Robin Treilles a , A. Cayla b,c , J. Gasperi a , B. Strich c , P. - - PowerPoint PPT Presentation

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Robin Treilles a , A. Cayla b,c , J. Gasperi a , B. Strich c , P. - - PowerPoint PPT Presentation

Jan 12, 2024 359 likes •578 views

Robin Treilles a , A. Cayla b,c , J. Gasperi a , B. Strich c , P. Ausset d and B. Tassin a a University of Paris-Est, LEESU, France b University of Lille Nord de France, Lille, France c ENSAIT, GEMTEX, Roubaix, France d University of Paris-Est

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SLIDE 1

Robin Treillesa, A. Caylab,c, J. Gasperia, B. Strichc, P. Aussetd and B. Tassina

a University of Paris-Est, LEESU, France b University of Lille Nord de France, Lille, France c ENSAIT, GEMTEX, Roubaix, France d University of Paris-Est Créteil, LISA, France

robin.treilles@enpc.fr

1 Microplastics 2018, October 30th, Ascona, Switzerland

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SLIDE 2

Digestion protocols are used to dissolve organic matter in environmental

  • samples. In recent works, we observe three important points:
  • 1. Fibers correspond to the greater fraction of microplastics in water

samples. 2. Quality Assurance/Quality Control (QA/QC) for digestion protocols are more and more developed for fragments but not for fibers.

  • 3. Impacts of digestion protocols on fibers?

2

Rain Waters Washing Machine Effluents Surface Waters Fibers (Item/Liter) 20 - 40 9,000 - 35,000 0.03 - 0.05 Fragments (Item/Liter) Not observed < 2 0.001 - 0.003

Table from ASTEE Presentation, Tassin et al., 2018

Picture from Soline Alligant

Microplastics 2018, October 30th, Ascona, Switzerland

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SLIDE 3

3

Vegetable Animal Artificial Cotton Flax Wool PA 6.6 PET Acrylic Viscose Synthetic

The most commonly used fibers (Raw fibers)

Natural Fibers Chemical Fibers

Microplastics 2018, October 30th, Ascona, Switzerland

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SLIDE 4

Four different digestion protocols have been selected:

  • KOH 10%, 40°C, 24h (Dehaut et al., 2016)
  • KOH 10%, 60°C, 24h (Karami et al., 2017)
  • H2O2 30%, 50°C, 48h (Stolte et al., 2015)
  • NaClO 9%, ambient temperature, one night (Collard et al., 2015)

4

After digestion and filtration

Microplastics 2018, October 30th, Ascona, Switzerland

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SLIDE 5

5

Fibers Caracterisation before and after digestion Morphological aspects Mechanical Properties Thermal and Chemical Properties

  • Mass variation
  • Microscope
  • bservation:
  • Optical
  • Scanning

Electron Microscope

  • Linear mass

density

  • Tenacity =

Breaking strain

  • Elongation at

break

  • Differential

Scannning Calorimetry (DSC)

  • Infrared

Spectroscopy (FTIR)

1 2 3

Microplastics 2018, October 30th, Ascona, Switzerland

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SLIDE 6

s:

Flax, Microscope x 40, before and after NaClO digestion

6

After digestion NaClO 9%, Ambient temperature 100 µm 100 µm

Flax Flax

Microplastics 2018, October 30th, Ascona, Switzerland 6

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7

After digestion KOH 10% 60°C 24 hours 100 µm 100 µm ~20 µm < 10 µm

PET PET

s:

PET, Microscope x 40, before and after KOH 60°C digestion

Microplastics 2018, October 30th, Ascona, Switzerland

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SLIDE 8

Results:

8

250 µm 25 µm 10 µm 10 µm

After digestion KOH 10% 60°C 24 hours

Increase of surface roughness

Microplastics 2018, October 30th, Ascona, Switzerland

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9

250 µm 25 µm 10 µm 10 µm

After digestion KOH 10% 60° 24 hours

  • PET is strongly affected by KOH 60°C digestion

(~70 % of mass loss), high degradation is confirmed with SEM.

  • Flax hull is shattered by NaClO digestion.

SEM analysis will complete this observation.

  • Wool is totally dissolved, except for H2O2.

Microplastics 2018, October 30th, Ascona, Switzerland

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SLIDE 10

10 Microplastics 2018, October 30th, Ascona, Switzerland

  • 1

1 2 3 4 5

Elongation at break (%)

Before Dig KOH 40°C KOH 60°C NaClO H2O2

20 40 60 80 100 120

PET PA 6.6 Acrylic Viscose Flax Cotton

Tenacity (cN/Tex)

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SLIDE 11

11 Microplastics 2018, October 30th, Ascona, Switzerland

  • 1

1 2 3 4 5

Elongation at break (%)

Before Dig KOH 40°C KOH 60°C NaClO H2O2

20 40 60 80 100 120

PET PA 6.6 Acrylic Viscose Flax Cotton

Tenacity (cN/Tex)

Mean ± standard deviation N = 30 for non digested fibers N = 3 to 5 for digested fibers

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SLIDE 12

12 Microplastics 2018, October 30th, Ascona, Switzerland

  • 1

1 2 3 4 5

Elongation at break (%)

Before Dig KOH 40°C KOH 60°C NaClO H2O2

20 40 60 80 100 120

PET PA 6.6 Acrylic Viscose Flax Cotton

Tenacity (cN/Tex)

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SLIDE 13

13 Microplastics 2018, October 30th, Ascona, Switzerland

  • 1

1 2 3 4 5

Elongation at break (%)

Before Dig KOH 40°C KOH 60°C NaClO H2O2

20 40 60 80 100 120

PET PA 6.6 Acrylic Viscose Flax Cotton

Tenacity (cN/Tex)

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SLIDE 14

14 Microplastics 2018, October 30th, Ascona, Switzerland

  • 1

1 2 3 4 5

Elongation at break (%)

Before Dig KOH 40°C KOH 60°C NaClO H2O2

20 40 60 80 100 120

PET PA 6.6 Acrylic Viscose Flax Cotton

Tenacity (cN/Tex)

  • PET becomes too brittle with KOH 60°C digestion to

be studied. The mechanical properties of the flax are also affected by this digestion.

  • Viscose becomes too brittle with H2O2 digestion to

be studied. This digestion affects the mechanical properties of PA 6.6, flax and cotton.

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SLIDE 15

15

Blue curve : before KOH 10 % 60°C digestion Red curve : after KOH 10% 60°C digestion

Wavenumber (cm-1) Optical density

PET FTIR Spectra

Microplastics 2018, October 30th, Ascona, Switzerland

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SLIDE 16

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Wavenumber (cm-1) Optical density

Blue curve : before KOH 10 % 60° digestion Red curve : after KOH 10% 60° digestion

PET FTIR Spectra

Microplastics 2018, October 30th, Ascona, Switzerland

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17

1 = Not affected 2 = Slightly affected 3 = Affected 4 = Very affected

1 2 3 4

Mass Modification Linear Mass Density Microscope Observation Tenacity Elongation at break

PET

1 2 3 4

Mass Modification Linear Mass Density Microscope Observation Tenacity Elongation at break

PA 6.6

KOH 40°C KOH 60°C NaClO H2O2

1 2 3 4

Mass Modification Linear Mass Density Microscope Observation Tenacity Elongation at break

Acrylic

1 2 3 4

Mass Modification Linear Mass Density Microscope Observation Tenacity Elongation at break

Viscose

KOH 40°C KOH 60°C NaClO H2O2

Microplastics 2018, October 30th, Ascona, Switzerland

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SLIDE 18

18

Number of criteria > 3

PET PA 6.6 Acrylic Viscose Wool Flax Cotton KOH 40°C 1 5 KOH 60°C 5 1 5 1 NaClO 1 5 1 H2O2 1 2 5

1 2 3 4

Mass Modification Linear Mass Density Microscope Observation Tenacity Elongation at break

Flax

1 2 3 4

Mass Modification Linear Mass Density Microscope Observation Tenacity Elongation at break

Cotton

KOH 40°C KOH 60°C NaClO H2O2

Microplastics 2018, October 30th, Ascona, Switzerland

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19

Wool Flax Totally Dissolved, except with H2O2 Ok except with NaClO PET Strongly affected by KOH 10% 24h 60°C Viscose Affected by H2O2 but 30% 48h 50°C

Microplastics 2018, October 30th, Ascona, Switzerland

PA Slightly Affected by all digestion protocols

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SLIDE 20

20 Microplastics 2018, October 30th, Ascona, Switzerland

KOH 40°C digestion seems more relevant for 6 types of fibers. Which Digestion ? Which Fibers ?!

  • More observations with

the SEM

  • Fenton’s reagent ?

Enzymatic digestion ?

  • What will happen with

environmental fibers ? T > 60°C Not recommended

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21

10 µm

Microplastics 2018, October 30th, Ascona, Switzerland

10 µm