Validation of Sample Preparation Methods for Microplastic Analysis in Wastewater Matrices—Reproducibility and Standardization
Abstract
:1. Introduction
1.1. Sample Preparation Methods for Removing Organic Matter
1.2. Parameters Used in Microplastic Monitoring
1.3. Research Objectives and State-of-the-Art
2. Materials and Methods
2.1. Selection of Sample Preparation Protocols
2.2. Materials
2.3. Contamination Mitigation and Quality Assurance
2.4. Investigating the Discrepancies in Fenton Reactions
2.5. Investigating the Effects of Sample Preparation on Microplastics
2.5.1. Size Distribution Analysis by Laser Diffraction
2.5.2. FTIR Analysis
2.5.3. Thermal Analysis by TD-Pyr-GC/MS
2.6. Determination of the Organic Matter Removal Efficiency from Sludge Samples
3. Results and Discussion
3.1. Discrepancies in Fenton Reactions
3.2. Investigating the Effects of Sample Preparation on Microplastics
3.2.1. Variation in Size Distribution (Laser Diffraction)
3.2.2. Variation in Infrared Spectra (FTIR)
3.2.3. Variations in Pyr-GC/MS Chromatograms
3.3. Organic Matter Removal Efficiency
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Conflicts of Interest
Appendix A
Acrylonitrile-butadiene-styrene | ABS |
Cellulose acetate | CA |
Crosslinked polystyrene | PSXL |
Expanded PS | EPS |
High-density PE | HPDE |
Low-density PE | LDPE |
Linear LDPE | LLDPE |
Nylon-6 or polyamide-6 | NY6 |
Nylon12 or polyamide-12 | NY12 |
Nylon-66 or polyamide-66 | NY66 |
Poly 1,4-butylene terephthalate | PBT |
Polyamide | PA |
Polycarbonate | PC |
Polyethylene | PE |
Polyethylene terephthalate | PET |
Poly(hexamethylene nonanediamide) | Nylon 6/9 |
Poly(methyl methacrylate) | PMMA |
Polypropylene | PP |
Polytetrafluoroethylene | PTFE |
Polyurethane | PUR |
Polyvinyl chloride | PVC |
Styrene acrylate | SA |
Un-plasticized polyvinyl chloride | uPVC |
Protocols | Conditions | Matrix | MPs | Effects on Organics | Effects on MP |
---|---|---|---|---|---|
H2O2 (30%) [7] | 60 °C for * 24/12 h or 70 °C for * 24 h | Sludge and soil | PP, LDPE, HDPE, PS, PET, NY66, PC, PMMA | Digestion > 80% for sludge and >96% for soil | Degradation of NY66 (at 70 °C), PP (at 70 °C). As for PS; less degradation at 60 °C and more at 70 °C |
H2O2 (35%) [11] | 50 °C for 96 h | Fish | LDPE, HDPE, PP, PS, PET, PVC, NY6, NY66 | Digestion of 98% | Discoloration of PET, loss of NY6 and NY6 |
H2O2 (30%) [12] | 55 °C for 7 days | Fish | PE, PS | ** Extraction efficiency of 70% | No report |
Density separation then H2O2 (15%) [12] | 50 °C overnight | Fish | PE, PS | ** Extraction efficiency of 95% | No effects |
H2O2 (30%) [13] | RT. For 7 days | Marine sediment | PVC, PET, PA, ABS, PC, PUR, PP, LDPE, LLDPE, HPDE | 50% digestion and the rest were discolored | Discoloration or degradation in PA, PC, PP, PET, LLDPE, PVC, PUR, LDPE |
H2O2 (35%) [13] | RT. For 7 days | Marine sediment | PVC, PP, LDPE, PE, HDPE, PET, PUR, PS, PC, PA, ABS, EPS | 92% digestion and discoloration | Size reduction PP and PE |
H2O2 (30%) then density separation [14] | 70 °C overnight | Sludge | PE | ** Extraction efficiency of 78% | No adverse effects reported |
Protocols | Conditions | Matrix | MPs | Effects on Organics | Effects on MP | |
---|---|---|---|---|---|---|
H2O2 (30%) + 20 g/L FeSO4 7H2O2 1:1 (v/v) [7] | <40 °C (Ice bath) | *24 h/20 min | Sludge and soil | PP, LDPE, HDPE, PS, PET, NY66, PC, PMMA | Digestion 87% for sludge and 106% for soil | No adverse effects |
H2O2 (30%) + 15 g/L FeSO4 7H2O2 1:1 (v/v) [15] | 50 °C for 1 h. | Plant and animal tissues | PE, PP, PS, PET, PVC, CA, PA | Digestion of 72.6% of fish tissue, 100% of algae, 26.3% driftwood, 17.5% paraffin | Degradation of CA | |
H2O2 (30%) + 15 g/L FeSO4 7H2O2 1:1 (v/v) [16] | 75 °C for >35 min | Water, beach and sediment | None tested | No reports | No reports | |
H2O2 (30%) + 20 g/L FeSO4 7H2O2 (2:1 v/v) [17] | RT. (no ice bath) | 10 min reaction + 10 min cooling | Sludge | PE, PP, PVC, PA | Effective removal (No exact details provided) | No observed effects |
Protocols | Conditions | Matrix | MPs | Effects on Organics | Effects on MP |
---|---|---|---|---|---|
HNO3 (69%) [11] | 25 °C for 96 h | Fish | LDPE, HDPE, PP, PS, PET, PVC, NY6, NY66 | Removal >95% | Loss of NY6, NY66. Melting of LDPE, HDPE, PP. Recovery of PVC 69%. Discoloration of others |
HNO3 (55%) [20] | Based on fish size: RT. For 3–10 h or 80 °C for 10–20 min | Fish | HDPE, PA, Nylon 6/9, PBT, PVC | Complete digestion of the fish | Tested at room temperature for 1 month. Loss of Nylon within 24 h, the rest showed no significant changes after 1 month. |
HNO3 (22.5 M) [21] | RT. Overnight then boiling for 2 h | Mussels | PS, PA | Good digestion of the tissues | PA fibers (30 × 200 µm) were lost. PA particles 100 × 400 µm were 98% recovered. PS particles 30 µm and 10 µm were recovered. |
HNO3 (22.5 M) [21] | 60 °C for 1 h. then 100 °C for 1 h | Mussels | PS, PA | Satisfactory digestion of the tissues | PS particles melting together when exposed to the reagent directly. This did not occur when PS was embedded in the tissues. PA was completely lost |
HNO3 (22.5 M) [12] | RT. overnight then boiling for 30 min | Fish | PS, PE | ** Extraction efficiency of only 4% | Almost complete loss of PS and PE |
HNO3 (65%) [22] | RT. overnight then 60 °C for 2 h | None | LDPE, HDPE, PP, NY12, PS | Not tested due to damaged polymers | Melting of NY12, yellowing of the rest |
HNO3 (35%) [25] | 60 °C overnight | Mussels | PET, HDPE, PVC, PA | Complete digestion | Melting together of PET, HDPE, loss of PA |
HCL (37%) [11] | 25 °C for 96 h | Fish | LDPE, HDPE, PP, PS, PET, PVC, NY6, NY66 | Digestion efficiency >95% | Loss of NY6, NY66. Melting and clumping of PET |
HCL (20%) [13] | RT. for 7 days | Marine sediment | PVC, PET, PA, ABS, PC, PUR, PP, LDPE, LLDPE, HPDE | No complete dissolution of any biogenic organic matter | Not reported |
Protocols | Conditions | Matrix | MPs | Effects on Organics | Effects on MP |
---|---|---|---|---|---|
KOH (10%) [7] | 60 °C for 24 h | Sludge and soil | PP, LDPE, HDPE, PS, PET, NY66, PC, PMMA | Digestion of sludge: 57% And for soil: 35% | A slight weight decrease for PC |
KOH (10%) [11] | 25 °C for 96 h or 40 °C for 48 h or 50 °C for 36 h or 60 °C for 24 h | Fish | LDPE, HDPE, PP, PS, PET, PVC, NY6, NY66 | Removal >95% (all temperatures) | Yellowing of NY66. Reduction in PVC and PET recovery that worsens with increased temperature |
KOH (10%) [22] | 0 °C for 24 h | Mussels, crabs, fish | CA, HDPE, LDPE, NY6, NY12, PC, PET, PMMA, PP, PS, PSXL, PTFE, PUR, uPVC, EPS | Digestion efficiency > 99.5% | Degradation of CA |
KOH (56, 224 g/L) [26] | RT. For 14 days | None | Cera Microcrystalline, PE | ** Extraction efficiency > 95% | Discoloration of cera microcrystalline and PE (for 224 g/L) |
KOH (10%) [28] | RT. For 2–3 weeks | Fish | No spiking: PE, PP, PET, SA | Digestion satisfactory | None tested |
KOH (10%) [29] | 60 °C for 24 h | Vegetal | PP, PE, PVC, PUR, PET, PS | No digestion observed | No effects observed |
NaOH (1, 10 M) [7] | 60 °C for 24 h | Sludge and soil | PP, LDPE, HDPE, PS, PET, NY66, PC, PMMA | Digestion of sludge: 61% (1M) 67% (10M) and soil: 68% (1 M) 65% (10 M) | Degradation of PET, PC (even more with 10 M) |
NaOH (20, 30, 40, 50%) [13] | RT. For 7 days | Marine sediment | PVC, PET, PA, ABS, PC, PUR, PP, LDPE, LLDPE, HPDE | No complete dissolution of any biogenic organic matter. Strongest reaction with NaOH (20%) | Not reported |
NaOH (10 M) [22] | 60 °C for 24 h | None | CA, HDPE, LDPE, NY6, NY12, PC, PET, PMMA, PP, PS, PSXL, PTFE, PUR, uPVC, EPS | Not tested due to damage to polymers | Degradation of CA, PC, PET |
NaOH (1 M) [25] | 60 °C overnight | Mussels | PET, HDPE, PVC, PA | Complete digestion and extraction efficiency of 93% | No significant effects |
NaOH (10 M) [27] | 60 °C for 24 h | Zooplankton | PS, PA, PET, PE, uPVC | Digestion efficiency of 91% | Partial degradation of PA, clumping of PE, yellowing of uPVC, partial loss of PS |
NaOH (10 M) [29] | 60 °C for 24 h | Vegetal | PP, PE, PVC, PUR, PET, PS | Almost no digestion | Degradation of PET |
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Protocols | Temperature | Time |
---|---|---|
Fenton (30% H2O2 + 20 g/L FeSO4) [17] | Unregulated | 10 min + 10 min cooling |
KOH (10%) [22] | 60 °C | 24 h |
H2O2 (30%) [7] | 60 °C | 24 h |
Protocols | Description |
---|---|
Control | 5 mL UPW @ Room Temperature |
Fenton | As described in Figure 1 (2 mL FeSO4 as a starting volume) |
H2O2 | As described in Figure 1 (5 mL H2O2) |
KOH | As described in Figure 1 (5 mL KOH) |
** Temperature control 60 °C | 5 mL UPW @ 60 °C and 24 h |
** Temperature control 90 °C | 5 mL UPW @ 90 °C and 20 Minutes |
H2O2 Batches | Tmax [°C] | pH @ Tmax [-] | Time Till Tmax [sec] |
---|---|---|---|
(i) | 86.9 ± 0.9 | 1.62 ± 0.03 | 157 ± 4 |
(ii) | 87.2 ± 0.2 | 1.67 ± 0.06 | 167 ± 19 |
(iii) | 70.4 ± 23 | 1.72 ± 0.23 | 510 ± 127 |
(iv) | 85 ± 0.4 | 1.67 ± 0.05 | 173 ± 11 |
(v) | 84.9 ± 1.7 | 1.69 ± 0.04 | 192 ± 5 |
Reaction Type | Tmax [°C] | pH @ Tmax [-] | Time to Tmax [sec] |
---|---|---|---|
Type (I) (batch (ii)) | 84.1 ± 3.4 | 1.65 ± 0.09 | 228 ± 3 |
Type (II) (batch (iii)) | 60.8 ± 29.3 | 1.7 ± 0.25 | 554 ± 190 |
Polymer Type | Particle Treatment | Pyrolysis Products in TD [%]/Standard Deviation [%] |
---|---|---|
PA | untreated | 74.5/19.0 |
Fenton | 17.1/12.65 | |
H2O2 | 3.0/3.67 | |
PS | untreated | 79.3/12.5 |
Fenton | 78.8/16.9 | |
H2O2 | 71.9/10.9 |
Protocol | Total Weight Removal | Corresponding Organic Matter Removal * |
---|---|---|
Fenton | 83.5% ± 1.8% | 118.4% ± 2.6% |
H2O2 | 71.3% ± 1.2% | 101.1% ± 1.6% |
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Al-Azzawi, M.S.M.; Kefer, S.; Weißer, J.; Reichel, J.; Schwaller, C.; Glas, K.; Knoop, O.; Drewes, J.E. Validation of Sample Preparation Methods for Microplastic Analysis in Wastewater Matrices—Reproducibility and Standardization. Water 2020, 12, 2445. https://doi.org/10.3390/w12092445
Al-Azzawi MSM, Kefer S, Weißer J, Reichel J, Schwaller C, Glas K, Knoop O, Drewes JE. Validation of Sample Preparation Methods for Microplastic Analysis in Wastewater Matrices—Reproducibility and Standardization. Water. 2020; 12(9):2445. https://doi.org/10.3390/w12092445
Chicago/Turabian StyleAl-Azzawi, Mohammed S. M., Simone Kefer, Jana Weißer, Julia Reichel, Christoph Schwaller, Karl Glas, Oliver Knoop, and Jörg E. Drewes. 2020. "Validation of Sample Preparation Methods for Microplastic Analysis in Wastewater Matrices—Reproducibility and Standardization" Water 12, no. 9: 2445. https://doi.org/10.3390/w12092445