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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 3.

Density separation and organic removal for MPs analysis in freshwater sediment.

No. Order Density separation (DS) Organic removal (OR) Filtration Ref.
Density solution Procedure Filter type Drying conditions
1 DS only NaCl (1.20 g/cm3) 1. Add 200 mL of NaCl solution
Stir for 2 min
Settle for 2 h

2. Sonicate for 5 min
Settle overnight
N/A 1.0 μm glass microfiber filter 50 °C for 48 h (Wang et al., 2017)
2 DS → OR CHKO2 (1.54 g/cm3) To overflow supernatant into stainless steel tray add solution and settle overnight Using H2O2 (30%) at 60 °C overnight 1.2 μm glass microfiber filter Dry in a desiccator (Xiong et al., 2018)
3 DS → OR 1. NaCl (saturated)
2. NaI (60%)
Perform a two step density separation
1. Add 1 L of NaCl solution Stir for 2 min
Settle for 10 min
Sieve using a 48 μm stainless steel sieve
Repeat three times

2. Add 375 mL of NaI solution
Shake 200 rpm on a shaker for 2 min
Settle for 10 min
WPO (30% H2O2) for 12 h 0.45 μm glass microfiber filter 50 °C (Di and Wang, 2018)
4 DS → OR ZnCl2 (1.50 g/cm3) Add 400 mL of ZnCl2 solution
Stir for 30 min
Settle for 24 h
WPO (30% H2O2) 0.22 μm glass microfiber filter 60 °C (Jiang et al., 2018)
5 DS only NaCl (1.20 g/cm3) Add NaCl solution
Stir for 2 min
Settle for 24 h
N/A 1.0 μm glass microfiber filter Dry to constant weight (Peng et al., 2018)
6 DS → OR ZnCl2 (1.60 g/cm3) Disaggregate with 400 mL of sodium polyphosphate (5.5 g/L)
Stir for 1 h at high rpm
Sieve sediments using a 5 mm and 0.055 mm sieve Add 300 mL of ZnCl2 solution and stir
Settle for 1 h and transfer supernatant to 0.055 mm sieve and rinse with Milli-Q water
WPO (30% H2O2 with 0.05 M Fe2+ catalyst) at 75 °C for 5/10 min until it starts boiling and afterwards react at room temperature for 15 h 0.45 μm membrane filter 40 °C for 3–5 days (Rodrigues et al., 2018)
7 OR → DS ZnCl2 (1.58 g/cm3) Add 36 mL of ZnCl2 solution
Settle for 24 h
WPO (30 mL of 30% H2O2) for overnight 1.2 μm nitrocellulose
filter paper
Air-dry (Shruti et al., 2019)
8 OR → DS → OR ZnCl2 (1.97 g/cm3) Perform a 2 step density separation
1. Add 1.5 L of ZnCl2 solution
Aerate for 1 h
Settle for 5 h
Drain off solution using a funnel

2. Aerate for 30 min
Settle overnight
Drain off solution
1. Pre-oxidation:
50 g of WW subsample was filled with 200 mL Milli-Q water before adding 30 mL of 30% H2O2 (achieving final concentration of 4%)
Heat at 50 °C and stir
Add 30 mL 30% H2O2 every 24 h (until no foaming)
Dry at 50 °C
Repeat processing for all of the 3 L sediments

2. Post-oxidation: Fenton reaction by adding 146 mL of 50% H2O2, 63 mL of 0.1 M FeSO4 and 65 mL of 0.1 M NaOH at 15–19 °C
Leave for 2 days at room temperature
500 μm sieve, 10 μm stainless steel filter 1. Dry particles on a 500 μm sieve at 50 °C
2. Collect the particles on a 10 μm filter into HPLC grade ethanol by ultrasonication and evaporate by nitrogen (N5.0) until dry
(Liu et al., 2019a)
9 DS → OR NaCl (saturated) Add NaCl solution
Stir for 2 min
Settle for 24 h
WPO (30 mL of 30% H2O2) at 100 rpm and 65 °C for 24 h 0.45 μm membrane filter paper 50 °C for 24 h (Ding et al., 2019)
10 DS only NaCl (1.20 g/cm3) Add 40–68 mL of NaCl solution
Stir for 1 min
Settle for 24 h
N/A 11 μm cellulose filter Room temperature (18–21 °C) (Blair et al., 2019)
11 DS → OR ZnCl2 (1.70 g/cm3) Leave a 1.5 cm margin, fill ZnCl2 solution into a 100 mL flask
Sonicate at 160 W/35 kHz for 15 min
Stir at 250 rpm for 1 h
Settle for 30 min
Add 20 mL of ZnCl2, allow the excess fluid to overflow
Store supernatants at 4 °C
1. Sieve using 500 μm sieve
Filter using 10 μm stainless steel disk

2. <500 μm particles: oxidation by adding Fenton reagent (10 mL of FeSO4 (7.2 mM, pH 5)) in a 20 °C water bath
Add 20 mL 30% H2O2 after 15 min and sonicate at 215 W/35 kHz for 5 min

3. >500 μm particles: retain for subsequent analysis
1. 0.2 μm anodisc (<500 μm)

2. 0.45 μm mixed cellulose ester (500 μm-2
50 °C for least 2 days (Mani et al., 2019)
12 DS → OR 1. NaCl (saturated)
2. NaI (60%)
1. Add 1 L of NaCl solution Settle for 2 h
Sieve using 50 μm stainless steel sieve and rinse with distilled water
Repeat three times

2. Add 500 mL of NaI solution and perform the same way and repeat three times
WPO (30 mL of 30% H2O2) 0.7 μm glass microfiber filter N/A (Yuan et al., 2019)
13 DS only NaCl (30%) Add 400 mL of NaCl solution
Stir for 2 min using spoon
Leave until no more visible material floats
N/A 1.2 μm glass microfiber filter 105 °C for 30 min (Alam et al., 2019)
14 DS → OR LMT (1.60 g/cm3) Shake with 300 mL of LMT solution for 1 min
Settle for 10 min
Transfer supernatant
Repeat twice with 200 mL of LMT
WPO (20 mL of 35% H2O2 with Fe2+ solution) at 75 °C at 180 rpm for 30 min
Add H2O2 every 30 min
5 μm polycarbonate filter paper Room temperature (Eo et al., 2019)
15 DS → OR ZnCl2 (1.80 g/cm3) Mix with ZnCl2 (1:10(w/v))
Stir for 15–20 min
Settle overnight
Collect on filter paper (0.7 μm glass microfiber filter)
WPO (30% H2O2) for 3 h 0.7 μm glass microfiber filter Dry in a desiccator for 36 h (Sarkar et al., 2019)
16 DS only 1. DI water (1.0 g/cm3)
2. NaI (1.60 g/cm3)
1. Elutriation step with water for 20 min
Mix sediments by air stone
Collect overflow materials on a 63 μm sieve by adding water (250 L/h flow rate)
Transfer into a 50 mL centrifuge tube

2. Add 30 mL of 3.3 M NaI solution
Centrifuge for 5 min at 3500 G
Settle for 1 h
Repeat once again
N/A 1.2 μm glass microfiber filter 60 °C (Dikareva and Simon, 2019)
17 DS, OR simultaneously NaCl (1.20 g/cm3) Use 200 mL of NaCl +20 mL of 30% H2O2 solution
Heat at 50 °C
Stir for 20 min at 200 rpm
Settle at 50 °C for 1 h and afterwards settle at room temperature for 1 h
Transfer foam from reaction and mix with 50 mL of NaCl + 20 mL of H2O2 and then heat, mix, settle, and filter supernatant

Meantime, add 20 mL of H2O2 to WPO solution and sediments, heat, mix and settle the mixture again and then collect and filter supernatant
0.7 μm glass microfiber filter 40 °C overnight (Simon-Sánchez et al., 2019)
18 DS → OR ZnCl2 (1.60–1.80 g/cm3) Fill with ZnCl2 solution
Settle for 24 h
WPO (30% H2O2 and 10% H2SO4) at 55 °C for 5 days

After filtration, repeat the washing process at least twice (until the washing water pH is 7)
Finally, transfer the suspended powder on the filter to the new filter
2.7 μm glass microfiber filter 55 °C for 7 days (For pyr-GC–MS analysis) (Scherer et al., 2020)
19 OR → DS NaCl (1.20 g/cm3) Add NaCl solution
Stir for 2 min
Settle for 24 h
WPO (30% H2O2) 1.0 μm glass microfiber filter 40 °C for 24 h (Peng et al., 2017)
20 DS → OR NaI - NaCl (1.50 g/cm3) Add 250 mL of NaI - NaCl solution
Air floatation for 40 s
Settle for 5 min
WPO (30 mL of 35% H2O2) at room temperature for 7 0.45 μm membrane filter N/A (Han et al., 2019b)