On the Identification of Rayon/Viscose as a Major Fraction of Microplastics in the Marine Environment: Discrimination between Natural and Manmade Cellulosic Fibers Using Fourier Transform Infrared Spectroscopy

Ionela Raluca Comnea-Stancu; Karin Wieland; Georg Ramer; Andreas Schwaighofer; Bernhard Lendl

Applied Spectroscopy
Vol. 71,
Issue 5,
pp. 939-950
(2017)

On the Identification of Rayon/Viscose as a Major Fraction of Microplastics in the Marine Environment: Discrimination between Natural and Manmade Cellulosic Fibers Using Fourier Transform Infrared Spectroscopy

Ionela Raluca Comnea-Stancu, Karin Wieland, Georg Ramer, Andreas Schwaighofer, and Bernhard Lendl

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Ionela Raluca Comnea-Stancu, Karin Wieland, Georg Ramer, Andreas Schwaighofer, and Bernhard Lendl, "On the Identification of Rayon/Viscose as a Major Fraction of Microplastics in the Marine Environment: Discrimination between Natural and Manmade Cellulosic Fibers Using Fourier Transform Infrared Spectroscopy," Appl. Spectrosc. 71, 939-950 (2017)

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Abstract

This work was sparked by the reported identification of man-made cellulosic fibers (rayon/viscose) in the marine environment as a major fraction of plastic litter by Fourier transform infrared (FT-IR) transmission spectroscopy and library search. To assess the plausibility of such findings, both natural and man-made fibers were examined using FT-IR spectroscopy. Spectra acquired by transmission microscopy, attenuated total reflection (ATR) microscopy, and ATR spectroscopy were compared. Library search was employed and results show significant differences in the identification rate depending on the acquisition method of the spectra. Careful selection of search parameters and the choice of spectra acquisition method were found to be essential for optimization of the library search results. When using transmission spectra of fibers and ATR libraries it was not possible to differentiate between man-made and natural fibers. Successful differentiation of natural and man-made cellulosic fibers has been achieved for FT-IR spectra acquired by ATR microscopy and ATR spectroscopy, and application of ATR libraries. As an alternative, chemometric methods such as unsupervised hierarchical cluster analysis, principal component analysis, and partial least squares-discriminant analysis were employed to facilitate identification based on intrinsic relationships of sample spectra and successful discrimination of the fiber type could be achieved. Differences in the ATR spectra depending on the internal reflection element (Ge versus diamond) were observed as expected; however, these did not impair correct classification by chemometric analysis. Moreover, the effects of different levels of humidity on the IR spectra of natural and man-made fibers were investigated, too. It has been found that drying and re-humidification leads to intensity changes of absorption bands of the carbohydrate backbone, but does not impair the identification of the fiber type by library search or cluster analysis.

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T. Baldinger, J. Moosbauer, and H. Sixta, . “Supermolecular Structure of Cellulosic Materials by Fourier Transform Infrared Spectroscopy (FT-IR) Calibrated by WAXS and 13C NMR”. Lenzinger Ber 2000; 79: 15–17.
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S. Navea, R. Tauler, E. Goormaghtigh, and A. de Juan, . “Chemometric Tools for Classification and Elucidation of Protein Secondary Structure from Infrared and Circular Dichroism Spectroscopic Measurements”. Proteins 2006; 63(3): 527–541.
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A. Domenighini and M. Giordano, . “Fourier Transform Infrared Spectroscopy of Microalgae as a Novel Tool for Biodiversity Studies, Species Identification, and the Assessment of Water Quality”. J. Phycol 2009; 45(2): 522–531.
M. Barker and W. Rayens, . “Partial Least Squares for Discrimination”. J. Chemom 2003; 17(3): 166–173.
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A. Celino, S. Freour, F. Jacquemin, and P. Casari, . “Characterization and Modeling of the Moisture Diffusion Behavior of Natural Fibers”. J. Appl. Polym. Sci 2013; 130(1): 297–306.
L.Y. Mwaikambo and M.P. Ansell, . “Chemical Modification of Hemp, Sisal, Jute, and Kapok Fibers by Alkalization”. J. Appl. Polym. Sci 2002; 84(12): 2222–2234.
V. Titok, V. Leontiev, S. Yurenkova, T. Nikitinskaya, T. Barannikova, and L. Khotyleva, . “Infrared Spectroscopy of Fiber Flax”. J. Nat. Fibers 2010; 7(1): 61–69.
M.L. Nelson and R.T. O’Connor, . “Relation of Certain Infrared Bands to Cellulose Crystallinity and Crystal Latticed Type. Part I. Spectra of Lattice Types I, II, III and of Amorphous Cellulose”. J. Appl. Polym. Sci 1964; 8(3): 1311–1324.
A. Célino, S. Freour, F. Jacquemin, and P. Casari, . “The Hygroscopic Behavior of Plant Fibres: A Review”. Front. Chem 2014; 1: 43.
K. Hofstetter, B. Hinterstoisser, and L. Salmen, . “Moisture Uptake in Native Cellulose – the Roles of Different Hydrogen Bonds: A Dynamic FT-IR Study using Deuterium Exchange”. Cellulose 2006; 13(2): 131–145.
A.-M. Olsson and L. Salmén, . “The Association of Water to Cellulose and Hemicellulose in Paper Examined by FTIR Spectroscopy”. Carbohydr. Res 2004; 339(4): 813–818.

2016 (1)

N. Cebi, M.Z. Durak, O.S. Toker, O. Sagdic, and M. Arici, . “An Evaluation of Fourier Transforms Infrared Spectroscopy Method for the Classification and Discrimination of Bovine, Porcine and Fish Gelatins”. Food Chem 2016; 190: 1109–1115.

2015 (2)

D.W. Lachenmeier, J. Kocareva, D. Noack, and T. Kuballa, . “Microplastic Identification in German Beer – an Artefact of Laboratory Contamination?”. Dtsch. Lebensm.-Rundsch 2015; 111(10): 437–440.

L.C. Woodall, C. Gwinnett, M. Packer, R.C. Thompson, L.F. Robinson, and G.L.J. Paterson, . “Using a Forensic Science Approach to Minimize Environmental Contamination and to Identify Microfibres in Marine Sediments”. Mar. Pollut. Bull 2015; 95(1): 40–46.

2014 (5)

G. Liebezeit and E. Liebezeit, . “Synthetic Particles as Contaminants in German Beers”. Food Addit. Contam., Part A 2014; 31(9): 1574–1578.

L.C. Woodall, A. Sanchez-Vidal, M. Canals, G.L.J. Paterson, R. Coppock, V. Sleight, A. Calafat, A.D. Rogers, B.E. Narayanaswamy, and R.C. Thompson, . “The Deep Sea is a Major Sink for Microplastic Debris”. R. Soc. Open Sci 2014; 1(4): 140317.

O. Faruk, A.K. Bledzki, H.-P. Fink, and M. Sain, . “Progress Report on Natural Fiber Reinforced Composites”. Macromol. Mater. Eng 2014; 299(1): 9–26.

A. Celino, O. Goncalves, F. Jacquemin, and S. Freour, . “Qualitative and Quantitative Assessment of Water Sorption in Natural Fibres using ATR-FTIR Spectroscopy”. Carbohydr. Polym 2014; 101: 163–170.

A. Célino, S. Freour, F. Jacquemin, and P. Casari, . “The Hygroscopic Behavior of Plant Fibres: A Review”. Front. Chem 2014; 1: 43.

2013 (5)

G. Zuckerstätter, N. Terinte, H. Sixta, and K.C. Schuster, . “Novel Insight into Cellulose Supramolecular Structure through 13C CP-MAS NMR Spectroscopy and Paramagnetic Relaxation Enhancement”. Carbohydr. Polym 2013; 93(1): 122–128.

A. Celino, S. Freour, F. Jacquemin, and P. Casari, . “Characterization and Modeling of the Moisture Diffusion Behavior of Natural Fibers”. J. Appl. Polym. Sci 2013; 130(1): 297–306.

C. Yan, B. Yang, and Z.C. Yu, . “Terahertz Time Domain Spectroscopy for the Identification of Two Cellulosic Fibers with Similar Chemical Composition”. Anal. Lett 2013; 46(6): 946–958.

A.L. Lusher, M. McHugh, and R.C. Thompson, . “Occurrence of Microplastics in the Gastrointestinal Tract of Pelagic and Demersal Fish from the English Channel”. Mar. Pollut. Bull 2013; 67(1–2): 94–99.

G. Liebezeit and E. Liebezeit, . “Non-Pollen Particulates in Honey and Sugar”. Food Addit. Contam., Part A 2013; 30(12): 2136–2140.

2011 (1)

M.A. Browne, P. Crump, S.J. Niven, E. Teuten, A. Tonkin, T. Galloway, and R. Thompson, . “Accumulation of Microplastic on Shorelines Worldwide: Sources and Sinks”. Environ. Sci. Technol 2011; 45(21): 9175–9179.

2010 (1)

V. Titok, V. Leontiev, S. Yurenkova, T. Nikitinskaya, T. Barannikova, and L. Khotyleva, . “Infrared Spectroscopy of Fiber Flax”. J. Nat. Fibers 2010; 7(1): 61–69.

2009 (1)

A. Domenighini and M. Giordano, . “Fourier Transform Infrared Spectroscopy of Microalgae as a Novel Tool for Biodiversity Studies, Species Identification, and the Assessment of Water Quality”. J. Phycol 2009; 45(2): 522–531.

2006 (2)

K. Hofstetter, B. Hinterstoisser, and L. Salmen, . “Moisture Uptake in Native Cellulose – the Roles of Different Hydrogen Bonds: A Dynamic FT-IR Study using Deuterium Exchange”. Cellulose 2006; 13(2): 131–145.

S. Navea, R. Tauler, E. Goormaghtigh, and A. de Juan, . “Chemometric Tools for Classification and Elucidation of Protein Secondary Structure from Infrared and Circular Dichroism Spectroscopic Measurements”. Proteins 2006; 63(3): 527–541.

2005 (2)

K. Bredereck and F. Hermanutz, . “Man-Made Cellulosics”. Rev. Prog. Color. Relat. Top 2005; 35(1): 59–75.

D. Klemm, B. Heublein, H.-P. Fink, and A. Bohn, . “Cellulose: Fascinating Biopolymer and Sustainable Raw Material”. Angew. Chem. Int. Ed 2005; 44(22): 3358–3393.

2004 (2)

A. Carrillo, X. Colom, J.J. Sunol, and J. Saurina, . “Structural FTIR Analysis and Thermal Characterisation of Lyocell and Viscose-Type Fibres”. Eur. Polym. J 2004; 40(9): 2229–2234.

A.-M. Olsson and L. Salmén, . “The Association of Water to Cellulose and Hemicellulose in Paper Examined by FTIR Spectroscopy”. Carbohydr. Res 2004; 339(4): 813–818.

2003 (3)

M. Barker and W. Rayens, . “Partial Least Squares for Discrimination”. J. Chemom 2003; 17(3): 166–173.

F. Carrillo, X. Colom, J. Valldeperas, D. Evans, M. Huson, and J. Church, . “Structural Characterization and Properties of Lyocell Fibers after Fibrillation and Enzymatic Defibrillation Finishing Treatments”. Text. Res. J 2003; 73(11): 1024–1030.

P. Garside and P. Wyeth, . “Identification of Cellulosic Fibres by FTIR Spectroscopy”. Stud. Conserv 2003; 48(4): 269–275.

2002 (2)

X. Colom and F. Carrillo, . “Crystallinity Changes in Lyocell and Viscose-Type Fibres by Caustic Treatment”. Eur. Polym. J 2002; 38(11): 2225–2230.

L.Y. Mwaikambo and M.P. Ansell, . “Chemical Modification of Hemp, Sisal, Jute, and Kapok Fibers by Alkalization”. J. Appl. Polym. Sci 2002; 84(12): 2222–2234.

2001 (1)

A. Stamboulis, C.A. Baillie, and T. Peijs, . “Effects of Environmental Conditions on Mechanical and Physical Properties of Flax Fibers”. Composites, Part A 2001; 32(8): 1105–1115.

2000 (1)

T. Baldinger, J. Moosbauer, and H. Sixta, . “Supermolecular Structure of Cellulosic Materials by Fourier Transform Infrared Spectroscopy (FT-IR) Calibrated by WAXS and 13C NMR”. Lenzinger Ber 2000; 79: 15–17.

1997 (1)

P.T. Larsson, K. Wickholm, and T. Iversen, . “A CP/MAS C-13 NMR Investigation of Molecular Ordering in Celluloses”. Carbohydr. Res 1997; 302(1–2): 19–25.

1964 (1)

M.L. Nelson and R.T. O’Connor, . “Relation of Certain Infrared Bands to Cellulose Crystallinity and Crystal Latticed Type. Part I. Spectra of Lattice Types I, II, III and of Amorphous Cellulose”. J. Appl. Polym. Sci 1964; 8(3): 1311–1324.

1949 (1)

P.H. Hermans and A. Weidinger, . “X-Ray Studies on the Crystallinity of Cellulose”. J. Polym. Sci 1949; 4(2): 135–144.

Ansell, M.P.

L.Y. Mwaikambo and M.P. Ansell, . “Chemical Modification of Hemp, Sisal, Jute, and Kapok Fibers by Alkalization”. J. Appl. Polym. Sci 2002; 84(12): 2222–2234.

M.P. Ansell and L.Y. Mwaikambo, “The Structure of Cotton and Other Plant Fibres”. In: S.J. Eichhorn, J.W.S. Hearle, M. Jaffe, and T. Kikutani, (eds). Handbook of Textile Fibre Structure , Cambridge, UK: Woodhead Publishing, 2009.

Arici, M.

Baillie, C.A.

A. Stamboulis, C.A. Baillie, and T. Peijs, . “Effects of Environmental Conditions on Mechanical and Physical Properties of Flax Fibers”. Composites, Part A 2001; 32(8): 1105–1115.

Baldinger, T.

Barannikova, T.

V. Titok, V. Leontiev, S. Yurenkova, T. Nikitinskaya, T. Barannikova, and L. Khotyleva, . “Infrared Spectroscopy of Fiber Flax”. J. Nat. Fibers 2010; 7(1): 61–69.

Barker, M.

M. Barker and W. Rayens, . “Partial Least Squares for Discrimination”. J. Chemom 2003; 17(3): 166–173.

Bledzki, A.K.

O. Faruk, A.K. Bledzki, H.-P. Fink, and M. Sain, . “Progress Report on Natural Fiber Reinforced Composites”. Macromol. Mater. Eng 2014; 299(1): 9–26.

Bohn, A.

D. Klemm, B. Heublein, H.-P. Fink, and A. Bohn, . “Cellulose: Fascinating Biopolymer and Sustainable Raw Material”. Angew. Chem. Int. Ed 2005; 44(22): 3358–3393.

Bredereck, K.

K. Bredereck and F. Hermanutz, . “Man-Made Cellulosics”. Rev. Prog. Color. Relat. Top 2005; 35(1): 59–75.

Browne, M.A.

Calafat, A.

Canals, M.

Carrillo, A.

A. Carrillo, X. Colom, J.J. Sunol, and J. Saurina, . “Structural FTIR Analysis and Thermal Characterisation of Lyocell and Viscose-Type Fibres”. Eur. Polym. J 2004; 40(9): 2229–2234.

Carrillo, F.

X. Colom and F. Carrillo, . “Crystallinity Changes in Lyocell and Viscose-Type Fibres by Caustic Treatment”. Eur. Polym. J 2002; 38(11): 2225–2230.

Casari, P.

A. Célino, S. Freour, F. Jacquemin, and P. Casari, . “The Hygroscopic Behavior of Plant Fibres: A Review”. Front. Chem 2014; 1: 43.

A. Celino, S. Freour, F. Jacquemin, and P. Casari, . “Characterization and Modeling of the Moisture Diffusion Behavior of Natural Fibers”. J. Appl. Polym. Sci 2013; 130(1): 297–306.

Cebi, N.

Celino, A.

A. Celino, S. Freour, F. Jacquemin, and P. Casari, . “Characterization and Modeling of the Moisture Diffusion Behavior of Natural Fibers”. J. Appl. Polym. Sci 2013; 130(1): 297–306.

Célino, A.

A. Célino, S. Freour, F. Jacquemin, and P. Casari, . “The Hygroscopic Behavior of Plant Fibres: A Review”. Front. Chem 2014; 1: 43.

Church, J.

Ciechanska, D.

D. Ciechańska, E. Wesołowska, and D. Wawro, “An Introduction to Cellulosic Fibres”. In: S.J. Eichhorn, J.W.S. Hearle, M. Jaffe, and T. Kikutani, (eds). Handbook of Textile Fibre Structure , Cambridge, UK: Woodhead Publishing, 2009.

Colom, X.

A. Carrillo, X. Colom, J.J. Sunol, and J. Saurina, . “Structural FTIR Analysis and Thermal Characterisation of Lyocell and Viscose-Type Fibres”. Eur. Polym. J 2004; 40(9): 2229–2234.

X. Colom and F. Carrillo, . “Crystallinity Changes in Lyocell and Viscose-Type Fibres by Caustic Treatment”. Eur. Polym. J 2002; 38(11): 2225–2230.

Coppock, R.

Crump, P.

Dai, D.

M. Fan, D. Dai, and B. Huang, “Fourier Transform Infrared Spectroscopy for Natural Fibres”. In: S.M. Salih, (eds). Fourier Transform – Materials Analysis , China: InTech, 2012.

de Haseth, J.A.

P.R. Griffiths and J.A. de Haseth, . Fourier Transform Infrared Spectrometry , Hoboken, NJ: John Wiley & Sons, Inc., 2006.

de Juan, A.

Domenighini, A.

Durak, M.Z.

Evans, D.

Fan, M.

M. Fan, D. Dai, and B. Huang, “Fourier Transform Infrared Spectroscopy for Natural Fibres”. In: S.M. Salih, (eds). Fourier Transform – Materials Analysis , China: InTech, 2012.

Faruk, O.

O. Faruk, A.K. Bledzki, H.-P. Fink, and M. Sain, . “Progress Report on Natural Fiber Reinforced Composites”. Macromol. Mater. Eng 2014; 299(1): 9–26.

Fink, H.P.

J. Ganster and H.P. Fink, “The Structure of Man-Made Cellulosic Fibres”. In: S.J. Eichhorn, J.W.S. Hearle, M. Jaffe, and T. Kikutani, (eds). Handbook of Textile Fibre Structure , Cambridge, UK: Woodhead Publishing, 2009.

Fink, H.-P.

O. Faruk, A.K. Bledzki, H.-P. Fink, and M. Sain, . “Progress Report on Natural Fiber Reinforced Composites”. Macromol. Mater. Eng 2014; 299(1): 9–26.

D. Klemm, B. Heublein, H.-P. Fink, and A. Bohn, . “Cellulose: Fascinating Biopolymer and Sustainable Raw Material”. Angew. Chem. Int. Ed 2005; 44(22): 3358–3393.

Freour, S.

A. Célino, S. Freour, F. Jacquemin, and P. Casari, . “The Hygroscopic Behavior of Plant Fibres: A Review”. Front. Chem 2014; 1: 43.

A. Celino, S. Freour, F. Jacquemin, and P. Casari, . “Characterization and Modeling of the Moisture Diffusion Behavior of Natural Fibers”. J. Appl. Polym. Sci 2013; 130(1): 297–306.

Galloway, T.

Ganster, J.

Garside, P.

P. Garside and P. Wyeth, . “Identification of Cellulosic Fibres by FTIR Spectroscopy”. Stud. Conserv 2003; 48(4): 269–275.

Giordano, M.

Goncalves, O.

Goormaghtigh, E.

Griffiths, P.R.

P.R. Griffiths and J.A. de Haseth, . Fourier Transform Infrared Spectrometry , Hoboken, NJ: John Wiley & Sons, Inc., 2006.

Gwinnett, C.

Hermans, P.H.

P.H. Hermans and A. Weidinger, . “X-Ray Studies on the Crystallinity of Cellulose”. J. Polym. Sci 1949; 4(2): 135–144.

Hermanutz, F.

K. Bredereck and F. Hermanutz, . “Man-Made Cellulosics”. Rev. Prog. Color. Relat. Top 2005; 35(1): 59–75.

Heublein, B.

D. Klemm, B. Heublein, H.-P. Fink, and A. Bohn, . “Cellulose: Fascinating Biopolymer and Sustainable Raw Material”. Angew. Chem. Int. Ed 2005; 44(22): 3358–3393.

Hinterstoisser, B.

Hofstetter, K.

Huang, B.

M. Fan, D. Dai, and B. Huang, “Fourier Transform Infrared Spectroscopy for Natural Fibres”. In: S.M. Salih, (eds). Fourier Transform – Materials Analysis , China: InTech, 2012.

Huson, M.

Iversen, T.

P.T. Larsson, K. Wickholm, and T. Iversen, . “A CP/MAS C-13 NMR Investigation of Molecular Ordering in Celluloses”. Carbohydr. Res 1997; 302(1–2): 19–25.

Jacquemin, F.

A. Célino, S. Freour, F. Jacquemin, and P. Casari, . “The Hygroscopic Behavior of Plant Fibres: A Review”. Front. Chem 2014; 1: 43.

A. Celino, S. Freour, F. Jacquemin, and P. Casari, . “Characterization and Modeling of the Moisture Diffusion Behavior of Natural Fibers”. J. Appl. Polym. Sci 2013; 130(1): 297–306.

Kaufman, L.

L. Kaufman and P.J. Rousseeuw, . Finding Groups in Data , Hoboken, NJ: John Wiley & Sons, Inc., 2005.

Khotyleva, L.

V. Titok, V. Leontiev, S. Yurenkova, T. Nikitinskaya, T. Barannikova, and L. Khotyleva, . “Infrared Spectroscopy of Fiber Flax”. J. Nat. Fibers 2010; 7(1): 61–69.

Klemm, D.

D. Klemm, B. Heublein, H.-P. Fink, and A. Bohn, . “Cellulose: Fascinating Biopolymer and Sustainable Raw Material”. Angew. Chem. Int. Ed 2005; 44(22): 3358–3393.

Kocareva, J.

Kuballa, T.

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