Microscopic imaging of fibre fractions from carpet tiles waste

CENTEXBEL • textile competence centre • www.centexbel.be • www.vkc.be GENT • Technologiepark 70 • BE-9052 Zwijnaarde, Belgium • phone +32 9 220 41 51 • fax +32 9 220 49 55 • [email protected] GRÂCE-HOLLOGNE • Rue du Travail 5 • BE-4460 Grâce-Hollogne, Belgium • phone +32 4 296 82 00 • [email protected] KORTRIJK • Etienne Sabbelaan 49 • BE-8500 Kortrijk, Belgium • phone +32 56 29 27 00 • fax +32 56 29 27 01 • [email protected] VAT BE 0459.218.289 • IBAN BE44 2100 4729 6545 • BIC GEBABEBB Centexbel Technologiepark 70 9052 ZWIJNAARDE Your notice of Your reference Date 10-11-2022 20-01-2023 Analysis Report 22.06007.01 Required tests : Centexbel Inspection Centexbel Determination of the emission profile by using dynamic headspace CEN ISO/TR 11827 (2016) fiber identification_recycling ISO 3451-1 (2019) Determination of the dry matter and the amount of ash ISO 1833 (2006) A quantitative analysis of mixtures of textile fibres Sample id Information given by the client Date of receipt T2222200 Aquafil 2022-10 A1 10-11-2022 T2222201 Aquafil 2022-10 A2 10-11-2022 T2222202 Aquafil 2022-10 B1 10-11-2022 T2222203 Aquafil 2022-10 B2 10-11-2022 T2222204 Aquafil 2022-10 D1 10-11-2022 T2222205 Aquafil 2022-10 D2 10-11-2022 Leen Desmet Order responsible This report may be reproduced, as long as it is presented in its entire form, without written permission of Centexbel. The results of the analysis cover the received samples. Centexbel is not responsible for the representativeness of the samples. In assessing compliance with the specifications, we did not take into account the uncertainty on the test results. Digitally signed by Centexbel Analysis Report 22.06007.01 Date 20-01-2023 Page 2/67 Comments made by Veerle Herrygers Reference: A2206007 Comments In this order, 6 samples were delivered. Each sample is a collection of fibrous and non fibrous material. The composition of the different materials was analysed. For the qualitative analysis of the fibres, the method 'fibre identification' (TR/ISO 11826) was used. Quantification of the fibres was done by the method ISO 1833. For the qualitative and quantitative analysis of the non fibrous materials, Centexbel methods are used. This is reported in the part 'inspection'. To summarise everything lcearly, a summary map was made of each sample. these can be found in the following files provided in Annex: Annex 1 schema T2222200.jpg Annex 2 schema T2222201.jpg Annex 3 schema T2222202.jpg Annex 4 schema T2222203.jpg Annex 5 schema T2222204.jpg Annex 6 schema T2222205.jpg Analysis Report 22.06007.01 Date 20-01-2023 Page 3/67 Performed in the chemical lab under the responsibility of Eddy Albrecht - microscopy - FTIR 4.1. T2222200 An overview of the sample can be seen in photo 1. Three types of non-fibrous materials were identified: a small plastic, grey chunks and darker chunks. (see photos 2, 3 & 4) Photo 1: Overview of T2222200 Reference: T2222200 - Aquafil 2022-10 A1 T2222201 - Aquafil 2022-10 A2 T2222202 - Aquafil 2022-10 B1 T2222203 - Aquafil 2022-10 B2 T2222204 - Aquafil 2022-10 D1 T2222205 - Aquafil 2022-10 D2 Inspection Date of ending the test 09-01-2022 Standard used Centexbel Apparatus A microscope with camera and image analysis with possible use of XRF-Orbis, FTIR 1. Question Search for the composition of the non-fibrous components 2. Description of the material non-fibrous components 3. Overview of the tests performed 4. Results and interpretation Analysis Report 22.06007.01 Date 20-01-2023 Page 4/67 Performed in the chemical lab under the responsibility of Eddy Albrecht Photo 2: small plastic piece in the sample Photo 3: grey chunks in the sample Photo 4: darker chunks in the sample Analysis Report 22.06007.01 Date 20-01-2023 Page 5/67 Performed in the chemical lab under the responsibility of Eddy Albrecht Microscopic examination: - plastic: polymer film - grey chunk: non-fibrous material + small synthetic fibres - darker chunk: non-fibrous material + small synthetic fibres The microscopic examination can be found in photos 5, 6 & 7. FTIR examination: - plastic: polyethylene spectrum - grey chunk: polyethylene + polyacrylate + calcium carbonate spectra - darker chunk: polyethylene + polyacrylate + calcium carbonate spectra Conclusion: polyethylene + polyacrylate + calcium carbonate Photo 5: microscopic image of a platic piece. Analysis Report 22.06007.01 Date 20-01-2023 Page 6/67 Performed in the chemical lab under the responsibility of Eddy Albrecht Photo 6: microscopic image of a grey chunk Photo 7: microscopic image of a darker chunk Analysis Report 22.06007.01 Date 20-01-2023 Page 7/67 Performed in the chemical lab under the responsibility of Eddy Albrecht 4.1. T2222201 An overview of the sample can be seen in photo 8. Five types of non-fibrous materials were identified: a small plastic, brown chunks, black chunks, wooden chips and white flakes. (see photos 9-13) Photo 8: Overview of T2222201 Photo 9: Small plastic piece in the sample Analysis Report 22.06007.01 Date 20-01-2023 Page 8/67 Performed in the chemical lab under the responsibility of Eddy Albrecht Photo 10: brown chunk in the sample Photo 11: black chunk in the sample Photo 12: wood chip Analysis Report 22.06007.01 Date 20-01-2023 Page 9/67 Performed in the chemical lab under the responsibility of Eddy Albrecht Photo 13: white flake Microscopic examination: - plastic: polymer film - brown chunk: non-fibrous material + small clear synthetic fibres - black chunk: non-fibrous material + small clear synthetic fibres - wood chip: wood chip - white flake: non-fibrous material The microscopic examination can be found in photos . FTIR examination: - plastic: polyethylene spectrum - brown chunk: calcium carbonate + poly(vinylacetate) spectrum - black chunk: calcium carbonate spectrum + a polyolefine (polyisoprene) - wood chip: cellulose spectrum - white flake: calcium carbonate + polystyrene + cellulose spectrum Conclusion: calcium carbonate + polyisoprene + poly(vinylacetate) + traces of polyethylene, polystyrene and wood Analysis Report 22.06007.01 Date 20-01-2023 Page 16/67 Performed in the chemical lab under the responsibility of Eddy Albrecht Microscopic examination: - black rubber: non-fibrous material - yellow rubber: non-fibrous material - clear chunk: non-fibrous material - grey chunk: non-fibrous material The microscopic examination can be found in photos . FTIR examination: - black rubber: poly(butadiene:acrylonitrile) + phthalate spectrum - yellow rubber: talc + calciumcarbonate + poly(butadiene:acrylonitrile) spectrum - clear chunk: poly(acrylate:styrene) spectrum - grey chunk: talc + calcium carbonate + polyester spectrum Conclusion: poly(butadiene:acrylonitrile) + traces of phthalate, talc, calcium carbonate, polyester and poly(acrylate:styrene) Analysis Report 22.06007.01 Date 20-01-2023 Page 17/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 26: Microscopic image of the black rubber photo 27: Microscopic image of the yellow rubber Analysis Report 22.06007.01 Date 20-01-2023 Page 18/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 28: Microscopic image of the clear chunk photo 29: Microscopic image of the grey chunk Analysis Report 22.06007.01 Date 20-01-2023 Page 19/67 Performed in the chemical lab under the responsibility of Eddy Albrecht 4.1. T2222205 An overview of the sample can be seen in photo 30. One type of non-fibrous component was identified: black rubber. (see photo 31) Photo 30: Overview of T2222205 photo 31: black rubber Analysis Report 22.06007.01 Date 20-01-2023 Page 20/67 Performed in the chemical lab under the responsibility of Eddy Albrecht Microscopic examination: - black rubber: non-fibrous material The microscopic examination can be found in photos . FTIR examination: - black rubber: poly(butadiene:acrylonitrile) + phthalate spectrum Conclusion: poly(butadiene:acrylonitrile) + traces of phthalate photo 32: Microscopic image of the black rubber Analysis Report 22.06007.01 Date 20-01-2023 Page 21/67 Performed in the chemical lab under the responsibility of Pablo Moerman Amount of sample: 21 –mg In figure 1 the chromatograms of the dynamic headspace (DHS) analysis for the samples have been compared. The emissions are quite low certainly for the stain. For A1 and A2 emissions are low without pronounced plasticisers. For D1 however a big peak for DOTP (even though this substance is heavy) is present. For A2 traces of DiBP and DBP are present. For A1 a small caprolactam peak is present along with some heavier n-alkanes. For A2 some antioxidant related (degradation products) are also visible. For D1 more peaks are present like benzothiazol, caprolactam and a cluster of acetophenone derivatives in the VOC region. A small diethylphthalate peak is also present. A series of substituted azulenes is present which may relate to PAHs. This is confirmed looking at fig 3: the specific ion 202 typical for eg fluoranthene and pyrene is present for D1. For the other samples only spikes are visible. In fig 4 a range of specific masses for PAHs (128naphtalene; 178 for anthracene and phenanthrene, 202 and 228 for heavier substances like eg chrysene) is combined with the TIC chromatogram. This shows that very low amounts of the lighter PAHs are present. Reference: T2222200 - Aquafil 2022-10 A1 T2222201 - Aquafil 2022-10 A2 T2222204 - Aquafil 2022-10 D1 Determination of the emission profile by using dynamic headspace Date of ending the test 12-12-2022 Standard used Centexbel Sample preparation 10-100mg sample is heated in a headspace vial at a fixed temperature. After incubation an inert gas flow leads the air out of the vial over a tenax filled tube where volatile organic compounds (VOC’s) are trapped. The tenax tube with the VOC’s is thermally desorbed. Released VOC’s are cryo trapped and injected into a GCMS. Analytical method Gas chromatography with Agilent MSD detector Results Determination limit 1 mg/kg Analysis Report 22.06007.01 Date 20-01-2023 Page 22/67 Performed in the chemical lab under the responsibility of Pablo Moerman 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 0 1000000 2000000 3000000 4000000 5000000 6000000 7000000 8000000 Time--> Abundance TIC: T2222200_6_DHS01.D\data.ms Aquafil 2022-10 A1 ester n-octadecane caprolactam VOC <->SVOC n-C16 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 0 1000000 2000000 3000000 4000000 5000000 6000000 7000000 8000000 Time--> Abundance TIC: T2222201_6_DHS01.D\data.ms Aquafil 2022-10 A2 2,6-Di-tert-butyl-4-hydroxy-4-methylcyclohexa-2,5-dien-1-one DBP DiBp antiox degrad 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 0 1000000 2000000 3000000 4000000 5000000 6000000 7000000 8000000 Time--> Abundance TIC: T2222204_6_DHS01.D\data.ms Aquafil 2022-10 D1 ethylhexanol 4-Isopropylacetophenone Ethanone, 1-[4-(1-hydroxy-1-methylethyl)phenyl]- alkylazulene n-C17 caprolactam benzothiazole DOTP diethylphthalate Fig 1: Total ion (TIC) chromatograms of the dynamic headspace (DHS) analysis of the samples Analysis Report 22.06007.01 Date 20-01-2023 Page 23/67 Performed in the chemical lab under the responsibility of Pablo Moerman 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 0 1000000 2000000 3000000 4000000 Time--> Abundance Ion 149.00 (148.70 to 149.70): T2222200_6_DHS01.D\data.ms A1 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 0 1000000 2000000 3000000 4000000 Time--> Abundance Ion 149.00 (148.70 to 149.70): T2222201_6_DHS01.D\data.ms A2 DiBP DBP 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 0 1000000 2000000 3000000 4000000 Time--> Abundance Ion 149.00 (148.70 to 149.70): T2222204_6_DHS01.D\data.ms D1 DOTP diethylphthalte Fig 2: single ion chromatograms for the specific mass 149 typical for orthoand terephthalates Analysis Report 22.06007.01 Date 20-01-2023 Page 24/67 Performed in the chemical lab under the responsibility of Pablo Moerman 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 0 5000 10000 15000 20000 25000 30000 35000 Time--> Abundance Ion 202.00 (201.70 to 202.70): T2222200_6_DHS01.D\data.ms A1 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 0 5000 10000 15000 20000 25000 30000 35000 Time--> Abundance Ion 202.00 (201.70 to 202.70): T2222201_6_DHS01.D\data.ms A2 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 0 5000 10000 15000 20000 25000 30000 35000 Time--> Abundance Ion 202.00 (201.70 to 202.70): T2222204_6_DHS01.D\data.ms D1 pyrene Fig 3: single ion chromatograms for the specific mass 202 typical for pyrene and fluoranthene Analysis Report 22.06007.01 Date 20-01-2023 Page 25/67 Performed in the chemical lab under the responsibility of Pablo Moerman 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 50000 100000 150000 200000 Time--> Abundance Ion 128.00 (127.70 to 128.70): T2222204_6_DHS01.D\data.ms naphthalene 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 50000 100000 150000 200000 Time--> Abundance Ion 178.00 (177.70 to 178.70): T2222204_6_DHS01.D\data.ms phenanthrene 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 50000 100000 150000 200000 Time--> Abundance Ion 202.00 (201.70 to 202.70): T2222204_6_DHS01.D\data.ms fluoranthene pyrene 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 50000 100000 150000 200000 Time--> Abundance Ion 228.00 (227.70 to 228.70): T2222204_6_DHS01.D\data.ms 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 50000 100000 150000 200000 Time--> Abundance TIC: T2222204_6_DHS01.D\data.ms Fig 4: Single ion chromatograms for PAH specific ions combined with the total ion chromatogram for sample D1 Analysis Report 22.06007.01 Date 20-01-2023 Page 32/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 1: Overview of the sample Reference: T2222201 - Aquafil 2022-10 A2 Fiber identification_recycling Date of ending the test 10-01-2022 Based on CEN ISO/TR 11827 (2016) Apparatus and techniques Macroscopic and microscopic examination + solubility test + FTIR Results Macroscopic identification of the sample: Analysis Report 22.06007.01 Date 20-01-2023 Page 33/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 2: small red yarn photo 3: loose fibres Analysis Report 22.06007.01 Date 20-01-2023 Page 34/67 Performed in the chemical lab under the responsibility of Eddy Albrecht Longitudinal view: small red yarn: red trilobal fibres loose fibres: black synthetic fibres trilobal fibres (black and red) natural fibres (cotton) fibres in brown chunks: clear synthetic fibres fibres in black chunks: clear synthetic fibres Dissolution test: The small red yarn dissolves fully in formic acid. FTIR: small red yarn: polyamide spectrum loose fibres: polyamide + polyester spectrum fibres in brown chunks: glass fibre fibres in black chunks: glass fibre Conclusion: Polyamide + polyester + traces of cotton and glass fibre Identified fibers: Analysis Report 22.06007.01 Date 20-01-2023 Page 35/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 4: microscopic image of the small red yarn photo 5: microscopic image of the loose fibres photo 6: second microscopic image of the loose fibres Analysis Report 22.06007.01 Date 20-01-2023 Page 36/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 7: third microscopic image of the loose fibres Analysis Report 22.06007.01 Date 20-01-2023 Page 37/67 Performed in the chemical lab under the responsibility of Eddy Albrecht Reference: T2222201 - Aquafil 2022-10 A2 Determination of the dry matter and the amount of ash Date of ending the test 04-01-2023 Based on ISO 3451-1 (2019) Apparatus Oven and muffle furnace Number of hours in muffle furnace at 550°C 3 Number of hours in muffle furnace at 1000°C 2 Results and interpretation Analysis executed in double T2222201 @2 1 2 1 2 % dry matter 100 101 Weight of residue at 550°C On wet compound (%) 72.23 68.95 On dry matter (%) 72.17 68.54 Weight of residue at 1000°C On wet compound (%) 47.83 43.89 On dry matter (%) 47.79 43.63 CO2 loss on dry matter (%) 24.38 24.91 CaCO3 On wet compound (%) 55.45 56.96 On dry matter (%) 55.41 56.62 Analysis Report 22.06007.01 Date 20-01-2023 Page 38/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 1: Overview of the sample Reference: T2222202 - Aquafil 2022-10 B1 Fiber identification_recycling Date of ending the test 10-01-2023 Based on CEN ISO/TR 11827 (2016) Apparatus and techniques Macroscopic and microscopic examination + solubility test + FTIR Results Macroscopic identification of the sample: Analysis Report 22.06007.01 Date 20-01-2023 Page 39/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 2: grey yarn photo 3: light grey yarn photo 4: yellow yarn Analysis Report 22.06007.01 Date 20-01-2023 Page 40/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 5: small red yarn photo 6: multicolour yarn Analysis Report 22.06007.01 Date 20-01-2023 Page 41/67 Performed in the chemical lab under the responsibility of Eddy Albrecht Longitudinal view: grey yarn: trilobal fibres light grey yarn: trilobal fibres yellow yarn: trilobal fibres small red yarn: trilobal fibres black synthetic fibres multicolour yarn: trilobal fibres (black, green and white) Dissolution test: All yarns dissolve completely in formic acid. However, a residue of non-fibrous components remains after dissolving the grey, light grey and yellow yarns. FTIR grey yarn: polyamide spectrum light grey yarn: polyamide spectrum yellow yarn: polyamide spectrum small red yarn: polyamide spectrum multicolour yarn: polyamide spectrum Conclusion polyamide Identified fibers: Analysis Report 22.06007.01 Date 20-01-2023 Page 48/67 Performed in the chemical lab under the responsibility of Eddy Albrecht Longitudinal view: multicolour yarn: trilobal fibres (green, white and black) black and white yarn: trilobal fibres small red yarn: trilobal fibres black synthetic fibres Dissolution test: All yarns dissolve completely in formic acid. However, a residue of non-fibrous components remains after dissolving the mulitcolour and black and white yarns. FTIR: multicolour yarn: polyamide spectrum black and white yarn: polyamide spectrum small red yarn: polyamide spectrum Conclusion: polyamide photo 5: Microscopic image of the multicolour yarn (white and green fibres) Identified fibers: Analysis Report 22.06007.01 Date 20-01-2023 Page 49/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 6: microscopic image of the multicolour yarn (black fibres) photo 7: microscopic image of the black and white yarn Analysis Report 22.06007.01 Date 20-01-2023 Page 50/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 8: microscopic image of the black and white yarn photo 9: microscopic image of the small red yarn Analysis Report 22.06007.01 Date 20-01-2023 Page 51/67 Performed in the chemical lab under the responsibility of Eddy Albrecht Reference: T2222203 - Aquafil 2022-10 B2 Determination of the dry matter and the amount of ash Date of ending the test 11-01-2023 Based on ISO 3451-1 (2019) Apparatus Oven and muffle furnace Number of hours in muffle furnace at 550°C 3 Number of hours in muffle furnace at 1000°C 2 Results and interpretation Analysis executed in double T2222203 1 2 % dry matter 97.7 97.6 Weight of residue at 550°C On wet compound (%) 12.79 10.77 On dry matter (%) 13.10 11.03 Weight of residue at 1000°C On wet compound (%) 8.26 6.20 On dry matter (%) 8.45 6.35 CO2 loss on dry matter (%) 4.64 4.69 CaCO3 On wet compound (%) 10.30 10.40 On dry matter (%) 10.55 10.65 Analysis Report 22.06007.01 Date 20-01-2023 Page 52/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 1: Overview of the sample Reference: T2222204 - Aquafil 2022-10 D1 Fiber identification_recycling Date of ending the test 10-01-2023 Based on CEN ISO/TR 11827 (2016) Apparatus and techniques Macroscopic and microscopic examination + solubility test + FTIR Results Macroscopic identification of the sample: Analysis Report 22.06007.01 Date 20-01-2023 Page 53/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 2: black fibres imbedded in rubber photo 3: grey fibres imbedded in rubber photo 4: red yarn Analysis Report 22.06007.01 Date 20-01-2023 Page 54/67 Performed in the chemical lab under the responsibility of Eddy Albrecht Longitudinal view: black fibres imbedded in rubber: black synthetic fibres grey fibres imbedded in rubber: natural fibres (cotton) red yarn: monofilament Dissolution test: The black fibres imbedded in rubber dissolve completely in trichloroacetic acid. The grey fibres imbedded in rubber dissolve completely in sulphuric acid. The red yarn dissolves completely in formic acid. FTIR: black fibres inbedded in rubber: polyester spectrum grey fibres inbedded in rubber: cellulose spectrum red yarn: polyamide spectrum Conclusion: traces of polyester, cotton and polyamide Identified fibers: Analysis Report 22.06007.01 Date 20-01-2023 Page 55/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 5: Microscopic image of the black fibres imbedded in rubber photo 6: Microscopic image of the grey fibres imbedded in rubber Analysis Report 22.06007.01 Date 20-01-2023 Page 56/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 7: Microscopic image of the red yarn Analysis Report 22.06007.01 Date 20-01-2023 Page 57/67 Performed in the chemical lab under the responsibility of Eddy Albrecht Reference: T2222204 - Aquafil 2022-10 D1 Determination of the dry matter and the amount of ash Date of ending the test 17-01-2023 Based on ISO 3451-1 (2019) Apparatus Oven and muffle furnace Number of hours in muffle furnace at 550°C 3 Number of hours in muffle furnace at 1000°C 4 Results and interpretation Analysis executed in double T2222204 1 2 % dry matter 99.6 99.7 Weight of residue at 550°C On wet compound (%) 36.77 37.91 On dry matter (%) 36.90 38.04 Weight of residue at 1000°C On wet compound (%) 4.67 3.67 On dry matter (%) 4.69 3.68 CO2 loss on dry matter (%) 32.21 34.36 CaCO3 On wet compound (%) 72.95 77.82 On dry matter (%) 73.21 78.09 Analysis Report 22.06007.01 Date 20-01-2023 Page 64/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 10: Microscopic image of the small white yarn photo 11: Microscopic image of the small white yarn Analysis Report 22.06007.01 Date 20-01-2023 Page 65/67 Performed in the chemical lab under the responsibility of Eddy Albrecht photo 12: Microscopic image of the small white yarn after dissolving in formic acid/ZnCl2 photo 13: Microscopic image of the loose blue fibres Analysis Report 22.06007.01 Date 20-01-2023 Page 66/67 Performed in the chemical lab under the responsibility of Eddy Albrecht Reference: T2222205 - Aquafil 2022-10 D2 Determination of the dry matter and the amount of ash Date of ending the test 19-01-2023 Based on ISO 3451-1 (2019) Apparatus Oven and muffle furnace Number of hours in muffle furnace at 550°C 3 Number of hours in muffle furnace at 1000°C 2 Results and interpretation Analysis executed in double T2222205 1 2 % dry matter 98.0 98.1 Weight of residue at 550°C On wet compound (%) 3.77 2.56 On dry matter (%) 3.84 2.61 Weight of residue at 1000°C On wet compound (%) 1.35 1.28 On dry matter (%) 1.37 1.30 CO2 loss on dry matter (%) 2.47 1.31 CaCO3 On wet compound (%) 5.50 2.92 On dry matter (%) 5.61 2.98 Analysis Report 22.06007.01 Date 20-01-2023 Page 67/67 Performed under accreditation in the chemical lab under the responsibility of Eddy Albrecht Reference: T2222205 - Aquafil 2022-10 D2 A quantitative analysis of mixtures of textile fibres Date of ending the test 18-01-2023 Standard used ISO 1833 (2006) Deviation from the standard The cotton and viscose fibres were dissolved at the same time. The amount present of both fibres is to low to accurately determine. Mixture polyamide - cotton - polyester We work according to the method variation 4. On one analysis sample, successively the first and then the second component are dissolved. Pretreatement Soxhlet extraction with light petroleum ether, followed by rinsing with cold and hot water Method dissolution test 1 ISO1833-7 (formic acid) Method dissolution test 2 ISO1833-11 (sulfuric acid 75%, 50°C) Remark Results A. Calculation based on clean dry mass polyamide cotton polyester 85.48 % 1.30 % 13.21 % 85.84 % 1.25 % 12.91 % Average 85.7 % 1.3 % 13.1 % B. Calculation based on clean dry mass with agreed allowances for the moisture Agreed allowance for moisture polyamide 5.75% Agreed allowance for moisture cotton 8.50% Agreed allowance for moisture polyester 1.50 % polyamide cotton polyester Average 86.1 % 1.3 % 12.6 %