm membrane filter

2. Remove particles stuck to beaker walls by 27% NaCl and settle for 24 h

Mix sample mixture at 800 rpm for 10 min
Centrifuge at 3450 G for 30 min
Wash particles from the filter and then treat them with 40–80 mL of 65% HNO3 at 90 °C for 48 h 0.2 μm infrared transparent anodisc filter N/A (Scheurer and Bigalke, 2018)
3 OR → DS → OR NaI (1.80 g/cm3) Add 150 mL of NaI solution
Centrifuge again
Wash with NaI solution
1. Pre-oxidation:
WPO (10 mL of 35% H2O2 + 1 mL of 10% FeSO4) at 50 °C
Add a few drops of butyl alcohol (if frothing was excessive)
Add 1 mL of 10% FeSO4 (to decompose the H2O2)
Add 30 mL of 0.5 M NaOH
Store for 24 h
Adjust to 150 mL using DI water
Agitate for 20 min using ultrasonic
Centrifuge at 2300 rpm for 10 min

2. Post-oxidation: WPO (2 mL of 35% H2O2)
1 mm, 0.25 mm, 0.05 mm sieve 80 °C (Zhang and Liu, 2018)
4 DS only 1. NaCl (1.20 g/cm3)

2. NaI (1.60 g/cm3)
1. Use a continuous flow and floating separation apparatus
Float using NaCl solution
Clean residues in the sieve (300 mesh) were cleaned using water

2. Residues were floated using NaI solution
Filter if it contained a large number of solid particles
N/A N/A Air dry (Zhou et al., 2018)
5 1. OR → DS → OR

2. DS → OR
1. NaCl (1.20 g/cm3), NaI (1.80 g/cm3), ZnCl2 (1.50 g/cm3)

2. Only using NaCl (1.20 g/cm3)
1. Test three types of floatation solutions
Add 200 mL of a solution
Stir at 200 rpm for 1 h using a shaker
Settle for 48 h and siphon out 100 mL of supernatant
Add 100 mL of the same floatation solution
Stir for 30 min and settle for 48 h
Combine supernatants

2. Repeat steps but by only using NaCl solution
1. Pre-oxidation:
WPO (200 mL of 30% H2O2)
If temperature remained stable, heating at 70 °C

2. Post-oxidation:
WPO (30% H2O2 + H2SO4 (3:1, v/v))
20 μm nylon filter Air dry (Li et al., 2019)
6 DS → OR NaCl (1.24 ± 0.05 g/cm3) Add NaCl solution
Stir for 30 min
Settle for 24 h
Repeat three times
Filter with 20 →m
Wash filter
WPO (100 mL of 30% H2O2) at 65 °C at 80 rpm for 72 h
20 μm nylon net filter Room temperature (Lv et al., 2019)
7 DS only 1. DI water (1.0 g/cm3)

2. NaCl (1.20 g/cm3)
3. ZnCl2 (1.55 g/cm3)
1. Add 20 mL of DI water stir at 21,000 rpm for 30 s
Centrifuge at 2000 rpm for 15 min
Filter supernatant using by 2–3 μm filter paper

2. Add 20 mL of NaCl
Stir, centrifuge and filter the same way

3. Add 20 mL of ZnCl2
Stir 32,000 rpm for 30 s
Centrifuge 2000 rpm for 15 min
Filter the same way
N/A 2.5 μm cellulose filter paper N/A (Corradini et al., 2019)
8 DS → OR NaBr (1.55 g/cm3) Add NaBr solution
Stir for 5 min
Settle for 2 h
Use automatic cycling device for 30 min
Filter using a 20 μm filter
WPO (30% H2O2) at 60 °C for 3 days 20 μm membrane filter N/A (Liu et al., 2019b)
9 DS → OR NaI Add 200 mL of NaI solution
Stir for 30 min
Settle for 12 h
Filter using a 7 μm glass fiber filter
WPO (100 mL of 30% H2O2) for 12 h 7 μm glass fiber filter Room
temperature
(Huang et al., 2020)
10 DS → OR DI water (1.0 g/cm3) Leach soil specimens using pressurized water
Add distilled water
Shake for 30 s
Precipitate for 5 min
Repeat three times
Oxidation using 10 mL of 98% H2SO4
Sonicate for 20 min
Place in ice bath
Dilute with distilled water
Membrane filter paper Dry at 50–60 °C (Li et al., 2020)
11 DS → OR 1. NaCl (1.20 g/cm3)

2. NaI (1.60 g/cm3)
Disperse dried soil with (NaPO3)6 (0.5 mol/L)
Add NaCl solution into beaker (flow rate 1.0 L/min) with air blowing at the bottom

Collect the over-flow materials on a vibrating sieve (pore 50 μm)
Settle residues on the sieve for 48 h in NaI solution
Filter using a 5 μm cellulose nitrate filter
Repeat three times
WPO (30% H2O2) at 70 °C for 72 h 20 μm glass fiber filter N/A (Zhou et al., 2020)
12 DS → OR ZnCl2 (1.60 g/cm3) Add ZnCl2 solution
Settle for 6 h at room temperature
Repeat three times
WPO (30% H2O2) at 70 °C in water bath N/A Air dry (Duan et al., 2020)
13 OR → DS NaCl (30%; w/v) Add 600 mL of NaCl solution
Settle for 12 h
WPO (50 mL of mixture (35% H2O2 + 0.5 M of ferrous sulfate)) at room temperature for 24–72 h 300, 150, 50 μm sieve N/A (Rafique et al., 2020)
14 DS only 1. DI water (1.0 g/cm3),

2. NaCl (1.20 g/cm3),

3. ZnCl2 (1.55 g/cm3)
1. For visual identification, centrifuge
5 g of soil and 20 mL of DI water at 2000 rpm for 15 min

Filter supernatant through a 2.5 μm filter paper

Fill remaining sediments with 20 mL of NaCl
Centrifuge at 21000 rpm for 30 s and filter supernatant a another time

Fill remaining sediments with 20 mL of ZnCl2
Centrifuge last time and filter supernatant through the same filter used the previous two times

2. For FTIR microscope analysis, sonicate
1 g soil and 10 mL of ZnCl2 for 10 min
Agitate at 2000 rpm for 15 s
Shake for 20 min at 180 oscillations per min
Before filtration, centrifuge for 10 min at 2500 rpm

Filter supernatant through a 0.4 μm polycarbonate membrane filter
Re-fill with ZnCl2 and underwent same step once again
N/A 1. 2.5 μm cellulose filter paper (for visual identification by optical microscope)

2. 0.4 μm polycarbonate membrane filter (for FTIR analysis)
Dried at 40 °C for 12 h (for FTIR analysis) (Corradini et al., 2021)
15 DS only Tap water Add tap water
Stir and settle overnight
N/A 1 mm sieve (collect >1 mm size) Dry at 60 °C for 24 h (Katsumi et al., 2021)
16 DS → OR ZnCl2 (1.70 g/cm3) Add 500 mL of ZnCl2 solution
Stir at 300 rpm for 5 min
Settle for 24 h
Repeat three times
WPO (20 mL of 0.05 M FeSO4 and 3 mL of conc. H2SO4 and 20 mL of 30% H2O2) at 75 °C for 24 h
Rinse with water and sieve using a 1 mm sieve
0.45 μm membrane filter Room temperature (Choi et al., 2021)
17 OR → DS ZnCl2:CaCl2 (2:1.4; 1.55–1.58 g/cm3) 1. Filter digested supernatant through 20 μm sieve, afterward, visually sort and analyze the >1 mm particles

2. Fill digested remnant with density solution
Filter supernatant through 20 μm
sieve
Sort >1 mm
Repeat this process two more times

3. Perform density separation of the particles of <1 mm obtained from the first process and >20 μm obtained from the second process and filter supernatant finally
WPO (200 mL of 30% H2O2) 0.7 μm glass fiber filter N/A (Kim et al., 2021)
18 DS → OR NaCl (1.19 g/cm3) Shake soil samples at 150 rpm for 30 min with 300 mL of distilled water using an orbital shaker
Settle for 24 h
Repeat 3–4 times until no more observed floating extract
Centrifuge the collected supernatant solution for 29 min at 1500 rpm
Mix supernatant with 100 mL of NaCl solution for 15 min at 150 rpm and settle overnight
Centrifuge supernatant for 10 min at 1500 rpm for 1 s
WPO (100 mL of 30% H2O2) for 7 days at 25 °C 0.45 μm cellulose nitrate filter Room
temperature
(Ragoobur et al., 2021)
19 OR → DS CaCl2 (1.40 g/cm3) Centrifuge with CaCl2 solution for 10 min at a speed of 3700 min−1
Stain samples with Nile red
Fenton reaction by adding 30 mL of 30% H2O2, 30 mL of iron catalyst for 1 h at 0 °C Glass fiber filter 60 °C (Grause et al., 2022)
20 OR → DS NaCl (1.20 g/cm3) Add 100 mL of NaCl solution
Stir for 1 min
Settle for 1.5 h
WPO (40 mL of 33% (w/v) H2O2) for 2 hat 60 °C
Stir at 300 rpm
50 μm stainless steel filter N/A (Pérez-Reverón et al., 2022)