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BOOK OF ABSTRACTS Organized by

Foreword

Dear contributors to the EPNOE Junior 2018. We would like to warmly welcome you in Slovenia and

are very greatful that you decided to share your valueable research results within the scientific

community on this occasion. The format of this conference was especially developed for young

researchers who are in the stage of developing their own carreer and research fields. It should bring

about new ideas, contacts and collaborations in an extremely divers and important area. It should also

provide an opportunity for young investigators to aquire new skills and knowledge and meet or make

friends in a jovial atmosphere. We therefore strived for combining food, technical, biomedical and

basic research topics into one conference which might be seen as a challenging task. In our opinion it

only demonstrates the versatility and significance of polysaccharides and matter composed of them.

The introductory lectures reflect this versatility, rangeing from wood based construction that

influences how our houses are made, to biomedical research that helps us cureing diseases. It covers

"sweet" organic synthesis and the thermodynamics of surfaces that is not only important in modern

composite materials. All lectures - and almost all food - of this conference however involve polymers

with the famous glycosidic bond, which brings about many of the peculiar properties everyone of us

dedicates most of the time to. We think that the diversity of these biomolecules and their derivatives

still bears tremendous opportunities and hope to provide you with a platform for the development of

new ideas and friendship with this conference. Have a good time and enjoy your stay.

Karin Stana Kleischek

Head of the Laboratory for Characterization and Processing of Polymers

Rupert Kargl

Chair of the Organizing Committee

Team involved in the organization of the conference:

Patrick Navard, President of EPNOE

Sylvie Massol, Secretary of EPNOE

LPCC: Manja Kurečič; Matej Bračič, Alenka Ojstršek, Zdenka Peršin, Silvo Hribernik; Mojca Božič; Tina

Maver; Tanja Pivec, Tanja Kos, Doris Tkaučič, Tamilselvan Mohan, Olivija Plohl, Martin Thonhofer,

Urška Jančič, Ana Bratuša, Barbara Kaker, Natalija Virant

© EPNOE Association and LCPP, 2018

LCPP consists of 20 people rangeing from skilled lab technicians to master and doctoral students,

postdocs, assistant and full professors. The main activities of LCPP include basic and applied R&D

connected to polymeric materials and especially polysaccharides which are used in many industrial

and biomedical applications. Special attention is given to the study of surface and structural

parameters of fibres, films, membranes, porous materials or powders. Correlations between the

surface/structural parameters and their properties, reactivity or interaction capacity are established.

New and ecologically friendly processes are developed with non-state of the art techniques among

them 3D printing and electrospinning. LCPP is collaborating on national and international scientific

and educational levels within several organizations. It is a member of EPNOE - The European

Polysaccharide Network of Excellence, POLIMAT – Centre of Excellence Polymer Materials and

Technologies, AUTEX - Association of Universities for Textile, EURATEX - European Technology

Platform for the Future of Textiles and Clothing. Our team is active in regional research activities

among neighboring Universities (Graz University of Technology, Karl Franzens University of Graz,

Montanuniversität Leoben, University of Primorska, Institute Jožef Stefan etc.) and embedded into

the international research community of polysaccharides and polymers over various EU and national

projects.

Abstract #

07:00 08:30 Registration Hallway 1st floor Slomškov Trg 15

08:30 Welcome - Vice Dean for Research - Faculty of Mechanical Engineering Simona Strnad

08:40 Welcome - Head of LCPP Karin Stana Kleinschek

08:45 Welcome - President of EPNOE Patrick Navard

08:55 Research at LCPP - organisational Rupert Kargl

09:05 Enabling technologies - the core assets of BioNanoNet network Andreas Falk 1

09:40 Thermodynamics of adsorption at nanocellulose surfaces Wim Thielemans 210:15 10:30 Poster and Coffee break room Antona Trstenjaka

10:30 Potential of fibrillated cellulose in papermaking. Looking for optimal conditions of fibrillation and addition rate to maximize paper performancesJulie BOSSU 3

10:50 Investigation of dissolution process of cellulose in NaOH-urea (system) and effect of regenerated material on properties of paper Velta Fridrihsone 4

11:10 Nanocellulose papers from elephant manure Andreas Mautner 5

11:30 From surface modification of cellulosic materials to paper-based biosensors Thomas Elschner 6

11:50 All-cellulose composites based on paper fines for energy storage devices Mathias A. Hobisch 7

12:10 13:10 Lunch in room Antona Trstenjaka

13:10 Up-scaling bioplastic formulations: from solvent casting to extrusion and injection processes Idalina Gonçalves 8

13:30 Lignocellulosic residues pretreatment with reactive extrusion using enzymes - Influence of process conditions on subsequent enzymatic hydrolysisEtienne Gatt 9

13:50 Reactive extrusion Alexander Feldner 10

14:10 Electrospinning water-soluble/insoluble polymer blends Timo Grothe 11

14:30 Microphase separation of cellulose derivates Gundula Teichert 12

14:50 16:00 Foto in front of the building - Poster session and Coffee break in room Antona Trstenjaka

16:00 Gas-esterification of cellulose particles for the production of PHBV based biocomposites Grégoire DAVID 13

16:20 Influence of low-pressure oxygen plasma on properties of hemp fibres (Cannabis sativa) Marija Gorjanc 14

16:40 Flame retardancy of flax fabrics by radiografting of phosphorus compounds Raymond Hajj 15

17:00 How is cellulose affected during the X-rays examination of manuscripts? Alice Gimat 16

17:20 Incorporation of Nanoparticles into Cellulose Matrices using Femtosecond Laser Pulses Werner Schlemmer 17

19:30 22:00 Dinner - Gostilna Maribor - Glavni trg 8

10:30 ENTIRELY BIO-SOURCED NANOCOMPOSITES FOR THE ELABORATION OF BIOMATERIALS Veronica Nessi 18

10:50 New composites for basic GTR principles: employment of nature- derived and bio-inspired materials in periodontal treatment Selestina Gorgieva 19

11:10 Definition of optimal “active” material for bio-printing through analyzing the thin films Tina Maver 20

11:30 A preliminary study of material suitability for growth of pancreatic cells Marko Milojevic 21

11:50 Alternative sigma factor F (SigF) regulates secretion and production of extracellular polysaccharides in Synechocystis sp. PCC 6803 Carlos Flores 22

12:10 13:10 Lunch in room Antona Trstenjaka

13:10 Dextran formamidines: A new and easily synthesizable non-viral vector in gene delivery Konrad Hotzel 23

13:30 Approaches for the derivatization of polyols with amino acids Ana Bratuša 24

13:50 Dextran-based hydrogels matrixes for biomedical applications - synthesis and characterization Kamila J. Szafulera 25

14:10 Pullulan-based microneedles for transdermal delivery of pharmaceutical ingredients Daniela F. S. Fonseca 26

14:30 Functional and Material Properties of a Novel Microcrystalline Cellulose for Drug Delivery Lalduhsanga Pachuau 27

14:50 16:00 Foto - Poster session and Coffee break in room Antona Trstenjaka

16:00 Isolation and purification of high molecular weight chitin from shrimp shells using deep eutectic solvents Bojana Bradic 28

16:20 Thermodynamic study of the interaction of various salts with cellulose nanocrystals Salvatore Lombardo 29

16:40 Surface treatment of chitosan fibers with polypyrrole Elena Dresvyanina 30

17:00 Mimicking biological mechanical behavior by a bioactive lactose-modified chitosan Franco Furlani 31

17:20 Electrospun cellulose acetate nanofibrous mats for detection of pH in the wound bed Natalija Virant 32

17:40 Development of cellulose wound dressing materials with rutin and polyrutin Tanja Pivec 33

19:30 22:00 Dinner - Gostilna Maribor - Glavni trg 8

Polysaccharides in technical applications - Chair: Stefan Spirk

Polysaccharides in technical applications - Chair: Martin Gericke

Monday 14th of May 2018

Room Frana Miklošiča

Room Frana Miklošiča - Chair: Rupert Kargl

Room Borisa PodreccePolysaccharides in biomedical applications - Chair: Yves Verhertbruggen

Polysaccharides in biomedical applications - Chair: Marco Beaumont

Polysaccharides in technical applications - Chair: Nicolas Le Moigne

Polysaccharides in biomedical applications - Chair: Zélia Alves

Abstract #

08:30 09:05 InnoRenew CoE Renewable Materials and Healthy Environments Research and Innovation Centre of Excellence  Črtomir Tavzes 34

09:05 09:40 Monosaccharide chemistry Martin Thonhofer 3509:40 10:00 Poster and coffee break in room Antona Trstenjaka

10:00 The influence of zinc oxide nanorods on chitosan-based film properties for food packaging Zélia Alves 36

10:20 The influence of neutralization on the properties and structure of chitosan films Urška Jančič 37

10:40 Physical, antioxidant and antimicrobial properties of chitosan-based films incorporated with hop extract Marijan Bajić 38

11:00 Starch films reinforced with broccoli by-products with antioxidant activity Sónia S. Ferreira 39

11:20 Development of chitosan/graphene oxide composites for potential application as anion-exchange membranes in fuel cells Barbara Kaker 40

11:40 Novel chitosan-based silica-coated magnetic nanocomposites as a potential adsorbent for heavy metals Olivija Plohl 4112:00 13:00 Lunch in room Antona Trstenjaka

13:00 Anisotropic Diffusion and Phase Behaviour of Cellulose Nanocrystal Suspensions Jonas Van Rie 42

13:20 Water vapor diffusivity estimation in a polydisperse sample of micrometric size cellulose particles Valentin Thoury 43

13:40 Nanofibrillated cellulose stabilized Pickering emulsion as templates for thermal superinsulating materials Clara Jimenez Saelices 44

14:00 Making bio-based materials from microalgae : solvent and plasticization routes Nicolas Le Moigne 45

14:20 Insights in electrostatic interactions between cationic modified cellulose and microalgae An Verfaillie 46

14:40 Cellulose metal sulfide based nanocomposite thin films Michael Weißl 4715:00 15:20 Poster and coffee break in room Antona Trstenjaka

15:20 Nanocellulose from citrus peel residue: A sustainable biorefinery approach Eduardo M. de Melo 48

15:40 From structure to functionality: an initial approach towards the application of the galactomannans extracted from Prosopis affinis Pilar Vilaró 49

16:00 Identification and characterisation of Micro-fibrillated cellulose (MFC) from pea fibre food waste. Jade Phillips 50

16:20 Break

17:00 17:30 Prizes and awards closing ceremony Organizers

10:00 Tailor-Made Polysaccharides with Defined Substitution Pattern by Enzymatic Polymerization of Arabinoxylan Oligosaccharides Deborah Senf 51

10:20 Investigations towards the Synthesis of Bismuth-sugar conjugates Martin Thonhofer 52

10:40 Polysaccharide Carbonates as Intermediates for Modular Synthesis Approaches Martin Gericke 53

11:00 Efficient solvent-free preparation of amidified carboxymethyl cellulose derivatives: study of the structure-properties relationships Asja Pettignano 54

11:20 Polysaccharide based 3D scaffolds: preparation, characterization, and application Tamilselvan Mohan 55

11:40 Functionalization of never-dried Nanocelluloses Marco Beaumont 56

12:00 13:00 Lunch in room Antona Trstenjaka

13:00 The potential of electrochemical methods in analysis of natural polysaccharides Slađana Strmečki Kos 57

13:20 Responsive chitosan/surfactant complexes for different applications Leonardo Chiappisi 58

13:40 The impact of the hemicellulose acetylation on interactions with model cellulose surfaces: a QCM-D study Zahraa Jaafar 59

14:00 Formation of Ethyl Cellulose Particles: Influence of Different Surface Active Polysaccharide Derivates and Particle Formation Methods Doris Tkaučič 60

14:20 Investigation of the decomposition process of cellulose during oxidation with ammonium persulfate Inese Filipova 61

14:40 RELATIONSHIP BETWEEN DEGREE OF SUBSTITUTION AND VISCOSITY OF CATIONIC STARCH Denys Zalyvchyi 62

15:00 15:20 Poster and coffee break in room Antona Trstenjaka

15:20 Coupling of alginate isolation with alternative method for polyphenol extraction from brown seaweed Laminaria Hyperborea Miša Mojca Cajnko 63

15:40 Does mannan interact with arabinogalactan proteins and impact wheat endosperm development? Yves Verhertbruggen 64

16:00 Kraft lignin as a modifier and binder: Esterification of lignin Matej Bračič 65

16:20 Break

17:00 17:30 Prizes and awards closing ceremony Organizers

Polysaccharides in technical applications - Chair: Andreas Mautner

Tuesday 15th of May 2018

Room Frana Miklošiča

Polysaccharides in technical applications - Chair: Franco Furlani

Polysaccharides in basic science - Chair: Silvo Hribernik

Room Frana Miklošiča - Chair: Matej Bračič

Room Frana Miklošiča

Polysaccharides in basic science - Chair: Thomas Elschner

Polysaccharides in basic science - Chair: Wim Thielemans

Polysaccharides in food science - Chair: Celestina Gorgieva

Room Frana Miklošiča

Room Borisa Podrecce

P1 Fractionation and structural analysis of polysaccharides from Chlorella vulgaris G11 biomass Leonid Sushytskyi food

P2 Redesign of collagen sausage casings for high quality performance using food grade polysaccharides Motolani Sobanwa food

P3 Chitin as a renewable source for the production of smart food packaging materials Bojana Bradic technical application

P4 Gelatin/PAN as a polymer blend for electrospinning Daria Wehlage technical application

P5 Influence of xylan on ions of 1-ethyl-3-methylimidazolium acetate solution Wafa Ezzawam technical application

P6 MATUROLIFE - Metallisation of Textiles to make Urban living for Older people more Independent and Fashionable Alenka Ojstršek technical application

P7 Oil encapsulation in core-shell alginate capsules using droplets based millifluidic Mariana Pereda technical application

P8 Using phenolics from potato peels for the production of active starch-based films Joana Lopes technical application

P9 Development and characterization of novel electrospun matrices with embedded CNC for air filtration Manja Kurečič technical application

P10 A comparative study of sample preparation for staining and immunodetection of plant cell walls by light microscopy Yves Verhertbruggen basic science

P11 A comprehensive approach to the analysis of anhydrosaccharides in wood pyrolysis products Kristine Meile basic science

P12 Fungal biomass polysaccharides: extraction of side stream from enzyme production Ida Nikkilä basic science

P13 Gas chromatographic-mass spectrometric determination of selected monosaccharides in wood hemicellulose samples Mitja Kolar basic science

P14 Lytic polysaccharide monooxygenases (LPMOs) as novel tools for the preparation of innovative nanocelluloses Amani Chalak basic science

P15 The improvement of wet spinning of chitosan fibers Ekaterina Maevskaia basic science

P16 Comparison of bacterial cellulose yield in two strains of Gluconacetobacter xylinus in Hestrinn-Schramm and molasses media Ceren Sagdic Oztan basic science

P17 Thin Films from Acetylated Lignin Stefanie Müller basic science

P18 Coated Cellulose Interface as Substrate for Dynamic Observation of Protein Adhesion and Coupling Processes with Liquid Atomic Force Microscopy Krisztina Zajki-Zechmeister basic science

P19 Determination of Surface Fractions of Cellulose Thin Films Carina Sampl basic science

P20 Bacterial cellulose on bioelectronics for the study and treatment of neurodegenerative disorders Tiago Carvalho biomedical application

P21 Bioresorption of porous three-dimensional chitosan-based matrices Pavel Popryadukhin biomedical application

Poster Monday 14th of May 14:50 - 16:00 - Antona Trstenjaka

Monday 14th of May 2018

ROOM FRANA MIKLOŠIČA

Enabling technologies - the core assets of BioNanoNet

network Andreas Falk 1, @

1 : BioNanoNet Forschungsgesellschaft mbH Steyrergasse 17 8010 Graz - Austria

Nanotechnological applications as it is with any new development in science and technology are challenges for all stakeholders

including society, science, economy, regulatory, and political bodies. Risk-benefit-balance is one of the key elements,

especially in medical applications. However, human health shall be of more importance than economic success. At the moment,

a lot of efforts are put into safety-approval of nanomedical applications. This is highly relevant, but needs some major

refreshment:in the benefit-discussion.

Everyone is aware of the fact that no innovation is possible without taking into account a certain amount of risk. These risks

have to be addressed, but they also have to be related to the high potential of this new technology. In addition to this, aspects

of European projects addressing commerzialisation aspects will be discussed.

Within this contribution, the approach taken by BioNanoNet will be addressed, showing aspects of safety-work related to

nanotechnology, as well as information about how BioNanoNet created a community, what our members are offering, and where we see a potential to collaborate with EPNOE.

1

Thermodynamics of adsorption at nanocellulose surfaces Wim Thielemans 1, *, @

1 : Renewable Materials and Nanotechnology Research Group, Department of Chemical Engineering, KU Leuven

Campus Kulak Kortrijk, Etienne Sabbelaan 53, 8500 Kortrijk, Belgium - Belgium

* : Corresponding author

Controlling the interactions of nanocellulose with molecules and polymers is key to a more structured approach to developing

materials with tailored properties and structure. We thus started to look into the interaction of nanocellulose with natural

polymers such as proteins and hemicelluloses, organic and inorganic ionic species, metal nanoparticles, and hydrophobic

molecules. We also varied the surface chemistry of the nanocellulose surface. In our studies, we relied largely on isothermal

titration calorimetry (ITC,) a very powerful technique to look into detail into the enthalpic and entropic interactions governing

nanoparticle-adsorbate interactions, yet, which is currently still a largely untapped technique for these applications. In this

presentation, I will give an overview of important findings of our work, show the power of ITC and its potential to elucidate

interactions at nanoparticle surfaces, and project how thermodynamic measurements could help us to improve control over

structure formation.

2

Potential of fibrillated cellulose in papermaking. Looking

for optimal conditions of fibrillation and addition rate to

maximize paper performances. Julie Bossu 1, @ , Winter Armin 2 , Rene Eckhart 1 , Wolfgang Gindl-Altmutter 2 , Wolfgang Bauer 1

1 : Institute of Paper, Pulp and Fiber Technology

Graz University of Technology, Inffeldgasse 23, 8010 Graz - Austria

2 : BOKU - University of Natural Resources and Life Sciences Konrad Lorenz-Straße 24/I 3430 Tulln an der Donau - Austria

In papermaking, the use of nano/micro fibrillated celluloses (NFC, MFC) can bring a wide range of remarkable properties to

the material 1,2. Because of their highly fibrillated structure, the addition of such products increases specific surface area and

improves the overall tensile strength, rigidity and Z-strength of paper by promoting the formation of fibre-fibre bonds. Such

results are encouraging and suggest that the addition of fibrillated cellulose could replace beating since it brings similar

mechanical properties without damaging fibres´ structure, improving products lifetime and reducing energy costs 3. Moreover,

fibrillated celluloses also feature good barriers properties while being biocompatible, biodegradable and non-toxic and can be

easily chemically modified to bring functional properties.

For these reasons, the potential of NFC/MFC for paper applications received a lot of attention in the past decade. A positive

correlation between the fibrillation rate of the material added to the pulp and paper mechanical performances have been

reported by many authors 4. Nonetheless, if the high fibrillation of NFC/MFC improve mechanical properties, it also entails

the plugging of the inter-fibre pores, which reduces sheets permeability 5. The resulting decreasing of drainage rate constitutes

a major limiting factor for industrial uses. A threshold then need to be found to maximize the effect on paper strength without

damaging drainage rate. The numerous studies addressing this topic report contrasting results depending on the nature and the

quantity of fibrillated cellulose added to the pulp. Indeed, different parameters come into play here: (i) the fibrillation rate of

the cellulose, (ii) the pre-treatment of NFC/MFC and (ii) the amount of material mixed to the pulp. This work aims to better

understand the combined effect of these parameters on paper´s structure to identify the optimal conditions leading to the highest

performances.

For this purpose, different types of fibrillated material originating from the same softwood bleached kraft pulp are produced:

(a) primary fines separated from the pulp with a lab scale pressure screen 6; (b) secondary fines separated from refined pulp

produced with an industrial single disk refiner; and (c) different NFC/MFC materials produced with a homogenizer using

varying high pressure steps. These samples of different degrees of fibrillation are morphologically characterised using methods

developed for this purpose 7. For a subsample, fluorescent markers are used to localize the added fibrillated cellulose in the

sheets. Subsequently, the different materials are mixed to the pulp in different proportions. After testing pulp properties,

handsheets of 60 g/m² are prepared on a Rapid – Köthen sheet former (ISO 5269-2:2004) using white water recirculation 8.

After successful preparation, the properties of the sheets are analysed, using standard paper testing and state of the art

methodologies such as CLSM, SEM, and atomic force microscopy.

The comparison between pulp composition, distribution of the fibrillated cellulose within the fibres and sheet properties is

expected to give interesting clues to better understand the interactions between fibres and fibrillated cellulose and their effect

on pulp properties and paper strength. This presentation will focus on the general design of the experiments which are targeted

to evaluate the potential of using such materials in the papermaking production lines.

1 Pinkl, S., S. Veigel, et al. (2017). Nanopaper Properties and Adhesive Performance of Microfibrillated Cellulose from

Different (Ligno-)Cellulosic Raw Materials. 9: 326.

2 Dufresne, A. (2017). Cellulose nanomaterials as green nanoreinforcements for polymer nanocomposites. 376.

3 González, I., S. Boufi, et al. (2012). "Nanofibrillated cellulose as paper additive in eucalyptus pulps." Bioressources 7(4):

5167-5180.

4 Boufi, S., I. González, et al. (2016). "Nanofibrillated cellulose as an additive in papermaking process: A review."

Carbohydrate Polymers 154 (Supplement C): 151-166.

5 Taipale, T., M. Österberg, et al. (2010). "Effect of microfibrillated cellulose and fines on the drainage of kraft pulp

suspension and paper strength." Cellulose 17(5): 1005-1020.

6 Jagiello, L.A. Separation and Thickening of Pulp Fibers and Fines in the Lab Scale and Application Thereof. Ph.D. Thesis,

Graz University of Technology, Graz, Austria, 2017.

7 Mayr, M.; Eckhart, R.; Bauer,W. Improved microscopy method for morphological characterisation of pulp fines. Nord. Pulp

Pap. Res. J. 2017, 32, 244–252.

8 Giner-Tovar, R.; Fischer, W.J.; Eckhart, R.; Bauer, W. White Water Recirculation Method as a Means to Evaluate the

Influence of Fines on the Properties of Handsheets. BioResources 2015, 10, 7242–7251.

3

Investigation of dissolution process of cellulose in NaOH-

urea (system) and effect of regenerated material on

properties of paper

Velta Fridrihsone 2, 1, @ , Juris Zoldners 1 , Marite Skute 1 , Uldis Grinfelds 1

2 : Institute of Polymer Materials, Faculty of Material Science and Applied Chemistry, Riga Technical University

Paula Valdena street 3, Riga, LV-1048 - Latvia

1 : Latvian State Institute of Wood Chemistry

Dzerbenes street 27, Riga LV-1006 - Latvia

Keywords: cellulose, regenerated materials, NaOH-urea, paper properties

Recycling of paper materials or other type of cellulose fibres is important regarding saving nature resources and environmental

protection. There are two ways how to recycle cellulose. First includes crushing of material, homogenization, separation of

impurities, decolouring, including beaching. Second includes use of specific solvents like inorganic molten salts [1], amine

complexes with metals (Cu, Cd, Ni, Zn, Pd) [2], monovalent (Li, Na) salt solutions in dimethylacetamide [3], ionic liquids [4]

and systems of monovalent hydroxides (LiOH, NaOH) [5,6]. Both ways have shortcoming from toxicologic and environmental

point of view.

System sodium (or lithium) hydroxide and urea in this context is environmentally friendlier and technologically easier due to

its cheapness and availability of raw materials, furthermore they do not create ecological endangerment.

Main goals of this research are to evaluate solubility of cellulose from different sources in system NaOH-urea and to evaluate

formation of regenerated cellulose films and investigate effect of regenerated material on properties of paper.

Different raw materials containing cellulose were chosen: bleached softwood cellulose, paper from newspaper, hygienic paper,

laboratory filter paper, egg carboard, as well as microcrystalline cellulose from birch cellulose and cotton.

Raw materials were crushed in mill. Cellulose materials were solubilised using system NaOH-urea. Solutions of NaOH 14wt%

and urea 24wt% were cooled till - 4°C. Cellulose was introduced in NaOH solution while stirring, the same amount of urea

was added stirring vigorously. Dosage of cellulose from 4g/100g was decreased to 2g/100g. Cellulose solution was filtered

thought glass filter, washed, dried and weighted to determine amount of not dissolved residue. Film forming: cellulose solution

was poured into Petri dish and immersed in 5% H2SO4.

Most of cellulose samples (bleached sulphate cellulose, cardboard, hygienic paper, newspaper) were soluble partly in used

system. However, they formed a transparent liquid gel. Microcrystalline cellulose from birch (solubility 97,0%) and cotton

(solubility 98,7%) as well as cotton cellulose (solubility 35,6%) dissolved completely. Using this solution films were formed.

However, homogeneous films without gel parts were not formed. Evaluating further uses of cellulose gel, paper samples were

made using gel as additive up to 20%. Results reveal correlation between paper strength as concentration of gel.

It was concluded that solubility of cellulose in NaOH-urea system was significantly dependent on cellulose source and adding

gel to paper mass increases paper strength.

Acknowledgement

Financial support for this research from Latvian State Insitute of Wood Chemistry Bio-economic grant “RenModCell”.

1. S.Fisher,H.Leipner,K.Thümler,E.Brendler,J.Peters. Inorganic molten salts as solvents for cellulose.Cellulose,

2003,10,N3,227-236

2. T.Heinze,T.Liebert. Unconvential methods in cellulose functionaliation.Progress in Cellulose Science.2001, 26, 9,1689-

1762.

3. A.Striegel. Theory and application of DMAC/LiCl in the analysis of polysaccharides.Carbohydrate Polymers, 1997, 34, 4,

267-274.

4. R.P.Swatloski,S.K.Spear,J.D.Holbrey,R.D.Rogers. Dissolution of cellulose with ionic liquids.Journal of the

AmericanChmical Society.2001,124,18,4974-4975.

5. M.Egal, T.Budtova, P.Navard. The dissolution of microcrystalline cellulose in sodium hydroxide-urea solutions.

Cellulose2008, 15, 361-370.

6 S,Qi, Q.Yang,L.Zhang, T.Liebert, T.Heinze. The dissolution of celluloseinNaOH-based aqueous system by two-step process. Cellulose 2008, 15, 361-370.

4

Nanocellulose papers from elephant manure Andreas Mautner 1, *, @ , Kathrin Weiland 1, @ , Alexander Bismarck 1, 2, @

1 : Department of Materials Chemistry - University of Vienna

Währinger Straße 42, 1090 Wien - Austria

2 : Polymer and Composite Engineering group, Imperial College London

South Kensington Campus, London SW7 2AZ - United Kingdom

* : Corresponding author

Recently, the interest in cellulose fibres, in particular micro- or nanofibrillated cellulose, utilized in paper and composite

materials as alternative to conventional fibre materials, has grown significantly. Thereby, particularly in countries without

access to large forest areas, an alternative to wood as raw material for natural fibres is highly desirable. Moreover, growing

quantities of animal manure constitute an increasing environmental burden. Thus, in order to promote an environmentally

sustainable, widely available and cheap raw material, animal manure was proposed as potential source. As elephants digest

only 30 to 40% of their diet, their manure contains large quantities of fibrous cellulosic material thus being an ideal model

system for the study of animal manure for this purpose. In addition, the mechanical, acidic and enzymatic pre-treatment during

ingestion and digestion initiates break down of the fibres. This makes this animal waste a suitable candidate for the use as

precursor for the production of micro- or even nanofibrillated cellulose. Commonly, nanocelluloses are prepared by mechanical

disintegration of plant material, optionally with chemical pre-treatment, thus requiring a lot of energy and chemicals during

the fibrillation process. Therefore, utilizing the elephant as first-stage bioreactor for the defibrillation of cellulose fibres by

mechanical and chemical means constitutes an energy-efficient approach.

We demonstrate that from chemically purified elephant manure, microfibrillated cellulose with controllable properties can be

isolated. The fibrils were characterized regarding their cellulose content and physico-chemical properties in order to optimize

the extraction process. Fibrils obtained from the optimized process were initially used for the preparation of papers that were

characterized regarding their physico-chemical and mechanical properties and served as reference material. Moreover, the

fibrils were further mechanically refined and papers produced from these refined elephant manure nanofibrils that were compared to the non-refined elephant manure papers and cellulose nanopapers.

5

From surface modification of cellulosic materials to

paper-based biosensors Thomas Elschner 1, *, @ , Frank Miletzky 1 , Karin Stana-Kleinschek 2, 3 , Rupert Kargl 2, 3 , Thomas

Heinze 4

1 : Papiertechnische Stiftung

Pirnaer Straße 37, 01809 Heidenau - Germany

2 : University of Maribor, Faculty of Mechanical Engineering, Laboratory for Characterization and Processing of Polymers

Smetanova 17, 2000 Maribor - Slovenia

3 : Graz University of Technology, Institute for Chemistry and Technology of Materials

Stremayrgasse 9 - 8010 Graz - Austria

4 : Friedrich-Schiller-University of Jena, Institute of Organic Chemistry and Macromolecular Chemistry, Center of

Excellence of Polysaccharide Research

Humboldt-Str. 10, 07743 Jena - Germany * : Corresponding author

Cellulose model films allow a detailed study of parameters such as film thickness, viscoelastic behaviour, and surface

morphology. On one hand, the processing of trimethylsilyl cellulose (TMSC) by spin coating or Langmuir–Blodgett technique

and subsequent regeneration with hydrochloric acid vapor has become a well-established procedure to yield a model surface.

On the other hand, surface plasmon resonance (SPR) and quartz crystal microbalance with dissipation (QCM-D) are powerful

analytical tools allowing the online monitoring of adsorption phenomena. Cellulosic surfaces can be modified by adsorption

of functional polymers. For instance, adsorption of 6-deoxy-6-(2-aminoethyl)amino cellulose was studied with SPR and QCM-

D at different pH-values and in the presence of electrolytes, onto cellulose model substrates [1]. Moreover, chemical

modification of the hydroxyl groups of cellulose is an innovative approach. The surface can be activated with N,N'-

carbonyldiimidazole and subsequent aminolysis may yield a film of functional cellulose carbamate [2]. Finally, this procedure

is adapted to functionalization of cellulose fibers.

Due to the abundance, low-cost, mass-production, and disposability of cellulose paper, it is routinely used for printing, writing,

and packaging, but also as a promising platform for chemical analyses [3]. Microfluidic paper-based analytical devices (μ-

PADs) became very popular after publishing by the Whitesides group in 2007 [4]. Since that time many review articles about

paper-based biosensing have been published. However, the current interest is focused on a pilot line for the fabrication of a

point-of-care test from roll-to-roll. Base paper definition, chemical functionalisation, surface modification and characterisation

are the tasks of paper experts. The overall work combines paper, printing and microchip technologies manufacturing a fully

integrated paper-based electrochemical biosensors that directly transfer the measured data to the user's smartphone. These

biosensors will be designed as self-powered disposable test strips that combine the simplicity of lateral flow tests with

quantitative readout, which is enabled by the implemented electrochemical detection method.

[1] K. Jedvert et al, Macromolecular Materials and Engineering, 2017, 302, 1700022

[2] T. Elschner et al, Cellulose, 2018, 25, 537–547

[3] K. Yamada et al, Lab Chip, 2017, 17, 1206-1249

[4] A. W. Martinez et al, Angew. Chem., Int. Ed., 2007, 46, 1318–1320

Acknowledgements: The financial support of the German Research Foundation (DFG, Research Fellowship EL843/1-1) and

the European Union's Horizon 2020 research and innovation action under IMPETUS project - grant agreement No 761167 is gratefully acknowledged.

6

All-cellulose composites based on paper fines for energy

storage devices Mathias A. Hobisch 1, *, @ , Eléonore Mourad 2, @ , Wolfgang J. Fischer 3, @ , Armin

Zankel 4, @ , Andreas Mautner 5, @ , Stefan A. Freunberger 2, @ , Rene Eckhart 1, @ , Wolfgang

Bauer 1, @ , Stefan Spirk 1, *, @

1 : IPZ - Graz University of Technology

Inffeldgasse 23, 8010 Graz - Austria

2 : ICTM - Graz University of Technology

Stremayrgasse 9, 8010 Graz - Austria

3 : Sappi Gratkorn

Brucker Str. 21, 8101 Gratkorn - Austria

4 : FELMI - Graz University of Technology

Steyrergasse 17, 8010 Graz - Austria

5 : Department of Materials Chemistry - University of Vienna

Währinger Straße 42, 1090 Wien - Austria * : Corresponding author

In this contribution, we explore applications of paper fines for advanced energy applications. Fines are a major side stream in

fiber manufacturing industries. Here, we developed a strategy how to make use of fines as electrode materials by implementing

them in supercapacitors. Different activation procedures for fines to obtain highly porous activated carbons are tested with

KOH being the most effective one, allowing for manufacturing materials with SSA as high as 1570 m2ˑg-1. A further increase

of the SSA (up to 2200 m2ˑg-1) is realized by incorporation of cellulose nanocrystals into the fines, thereby creating a

hierarchical order. The electrode materials are implemented in symmetric supercapacitors using organic electrolytes (TEABF4

in acetonitrile). The capacitance of the materials is up to 164 Fˑg-1, but easily modified by the amount of CNCs in the

composite. The Ragone plot demonstrates that the performance of the fines based carbonaceous materials is significantly better than those reported in literature.

7

Up-scaling bioplastic formulations: from solvent casting

to extrusion and injection processes Idalina Gonçalves 1, 2, *, @ , Joana Lopes 2, @ , Gonçalo Oliveira 2, @ , Liliana Pires 2, 3, @ , Cláudia

Nunes 1, 2, @ , José Martinho Oliveira 2, 3, @ , Paula Ferreira 2, @ , Manuel A. Coimbra 1, @

1 : QOPNA, Department of Chemistry, University of Aveiro

Campus Universitário de Santiago 3810-193 Aveiro, Portugal - Portugal

2 : CICECO - Aveiro Institute of Materials, Department of Materials and Ceramic Engineering, University of Aveiro

Campus Universitário de Santiago 3810-193, Aveiro, Portugal - Portugal

3 : School of Design, Management and Production Technologies

University of Aveiro, Santiago de Riba-Ul, Oliveira de Azeméis, Portugal - Portugal

* : Corresponding author

Nowadays, a huge amount of plastic and organic wastes resulting from human activity has a significant impact on the

environment. For instance, the agrofood industry and its extensive trade are targets of major concern. The implementation of

a circular economy by adding value to non-reused agrofood industrial wastes viz. potato chips industry byproducts as

biomolecules sources for the development of renewable packaging materials is an opportunity.

In this work, various potato chips industry byproducts were reused to produce bioplastics formulations. Potato starch from

washing slurries, potato peel and frying oils were used. After investigating the optimum experimental conditions to prepare

hydrophobic and flexible potato starch-based films, the most promising formulations were up-scaled from solvent casting to

extrusion and injection processes, aiming to mimic industrial processing conditions. Herein, each developed formulation was

produced as a biogranulate and further extruded and injected. Experimental conditions as byproducts combination at different

ratios (1; 2; 3; 5; and 10% related to the dry potato starch weight), speed, residence time, and processing temperature were

adjusted according to the biogranulates flow index and calorimetry.

According to the byproducts ratios used, different mechanical profiles were obtained. Up to 3%, the oil incorporation increased

the starch granulates flow properties. On contrary, only above 5%, the potato peel incorporation prompted this effect. When

combined, both oil and potato peel improved the biogranulates fluidity. Moreover, adding oil and/or potato peels decreased

the relative humidity content of starch-based granulates, thus contributing to stabilize the starch-base formulation. Each

produced biogranulate was effectively extruded and injected, showing good mechanical performances.

Therefore, potato industry byproducts revealed to be suitable raw materials to produce biogranulates that fit with industrial

extrusion and injection processes.

Acknowledgments: Thanks are due to FCT through national founds and FEDER, within the PT2020 Partnership Agreement,

for funding QOPNA (FCT UID/QUI/00062/2013) and CICECO-Aveiro Institute of Materials (FCT UID/CTM/50011/2013;

POCI-01-0145-FEDER-007679). I.G. (SFRH/BPD/104712/2014), C.N. (SFRH/BPD/100627/2014) and P.F. (IF/00300/2015)

also thank the support of FCT. The authors also acknowledge to POTATOPLASTIC project (POCI-01-0247-FEDER-

017938), financed by FEDER trough POCI, “Isolago – Indústria de Plásticos, S. A.”, the project leader and to “A Saloinha,

Lda.” for providing potato byproducts, and to Polysyc group from Chemical Engineering Department of University of Coimbra (Portugal) for using the PolyLab QC Rheometer.

8

LIGNOCELLULOSIC RESIDUES PRETREATMENT

WITH REACTIVE EXTRUSION USING ENZYMES –

INFLUENCE OF PROCESS CONDITIONS ON

SUBSEQUENT ENZYMATIC HYDROLYSIS Etienne Gatt 1, @ , Virginie Vandenbossche 1, @

1 : Laboratoire de Chimie Agro-Industrielle

Institut National de la Recherche Agronomique : UMR1010, Institut National Polytechnique de Toulouse - INPT

Laboratoire de Chimie Agro-Industrielle LCA-INPT, 4 allée Emile Monso 31030 TOULOUSE, FRANCE. - France

Agricultural by-products are renewable, cheap, worldwide and abundantly available resources that can be used to produce

carbon neutral energy, materials and chemicals. However, because of the complex and resistant structure of the lignocellulosic

biomass, its deconstruction and conversion is difficult and requires a transformation process1. Biomass pretreatment and

enzymatic hydrolysis are commonly the two steps used during a refining process2.

The extrusion process is a classical continuous pretreatment used with lignocellulosic biomass3. Reactive extrusion using

enzymes (also called bioextrusion), intend to initiate the enzymatic hydrolysis as a last step of the extrusion pretreatment

process, thanks the particular adaptability of the extrusion technique. Even with very short residence time, bioextrusion of

lignocellulose residues has been several times proved to enhance the subsequent enzymatic sugar production4,5.

The objective of this study was to compare different bioextrusion process conditions to optimize the biocatalytic

mono/oligosaccharides production while reducing the use of solvent and observing the biomass deconstruction. Extruders with

a specific reactive extrusion screw profile, agricultural stem residues from crop cultures (wheat, corn), and cellulolytic

cocktails were used.

The experiments were carried out at 50°C, with pH buffer at 5, different S/L ratios and enzyme concentrations were tested.

Enzymatic hydrolysis reactions were done with or without prior bioextrusion during 48 h. Carbohydrates content and biomass

deconstruction were followed during the reaction kinetic, in order to better understand the enzymatic hydrolysis process and

limitations. In particular, the cellulose accessibility was assessed using specific fluorescent probes6.

1. Himmel, M. E. et al. Biomass Recalcitrance: Engineering Plants and Enzymes for Biofuels Production. Science 315, 804–

807 (2007).

2. Van Dyk, J. S. & Pletschke, B. I. A review of lignocellulose bioconversion using enzymatic hydrolysis and synergistic

cooperation between enzymes—Factors affecting enzymes, conversion and synergy. Biotechnol. Adv. 30, 1458–1480 (2012).

3. Karunanithy, C. & Muthukumarappan, K. Thermo-Mechanical Pretreatment of Feedstocks. in Green Biomass Pretreatment

for Biofuels Production (ed. Gu, T.) 31–65 (Springer Netherlands, 2013).

4. Duque, A. et al. Sugar production from barley straw biomass pretreated by combined alkali and enzymatic

extrusion. Bioresour. Technol.158, 262–268 (2014).

5. Vandenbossche, V., Brault, J., Vilarem, G. & Rigal, L. Bio-catalytic action of twin-screw extruder enzymatic hydrolysis on

the deconstruction of annual plant material: Case of sweet corn co-products. Ind. Crops Prod. 67, 239–248 (2015).

6. Hébert-Ouellet, Y. et al. Tracking and predicting wood fibers processing with fluorescent carbohydrate binding modules. Green Chem. 19,2603–2611 (2017).

9

Reactive extrusion Alexander Feldner 1, @ , Martin Zahel 1, *, @ , Tiemo Arndt 1, *, @

1 : Alexander Feldner

Pirnaer Straße 37, PTS Paper, 01809 Heidenau - Germany * : Corresponding author

Cellulose which is the most abundant polymer on earth has a large opportunity to become an important feedstock in a

sustainable bioeconomy by means of pulp. Besides applications that can be targeted by its natural properties such as paper,

value added products are achieved by a broad variety of derivatization reactions developed during the last century.

An important cellulose derivative is carboxymethyl cellulose (CMC), which is widely used as a binder or thickener, paper

sizing agent in the paper industry or oil drilling additive. In industrial production, CMC is generated in a two-step semi-batch

process consisting of a mercerization and etherification in alcoholic media (usually isopropanol).

The present talk focus on CMC synthesis by reactive extrusion. Recent work on PTS showed that producing CMC with

different degrees of substitution (DoS) in a wide range of 0.05 to 1.1 is possible by using a twin screw extruder as a continuous

reactor. During the extrusion process, the fibre material and the liquid process chemicals sodium hydroxide and

monochloroacetic acid are metered by means of gravimetric feeders or peristaltic pumps respectively. Due to high shearing

behavior in combination with high possible stock consistency in the extruder it is possible to perform both reaction steps

(mercerization and etherification) together as a one without any sample pretreatment in completely aqueous milieu. Following

this approach water soluble CMC as well as anionic fibre materials are accessible.

The use of low-substituted fibre material produced (DoS < 0.05) by reactive extrusion as a paper additive leads to significant improvement in tensile and tear strength as well as barrier properties against air permeability (Bendtsen).

10

Electrospinning water-soluble/insoluble polymer blends Robin Böttjer 1 , Timo Grothe 1, *, @ , Daria Wehlage 1 , Andrea Ehrmann 1, *, @

1 : Bielefeld University of Applied Sciences

Interaktion 1, 33619 Bielefeld - Germany * : Corresponding author

Electrospun nanofibers can be used for different application, e. g. as filter materials, in biotechnological and medical fields,

tissue engineering, for adherent cell grow, etc. But many (bio-)polymers cannot be spun alone; they need a spinning-agent to

be spinnable.

In recent experiments, the used spinning-agent is polyacrylonitrile (PAN) which was spun with seven water-soluble polymers

to test the spinnability of these polymer blends. After the spinning process, the different nanofiber mats were watered to

investigate the stability of the water-soluble part. Optical examination before and after watering shows the impact of different

polymer combinations and blend ratios on the nanofiber mat morphology and the water solubility, giving rise to tailoring the

fiber dimensions.

11

Microphase separation of cellulose derivates Gundula Teichert 1, @ , Maximilian Nau 2 , Katrin Niegelhell 1 , Mathias A. Hobisch 1, @ , Chonnipa

Palasingh 3 , Tiina Nypelö 3, @ , Markus Biesalski 2, 4, @ , Stefan Spirk 5, 6, *, @

1 : IPZ - Graz University of Technology

Inffeldgasse 23, 8010 Graz - Austria

2 : Technische Universität Darmstadt

Petersenstr. 22, 64287 Darmstadt - Germany

3 : Chalmers University of Technology [Göteborg]

SE-412 96 Göteborg, Sweden - Sweden

4 : Technische Universität Darmstadt - Website

Petersenstr. 22, 64287 Darmstadt - Germany

5 : Graz University of Technology, Institute for the Chemistry and Technology of Materials (TU Graz)

Stremayrgasse 9, 8010 Graz - Austria

6 : University of Maribor, Institute for the Engineering and Design of Materials (Uni MB)

Smetanova Ulica 17, 2000 Maribor - Slovenia * : Corresponding author

A very intriguing area of research is the exploration of blend thin films derived from spin coating. During the spin coating

step, macroscopically homogeneous solutions of two polymers phase separate into different domains. Depending on the ratio

of the two polymers (and other factors such as molecular weight, solvent, spin coating conditions etc.) different feature sizes

and shapes are observed. While for synthetic polymers a wide range of examples is known, for biopolymers the knowledge on

blend thin films is scarce. So far blends of cellulose with polyhydroxybutyrate[1], cellulose acetate[2], cellulose stearate[3],

lignin palmitate[4], polymethylmethacrylate[5] and polystyrene[6]have been reported. [lit]

Here we present our recent results in the exploration of a new blend film system, namely cellulose / hydroxypropylstearate

cellulose (HPCE) having different degrees of substitution (DS 1 and 3, respectively). The blend films were prepared by mixing

a cellulose precursor (trimethylsilyl cellulose, TMSC) with HPCE in different ratios (1:3, 1:1, 3:1) followed by spin coating.

After the spin coating process, the films have been subjected to HCl vapors to convert the TMSC into cellulose. These surfaces

have been investigated by a wide range of surface sensitive techniques (AFM, ATR-IR, wettability, profilometry, etc.). Further,

the films have been investigated towards their interaction with biological macromolecule whereas BSA was mainly used as

biological probe. As SPR and QCM-D experiments showed, the surfaces show a low protein affinity, which depends on the

nature of the used HPCE.

[1] Niegelhell, K.; Süßenbacher, M.; Jammernegg, K.; Ganner, T.; Schwendenwein, D.; Schwab, H.; Stelzer, F.; Plank, H.;

Spirk S. Enzymes as Biodevelopers for Nano- And Micropatterned Bicomponent Biopolymer Thin

Films. Biomacromolecules 2016, 17, 11, 3743–3749.

[2] Taajamaa, L.; Rojas, O. J.; Laine, J.; Kontturi, E. Phase-specific pore growth in ultrathin bicomponent films from cellulose-

based polysaccharides. Soft Matter 2011, 7, 21, 10386.

[3] Niegelhell, K.; Süßenbacher, M.; Sattelkow, J.; Plank, H.; Wang, Y.; Zhang, K.; Spirk, S. How Bound and Free Fatty Acids

in Cellulose Films Impact Nonspecific Protein Adsorption. Biomacromolecules 2017, 18, 12, 4224–4231.

[4] Strasser, S.; Niegelhell, K.; Kaschowitz, M.; Markus, S.; Kargl, R.; Stana-Kleinschek, K.; Slugovc, C.; Tamilselvan M.;

Spirk, S. Exploring Nonspecific Protein Adsorption on Lignocellulosic Amphiphilic Bicomponent

Films. Biomacromolecules 2016, 17, 3, 1083–1092.

[5] Kontturi, E.; Johansson, L.-S.; Laine, J. Cellulose Decorated Cavities on Ultrathin Films of PMMA. Soft Matter 2009, 5,

1786−1788.

[6] Kontturi, E.; Nyfors, L.; Laine, J. Utilizing Polymer Blends to Prepare Ultrathin Films with Diverse Cellulose

Textures. Macromol. Symp. 2010 294, 2, 45–50.

12

Gas-esterification of cellulose particles for the production

of PHBV based biocomposites Grégoire David 1, @ , Jérôme Lecomte 2 , Nathalie Gontard 3 , Laurent Heux 4 , Angellier-Coussy

Hélène 1, *, @

1 : Ingénierie des Agro-polymères et Technologies Émergentes

Université de Montpellier : UMR1208

2 place Pierre Viala, 34060 Montpellier - France

2 : Ingénierie des Agro-polymères et Technologies Émergentes

Centre de Coopération Internationale en Recherche Agronomique pour le Développement : UMR1208

2 Place Pierre Viala, 34060 Montpellier - France

3 : Ingénierie des Agro-polymères et Technologies Émergentes

Institut National de la Recherche Agronomique : UMR1208

2 Place Pierre Viala, 34060 Montpellier - France

4 : Centre de recherches sur les macromolécules végétales

Centre National de la Recherche Scientifique : UPR5301

601 Rue de la Chimie 38400 ST MARTIN D HERES - France * : Corresponding author

The combination of awareness of environmental issues and oil crisis results in the fact that biodegradable and bio-sourced

materials are becoming serious candidates to replace traditional petro-sourced plastics that accumulate in natural systems. In

the frame of the European NoAW project (No Agricultural Waste), new biocomposite materials are designed from agro-wastes,

i.e. a bacterial polyester (poly(hydroxy-butyrate-co-valerate, noted PHBV) as matrix and lignocellulosic fillers from vine

shoots. The main drawbacks of natural fibers in composites are the poor compatibility with the non-polar matrix and their

relative high moisture absorption. In this study, a new treatment is explored on cellulose particles to make them more

hydrophobic and pave the way for lignocellulose treatment. A solvent-free gas-phase-esterification was applied to cellulose

particles in order to graft palmitoyl chloride at the surface of particles and makes them more compatible with non-polar

polymers for composite applications. The efficiency of the treatment was evidenced from FT-IR analysis and the degree of

substitution (DS) was quantified by solid-state 13C-NMR spectroscopy. The effect of surface grafting on resulting intrinsic

characteristics of cellulose particles, i.e. surface free energy, thermal stability, crystallinity and morphology, was investigated

respectively by contact angle measurements, thermogravimetric analysis, X-ray diffraction analysis and SEM observations

coupled with image analysis. It was shown that a DS as low as 0.01 was enough to drastically increase the hydrophobicity of

cellulose particles without affecting the inner properties of cellulose. PHBV-based composite materials were prepared to

qualitatively validate the expected impact on the filler/matrix interfacial adhesion. It was concluded from SEM observations

of cryo-fractured cross-sections that gas-phase-esterification was a promising method to enhance the filler/matrix

compatibility.

Keywords: Cellulose; Gas-phase esterification; Biocomposite

Acknowledgements Project financed by the European Union's Horizon 2020 research and innovation programme under grant agreement No 688338.

13

Influence of low-pressure oxygen plasma on properties of

hemp fibres (Cannabis sativa) Peter Simčič 1 , Marija Gorjanc 1, @ , Miran Mozetič 2, @

1 : University of Ljubljana, Faculty of Natural Sciences and Engineering

Aškerčeva 12, 1000 Ljubljana - Slovenia

2 : Jozef Stefan Institute Jamova 39, 1000 Ljubljana - Slovenia

Hemp fibres, which are obtained from the stem of the Cannabis sativa plant, are used for many products, from clothing to

composites. Although, the main component of the fibres is cellulose, the high quantity of noncellulosic components

(hemicelluloses, lignin, pectin and waxes) and impurities negatively influence further fibres processing and fibres properties.

The modification of hemp fibres is usually performed by wet-chemical processes, such as alkali, acetylation and enzymatic.

However, from the environmental aspects, the plasma treatment could be a promising solution, since it has been already proven

to be efficient in modification of other natural and synthetic fibres.

The purpose of our research was to evaluate the influence of oxygen plasma treatment on the properties of hemp fibres. For

that purpose, raw hemp fibres were treated in radiofrequency inductively coupled plasma system for different time periods (1,

2, 3, 5, 10, 20, 30, 100 and 300 s). The untreated and plasma-treaded samples of hemp fibres were tested for their water

absorptivity and water retention. The chemical changes after plasma treatment were analysed with Fourier-transform infrared

spectroscopy (FTIR), and the morphological changes were analysed with scanning electron microscopy (SEM). The results

show that with increasing the plasma treatment time up to 30 s, the water absorption and retention increase, but they start

slowly descending with further plasma treatment time. However, the capillary rise of water was highest in fibres treated with

oxygen plasma for 300 s. The SEM images showed that the surface of the fibres becomes rougher after plasma treatment,

especially after 300 s of treatment. Such increased etching influences higher sorption of fibres and capillary rise of water. The

increased roughness also promotes higher adhesion capability with other polymers. The FTIR results showed the oxidisation of samples after plasma treatment which led to increased hydrophilicity of fibres.

14

Flame retardancy of flax fabrics by radiografting of

phosphorus compounds Raymond Hajj 1, 2, @ , Rodolphe Sonnier 3, *, @ , Roland El Hage 2, *, @ , Belkacem

Otazaghine 3, @ , Michel Nakhl 2, @ , José-Marie Lopez-Cuesta 4, @

1 : Centre des Matériaux des Mines dÁlès

IMT - Mines Alès Ecole Mines - Télécom

École des Mines dÁlès / Centre des Matériaux des Mines dÁlès6 Avenue de Clavières30319 ALES cedexTéléphone : +33 4

66 78 50 00Par courrier électronique : c2ma@mines-ales.fr - France

2 : Lebanese University, Plateforme de Recherche en Nanosciences et Nanotechnologies, LCPM

B.P 90656 Jdeideth El Matn, Fanar, Lebanon - Lebanon

3 : Centre des Matériaux des Mines d'Alès (C2MA) - Website

Ecole Nationale Supérieure des Mines d'Alès

6 avenue de Clavières 30100 Alès - France

4 : Centre des Matériaux des Mines d'Alès (C2MA)

C2MA

6 avenue de Clavières, 30319 Alès cedex - France * : Corresponding author

Many natural fibers have been used for a long time in textile industry as cotton and flax [1]. Moreover, natural fibers are

getting more importance in composites industry as a substitute for glass, carbon, or aramid fibers [2, 3]. However, they must

be modified to overcome some disadvantages such as flammability [4]. In previous studies [4, 5], phosphorus flame retardants

were grafted by e-beam radiation. The P-monomers can be grafted directly on the flax components or can homopolymerize

inside the fibers. In the present study, the reactivity of the double bond C=C of the P-monomers was studied to control the

grafting yield of various FRs. Phosphorus content reached 1.4 wt% using vinyl phosphonic acid. Grafting efficiency was

assessed by X-ray fluorescence and Energy Dispersive X-Ray Analysis (EDX) / Scanning Electron Microscopy (SEM). Fire

behavior of the modified fabrics was studied using thermogravimetric analysis, pyrolysis combustion flow calorimetry and a

preliminary fire test. Flame retardant fabrics were successfully developed.

References: [1] R. M. Kozasowski, M. Mackiewicz-Talarczyk, and A. M. Allam, Bast fibres: flax. Woodhead Publishing Limited, 2012.

[2] M. Zimniewska and M. Wladyka-Przybylak, “Natural Fibers for Composite Applications,” S. Rana and R. Fangueiro, Eds.

Singapore: Springer Singapore, 2016, pp. 171–204.

[3] O. Faruk et al., “Biocomposites reinforced with natural fibers: 2000–2010,” Progress in Polymer Science, vol. 37, pp.

1552–1596, 2012.

[4] R. Sonnier et al., “Improving the flame retardancy of flax fabrics by radiation grafting of phosphorus

compounds,” European Polymer Journal, vol. 68, pp. 313–325, 2015.

[5] R. Hajj et al., “Grafting of phosphorus flame retardants on flax fabrics: Comparison between two routes,” Polymer Degradation and Stability, vol. 147, pp. 25–34, 2018.

15

How is cellulose affected during the X-rays examination

of manuscripts? Alice Gimat 1, *, @ , Sabrina Paris 1, @ , Véronique Rouchon 1, @ , Ira Rabin 2, @ , Leif

Glaser 3, @ , Sebastian Schoeder 4, @ , Mathieu Thoury 4, @ , Anne-Laurence Dupont 1, @

1 : Centre de Recherche sur la Conservation (CRC)

CNRS : USR3224, Muséum National d'Histoire Naturelle (MNHN), Ministère de la Culture et de la Communication

36 rue Geoffroy Saint Hilaire, 75005 Paris - France

2 : BAM Bundesanstalt für Materialforschung u. -prüfung

Unter den Eichen 87;12205;Berlin - Germany

3 : Deutsches Elektronen-Synchrotron [Hamburg]

Notkestraße 85 D-22607 Hamburg - Germany

4 : IPANEMA

CNRS : USR3461, Ministère de la Culture et de la Communication, Université de Versailles Saint-Quentin-en-Yvelines

(UVSQ)

Site du Synchrotron SOLEIL BP 48 St Aubin F-91192 Gif Sur Yvette (France) - France * : Corresponding author

X-rays techniques (XRF, XRD, XANES, X-ray computed tomography...) are often used to examine cultural heritage artefacts

including paper-based artworks and manuscripts. Due to their high energy, X-rays can break molecular bonds and ionize atoms

thereby damaging cellulose by promoting depolymerization and enhancing radicals formation and oxidation. The alteration of

various cultural heritage materials (proteins, parchment and pigments) under synchrotron X-rays has been reported [1,2,3,4]

but few studies have been dedicated to X-rays damage to cellulosic material [5,6,7]. Among them, only one [5] focused on

paper and moreover reported mainly on macro and microscopic level examination (visual and SEM). The lack of systematic

studies prompted this research on the impact on cellulose of exposure to X-rays and the dose-damage response. Model and

ancient papers made of cotton linters and linen rag (flax) were used. The impact of residual humidity in the paper and the

presence of several common additives usually found in paper (calcium carbonate, ink and gelatin size) was examined. The

changes in paper and cellulose upon synchrotron X-ray irradiation were monitored at the macro/microscopic level

(colorimetry, fluorescence) and at the macromolecular level (Size Exclusion Chromatography). The formation of peroxides

and hydroxyl radicals was investigated using High Performance Liquid Chromatography and Electron Spin Resonance

spectroscopy. The aim of this investigation is to help developing safe procedures to analyze manuscripts with X-rays

techniques.

[1] Bertrand L et al. TrAC Trends in Analytical Chemistry. 2015;66:128-45.

[2] Moini M et al, Anal Chem. 2014;86(19):9417-22.

[3] Young G. Canadian Conservation Institute; 2005 p. 1-27.Report No.Proteus 92195.

[4] Gervais C et al Appl Phys A. 2015;121(3):949-55.

[5] Mantler, M and Klikovits, J 2004 Powder Diffr., 19(1): 16–19.

[6] Kozachuk M, et al. Journal of Conservation and Museum Studies. 2016;14(1). [7] Brown NMD et al. Surf. Interface Anal. 1992, 18, 199-209

16

Incorporation of Nanoparticles into Cellulose Matrices

using Femtosecond Laser Pulses Werner Schlemmer 1, @ , Nikša Krstulović 2 , Damjan Blažeka 2 , Hrvoje Skenderović 2 , Mario

Rakić 2 , Tomislava Vukušić 3 , Gregor Filipič 4 , Jurov Andrea 4 , Armin Zankel 5 , Michael

Weißl 1 , Gregor Trimmel 6 , Thomas Rath 6 , Stefan Spirk 1, *

1 : Graz University of Technology, Institute for Paper-, Pulp- and Fibre Technology (IPZ),

Inffeldgasse 23a, 8010 Graz - Austria

2 : Institute of Physics

Bijenička 46, 10000 Zagreb - Croatia

3 : Faculty of Food Technology and Biotechnology, University of Zagreb

Pierottijeva 6, 10000 Zagreb - Croatia

4 : Jožef Stefan Institute

Jamova 39, Ljubljana 1000 - Slovenia

5 : Institute of Electron Microscopy and Nanoanalysis (FELMI)

Steyrergasse 17, 8010 Graz - Austria

6 : Institute for Chemistry and Technology of Materials

Stremayrgasse 9 - Austria

* : Corresponding author

There are a variety of approaches to modify polysaccharide based materials for realizing particular functionalities. One option

is to functionalize the hydroxyl groups of the subunits using synthetic chemistry. Alternatives include incorporation of

polymers, particles and small molecules.

In this work, the incorporation of nanoparticles (Ag, Au, Bi) into such cellulose matrices will be investigated using different

„green methods“. In order to generate nanoparticles in an environmentally friendly way, laser ablation of gold and silver metal

in water is employed using femtosecond laser pulses that are focused onto metal surfaces. The generated colloidal solutions

were then incorporated in cellulose matrixes by either drop coating or the addition of colloidal solutions at certain steps of the

paper making process. Additionally, the direct synthesis of nanoparticles inside cellulose derived thin films is investigated

using bismuth 2-ethyl-hexanoate as precursors (define hex) which are then converted into bismuth sulfide nanoparticles using

femtosecond laser pulses.

All materials have been characterized using state of tha art analytical methods such as TEM, EDX-SEM and XPS as well as

contact angle and leaching tests. In addition the anti-microbial effect of Ag is investigated. This research provides simple, green methods for the impregnation of different nanoparticles into cellulosic matrices.

17

ROOM BORISA PODRECCE

ENTIRELY BIO-SOURCED NANOCOMPOSITES

FOR THE ELABORATION OF BIOMATERIALS Veronica Nessi 1, @ , Chloé Chevigny 1, @ , Nicolas Descamps 2 , Valérie Gaucher 3, @ , Denis

Lourdin 1, @

1 : Unité de recherche sur les Biopolymères, Interactions Assemblages

Institut National de la Recherche Agronomique - INRA : UR1268, Institut national de la recherche agronomique (INRA) :

UR1268

Rue de la Géraudière BP 71627 44 316 Nantes Cedex 3 - France

2 : Roquette R&D

ROQUETTE

Rue de la Haute Loge, 62136 Lestrem - France

3 : Unité Matériaux et Transformations - UMR 8207

Université de Lille, Sciences et Technologies Université Lille 1 Bâtiment C6 59655 Villeneuve dÁscq - France

Starch is the main storage carbohydrate of plants and the major energy source of the human diet. Growing concern about the

preservation of the environment has encouraged its use as a degradable polymer. Among these, the development of starch-

based materials for biomedical use has been generating a lot of interest recently due to the biodegradability and high

biocompatibility of starch with the human body [1]. Starch-based biomaterials cover a wide range of biomedical applications,

from tissue scaffolds [2] to implants [3].

However once in place, in contact or within the human body, the functioning span of starch-based materials is generally short,

as starch is degraded quickly by the action of amylases and water. Water sorption and swelling cause specific structural and

physicochemical transformations in processed starches [4]. These transformations can be slowed down and controlled by the

addition of other components, for example plasticizers such as glycerol or nano-fillers [5]. This modifies the structure and

consequently the properties. A better understanding of the role of the structural organization of starch and filler could be critical

in designing materials with controlled degradation rates and improved functionality [6].

To investigate this question, native potato starch was mixed with glycerol and crystalline cellulose nano-fillers in various

concentrations. Materials were produced via twin-screw extrusion and their local structures characterized using X-rays

diffraction, CP-MAS NMR and Differential Scanning Calorimetry. The macroscopic properties relevant to biomaterials, i.e.

behavior during immersion in physiological media-swelling, degradability, diffusion-have been studied. A progressive

reduction of swelling is observed at increasing rates of fillers concentration in the starch matrix. A similar reduction of the

enzymatic degradability of the material is expected. These effects are then linked to the local structure.

[1] D. Velasquez, G. Pavon-Djavid, L. Chaunier, A. Meddahi-Pellé, and D. Lourdin, “Effect of crystallinity and plasticizer on

mechanical properties and tissue integration of starch-based materials from two botanical origins,” Carbohydr. Polym., vol.

124, pp. 180–187, 2015.

[2] M. E. Gomes, A. S. Ribeiro, P. B. Malafaya, R. L. Reis, and A. M. Cunha, “A new approach based on injection moulding

to produce biodegradable starch-based polymeric scaffolds: morphology, mechanical and degradation

behaviour,” Biomaterials, vol. 22, no. 9, pp. 883–889, May 2001.

[3] M. A. Araújo, A. M. Cunha, and M. Mota, “Changes in morphology of starch-based prothestic thermoplastic material

during enzymatic degradation,” J. Biomater. Sci. Polym. Ed., vol. 15, no. 10, pp. 1263–1280, Jan. 2004.

[4] A. Briffaz, C. Mestres, J. Escoute, M. Lartaud, and M. Dornier, “Starch gelatinization distribution and peripheral cell

disruption in cooking rice grains monitored by microscopy,” J. Cereal Sci., vol. 56, no. 3, pp. 699–705, 2012.

[5] P. R. Chang, R. Jian, P. Zheng, J. Yu, and X. Ma, “Preparation and properties of glycerol plasticized-starch (GPS)/cellulose

nanoparticle (CN) composites,” Carbohydr. Polym., vol. 79, no. 2, pp. 301–305, 2010.

[6] M. Li, T. Witt, F. Xie, F. J. Warren, P. J. Halley, and R. G. Gilbert, “Biodegradation of starch films: The roles of molecular and crystalline structure,” Carbohydr. Polym., vol. 122, pp. 115–122, 2015.

18

New composites for basic GTR principles: employment

of nature- derived and bio-inspired materials in

periodontal treatment Selestina Gorgieva 1, *, @ , Silvo Hribernik 1

1 : Institute of Engineering Materials and Design, University of Maribor

Smetanova ulica 17, Maribor - Slovenia * : Corresponding author

Guided tissue regeneration (GTR) is surgical technique performed to regenerate the tooth supporting tissues affected by

periodontal disease. This procedure aims at the reconstruction of a periodontal ligament with well-oriented and organized

collagen fibers inserted in newly formed cementum and newly regenerated alveolar bone. The cell-occlusive, space making,

tissue integrative, clinically manageable and biocompatible are attributes to ˝ideal˝ membrane, for which the large diversity of

(non)biodegradable, and bioactive materials have been used [1], [2]. Despite diversity, their limited success have been reported,

due to lack of attention to µ-structural features as highly relevant for materials intended to interface with- and integrate to

structurally diverse tissues.

Within presented study, we attempt to develop multilayer composite membranes with compositional and µ-structural diversity

in orthogonal direction by merging post-synthetic oxidised bacterial cellulose and gelatine biopolymers through freeze-

thawing-mediated cross-linking process. Additional mineral layers surrounding the composite pores were formed in rapid (<

1day) mineralization process, being newly introduced procedure for such (soft) materials. The surface and bulk µ-structuring

features were followed-up by means of CFM and SEM microscopies (Fig.1), while rapid mineralization process outcome was

assessed from FTIR and XRD spectroscopic spectral lines as well as from EDX data. Finally, the specific cellular response

will be elaborated in light of foreseen biomedical application.

References [1] Zhang Y, Zhang X, Shi B, and Miron R, Membranes for guided tissue and bone regeneration, 2013, Ann. Oral Maxillofac.

Surg., vol. 1, no. 1, pp. 1–10.

[2] Dimitriou R, Mataliotakis G I, Calori M, and Giannoudis P V, The role of barrier membranes for guided bone regeneration

and restoration of large bone defects: current experimental and clinical evidence, 2012, BMC Med., vol. 10, no. 1, p. 81.

Acknowledgments The authors acknowledge the project (ID Z7-7169) was financially supported by the Slovenian Research Agency.

19

Definition of optimal “active” material for bio-printing

through analyzing the thin films Tina Maver 1, @ , Manja Kurečič 1, 2, @ , Maja Dragica Smrke 3, @ , Karin Stana-Kleinschek 1, 2, @ , Uroš

Maver 4, @

1 : Faculty of Mechanical Engineering [Maribor] Smetanova 17, SI-2000 Maribor, Slovenia - Slovenia

2 : Graz University of Technology

Stremayrgasse 9, 8010, Graz - Austria

3 : University Medical Centre Ljubljana

Zaloška cesta 2, SI-1000, Ljubljana - Slovenia

4 : Faculty of Medicine, Institute of Biomedical Sciences and Institute for Palliative Medicine and Care Taborska ulica 8, SI-2000 Maribor - Austria

Early and late complications connected with wound healing are still common causes for patient disability. and even mortality

(1). These not only lower the patient`s quality of life significantly, but also present a huge financial burden for the healthcare

systems around the world (2, 3). Treatment of larger wounds often requires the use of more complex materials, which can

ensure a successful renewal or replacement of damaged or destroyed tissues (4).

Since alginate (ALG) and carboxymethyl cellulose (CMC) are two of the most commonly used materials in the field of wound

care (5-11), these two base materials were used in this study as model systems in the shape of thin films. The influence of

material, growth factors and in situ included skin cells (fibroblasts, keratinocytes) into the material on the proliferation of skin

cells was evaluated.

The study was performed as preliminary study for development of 3D bio printed material for wound care application. Since

there was relevant influence of in situ included active substance on the proliferation of skin cells, such option will be

considered for the further development of 3D materials.

Acknowledgements The authors acknowledge the financial support from the Slovenian Research Agency for Research Core

Funding Nos. P2-0118 and P3-0036, and for the financial support through the Project No. Z2-8168.

References 1. Zarchi K, Martinussen T, Jemec GB. Wound healing and all‐ cause mortality in 958 wound patients treated in home care.

Wound Repair and Regeneration. 2015;23(5):753-8.

2. Finkelstein E, Corso PS, Miller TR. The incidence and economic burden of injuries in the United States: Oxford University

Press, USA; 2006.

3. Guest JF, Ayoub N, McIlwraith T, Uchegbu I, Gerrish A, Weidlich D, et al. Health economic burden that wounds impose

on the National Health Service in the UK. BMJ open. 2015;5(12):e009283.

4. Powers JG, Higham C, Broussard K, Phillips TJ. Wound healing and treating wounds: Chronic wound care and management.

Journal of the American Academy of Dermatology. 2016;74(4):607-25.

5. Mayet N, Choonara YE, Kumar P, Tomar LK, Tyagi C, Du Toit LC, et al. A Comprehensive Review of Advanced

Biopolymeric Wound Healing Systems. J Pharm Sci. 2014;103(8):2211-30.

6. Dornseifer U, Lonic D, Gerstung TI, Herter F, Fichter AM, Holm C, et al. The ideal split-thickness skin graft donor-site

dressing: a clinical comparative trial of a modified polyurethane dressing and aquacel. Plast Reconstr Surg. 2011;128(4):918-

24.

7. Ryssel H, Germann G, Riedel K, Reichenberger M, Hellmich S, Kloeters O. Suprathel-acetic acid matrix versus acticoat

and aquacel as an antiseptic dressing: an in vitro study. Ann Plast Surg. 2010;65(4):391-5.

8. Tickle J. Effective management of exudate with AQUACEL extra. British journal of community nursing. 2012;Suppl:S38,

S40-6.

9. Petrulyte S. Advanced textile materials and biopolymers in wound management. Danish medical bulletin. 2008;55(1):72-7.

10. O'Donoghue JM, O'Sullivan ST, Beausang ES, Panchal JI, O'Shaughnessy M, O'Connor TP. Calcium alginate dressings

promote healing of split skin graft donor sites. Acta Chir Plast. 1997;39(2):53-5.

11. Mogoşanu GD, Grumezescu AM. Natural and synthetic polymers for wounds and burns dressing. Int J Pharmaceut. 2014;463(2):127-36.

20

A preliminary study of material suitability for growth of

pancreatic cells Marko Milojevic 1, *, @ , Lidija Gradišnik 1, @ , Maša Skelin Klemen 2, @ , Andraž Stožer 2, @ , Karin

Stana-Kleinschek 3, @ , Uroš Maver 1, 4, @

1 : Institute of Biomedical Sciences, Faculty of Medicine, University of Maribor

Taborska ulica 8, 2000 Maribor - Slovenia

2 : Institute of Physiology, Faculty of Medicine, University of Maribor

Taborska ulica 8, 2000 Maribor - Slovenia

3 : Laboratory for Characterization and Processing of Polymers (LCCP), Faculty of Mechanical Engineering, University of

Maribor

Smetanova 17, 2000 Maribor - Slovenia

4 : Department of Pharmacology, Faculty of Medicine, University of Maribor

Taborska ulica 8, 2000 Maribor - Slovenia * : Corresponding author

Keywords: pancreatic cell culture, scaffolds, 3D bioprinting

Abstract In vitro models are defined as alternative experimental systems containing living human cells that recapitulate tissue- and

organ-level physiology in vitro, made by leveraging recent advances in tissue engineering and microfabrication. In this

sense, in vitro modelling does not mean to perfectly replicate the native tissue or organ, but that the model should be designed

to replicate the conditions that are intended to be mimicked. It is known that when compared with cells cultured on 2D flat,

rigid plastic substrates, 3D cell cultures establish cell–cell and cell–extra cellular matrix (ECM) interactions that better mimic

the biochemistry and mechanics of the native cell microenvironment [1, 2]. When designing a 3D in vitro model, the

fundamental elements that should be considered are: source of cells, scaffold structure and building blocks, as well chemical

and physical stimuli suiting the simulated cell phenotype. In the context of this study, this involves the combination of primary

pancreatic cells with natural and synthetic scaffolds to develop a 3D construct that is structurally, mechanically, and

functionally similar to pancreatic tissue. The scaffold must be designed to replicate the architecture of the native pancreatic

tissue, such as its ECM to let cells to adhere, proliferate, differentiate, maturate, and produce ECM. Material selection should

depend on tissue mechanical properties because material surface plays a key role in guiding cell behaviour and fate, being the

primary interface for cell interaction. The scaffolds should also possess the appropriate topographical and morphological

characteristics, such as adequate pore size and high porosity permitting cells to migrate and enabling nutrient/oxygen diffusion

and waste removal [3, 4]. Pancreas is a non-linear viscoelastic soft tissue, so synthetic and natural-derived hydrogels are

probably the best candidates as scaffold materials for in vitro pancreas engineering because of structural and mechanical

similarities with the native ECM.

Before choosing a specific material for scaffold production, it makes sense to first test the suitability of different raw materials

in regard to growth and viability of pancreatic cells when in contact with the material. In this preliminary study we will test a

number of commonly used polymers: carboxymethyl cellulose, alginate, sulphated alginate, polycaprolactone and a polymer

mixture of poly(2-hydroxyethyl methacrylate), poly(2-hydroxypropyl methacrylate) and sodium deoxycholate. For this

purpose, we will bioprint 3D scaffolds a few layers thick made of mentioned materials, culture them with pancreatic cells and

perform basic biocompatibility and cell attachment tests using the MTT and the Live/Dead cell viability assay. Specific testing

to show preservation of the cell phenotype will be performed as well.

Acknowledgement: The authors would like to acknowledge the financial support for this study received from the Slovenian

Research Agency (grant number: P3-0036) and through the Young Researcher Programme.

REFERENCES [1] K.H. Benam, S. Dauth, B. Hassell, A. Herland, A. Jain, K.-J. Jang, K. Karalis, H.J. Kim, L. MacQueen, R. Mahmoodian,

Engineered in vitro disease models, Annual Review of Pathology: Mechanisms of Disease 10 (2015) 195-262.

[2] S. Caddeo, M. Boffito, S. Sartori, Tissue Engineering Approaches in the Design of Healthy and Pathological In Vitro

Tissue Models, Frontiers in bioengineering and biotechnology 5 (2017) 40.

[3] Z. Li, H. Sun, J. Zhang, H. Zhang, F. Meng, Z. Cui, Development of in vitro 3D Tissueflex® islet model for diabetic drug

efficacy testing, PloS one 8(8) (2013) e72612.

[4] M.M. Coronel, C.L. Stabler, Engineering a local microenvironment for pancreatic islet replacement, Current opinion in biotechnology 24(5) (2013) 900-908.

21

Alternative sigma factor F (SigF) regulates secretion and

production of extracellular polysaccharides in

Synechocystis sp. PCC 6803 Carlos Flores 1, 2, 3, *, @ , Marina Santos 1, 2, 3, @ , Rita Mota 1, 2, @ , Sara B. Pereira 1, 2, @ , Paulo

Oliveira 1, 2, @ , Raquel T. Lima 1, 4, 5, @ , Paula Soares 1, 4, 5, @ , Paula Tamagnini 1, 2, 6, @

1 : i3S - Instituto de Investigação e Inovação em Saúde

Porto - Portugal

2 : IBMC - Instituto de Biologia Molecular e Celular, Universidade do Porto

Porto - Portugal

3 : ICBAS - Instituto de Ciências Biomédicas de Abel Salazar, Universidade do Porto

Porto - Portugal

4 : IPATIMUP - Instituto de Patologia e Imunologia Molecular da Universidade do Porto

Porto - Portugal

5 : FMUP - Faculdade de Medicina da Universidade do Porto, Departamento de Patologia

Porto - Portugal

6 : FCUP - Faculdade de Ciências da Universidade do Porto, Departamento de Biologia

Porto - Portugal * : Corresponding author

Many cyanobacteria produce extracellular polymeric substances (EPS), mainly composed of heteropolysaccharides that can

remain associated to the cell or be released into the surrounding environment (RPS). Their particular characteristics, such as

the presence of two different uronic acids, the high number of different monosaccharides and the high content in sulphate

groups make them very attractive for biotechnological applications (1,2,3). Despite the increasing interest on cyanobacterial

EPS, the knowledge on the biosynthetic pathways and regulatory factors involved in EPS production and export is still limited,

hindering the implementation of industrial systems based on these polymers. In addition, their biological effect in human tumor

cells has been poorly understood. In this work, we show that the transcription regulator group 3 sigma factor F (SigF) is

involved in the regulation of EPS production in Synechocystis PCC 6803. The results obtained with a knockout mutant

ΔsigF (4) indicate that, although growth is significantly impaired (≈50%), the total carbohydrates content of the culture is 2-

fold higher and the production of RPS is 3 to 4-fold higher compared to the wild-type. The RPS from Synechocystis wild-type

and ΔsigF cultures were isolated and characterized in terms of monossacharidic composition, protein and sulphate content,

and rheological properties. Furthermore, the biological activity of the RPS from the ΔsigF mutant are being evaluated on well-

established human cancer cell lines. The results showed that this polymer decreased the cellular viability of melanoma, thyroid

and ovary cancer cell lines through a mechanism that may involve apoptosis. Overall, Synechocystis ΔsigF is a promising

platform to study/manipulate EPS production and to obtain higher amounts of a biological active polymer. Moreover, SigF is

the first regulatory element associated to RPS production in Synechocystis, and the features associated to this polymer makes

it suitable for a wide range of biomedical applications.

(1) Mota, R et al. 2016. Appl Microbiol Biotechnol 1-11. (2) Leite, JP et al. 2016. Macromol Biosci

DOI:10.1002/mabi.201600206. (3) Pereira, S et al. 2009. FEMS Microbiol Rev 33:917-941. (4) Huckauf, J. et al. 2000. Microbiology 146: 2877-2889.

22

Dextran formamidines: A new and easily synthesizable

non-viral vector in gene delivery Konrad Hotzel 1, @ , Niels Dusek 2, @ , Dagmar Fischer 2, @ , Thomas Heinze 1, @

1 : Center of Excellence for Polysaccharide Research, Institute of Organic Chemistry and Macromolecular Chemistry,

Friedrich Schiller University of Jena

Humboldtstraße 10, 07743 Jena - Germany

2 : Institute of Pharmacy, Friedrich Schiller University of Jena Philosophenweg 14 07743 Jena - Germany

Although being a great concept with a lot of potential to treat various inherited and acquired diseases, gene delivery is still an

idea that suffers from the lack of suitable vectors. Synthetic polycations like polyethylenimine (PEI) show high transfection

but also high cytotoxicity. It is preferable to use biopolymers like dextran as backbone of non-viral vectors due to their inherent

biocompatibility, non-immunogenicity and non-antigenicity and to add cationic charge to it.

We recently reported a simple one-pot synthesis in which both reactive groups of the amino acid β-alanine react simultaneously

after activation with iminium chloride to form an ester bond with the polyol dextran and a formamidine group (1).

Formamidines are structurally related to guanidine-groups, which play key roles in the natural process of DNA-binding and

cell-penetration. The surprising structure was proven by NMR-spectroscopy. The resulting products show good properties as

potent new non-viral vectors in gene delivery by having good transfection rates with low cytotoxicity.

References

(1) K. Hotzel, T. Heinze; Carbohydrate Research, 434 (2016), 77-82

23

Approaches for the derivatization of polyols with amino

acids Ana Bratuša 1, *, @ , Silvo Hribernik 1, Thomas Elschner 3, Karin Stana-Kleinschek 1, 2, @ , Rupert

Kargl 1, 2, @

1 : University of Maribor, Faculty of mechanical engineering, Laboratory for the characterization and processing of

polymers

Smetanova ulica 17, 2000 Maribor, Slovenia - Slovenia

2 : Institute for Chemistry and Technology of Materials (ICTM), Graz University of Technology, Graz, Austria.

Stremayrgasse 9 A-8010 Graz - Austria - Austria

3 : Papiertechnische Stiftung

Pirnaer Straße 37, 01809 Heidenau - Germany

* Corresponding author

Polymer analogous derivatization reactions (homogeneous and heterogeneous) are powerful means of increasing the property

range and applicability of polysaccharides and synthetic polymers. Final properties of both polymer classes are defined by the

chirality, regioselectivity, solubility and chemical stability. Understanding and influencing the reactivity is very important,

because it allows us to synthesize materials with desired structure and properties. In this work derivatization of dextran and

polyvinyl alcohol (PVA) polymers with amino-acids or peptides was used to produce bioactive materials of interest. The

reactivity of natural polysaccharide was compared with those of polyvinyl alcohols in order to increase understanding and

estimate the influence of the polymer backbone on the outcome of the reaction and the final properties. Amino acids and

peptides were bound to the polymers via homogeneous esterification reactions in organic solvents using proper activating

reagents. The necessity of protecting groups was evaluated and protocols for their removal were established. Detailed analysis

of the degree of substitution (DS) was performed by charge titration, NMR and IR-spectroscopy. Selected obtained materials

were evaluated with respect to their bioactivity using cell viability tests. Common material forming techniques for polymers

(nano-precipitation, thin film preparation) were employed to obtain various shapes suitable to be used as biomaterials for regenerative medicine or theranostics.

24

Dextran-based hydrogels matrixes for biomedical

applications – synthesis and characterization. Kamila J. Szafulera 1, @ , Radoslaw A. Wach 1 , Piotr Ulanski 1

1 : Institute of Applied Radiation Chemistry, Faculty of Chemistry, Lodz University of Technology Wroblewskiego 15, 93-590 Lodz - Poland

Current scientific literature reports a number of applications for polysaccharides and their derivatives for biomedical purposes,

such as soft tissue engineering. Natural polymers are known for excellent biocompatibility and biodegradability, moreover

many of them are also able to support and intensify biological processes [1]. For this reason polysaccharides can be a

component of bioactive wound dressings, constituting so-called third generation of dressings for chronic wound healing.

Additionally, hydrogels of submicron dimensions (nano- and mikrogels) synthesized from natural-origin polymers can be

considered as drug delivery systems (DDS). Among many natural polymers, dextran and its functionalized derivatives are very interesting. Biomaterials based on dextran

are widely used for biomedical applications due to well-documented biocompatibility and biodegradability of this biopolymer

in physiological environment and its biological activity - it promotes vascularization. Its biomedical applications include

plasma expander, drug delivery systems and wound dressings dedicated to chronic wounds. In recent years, dextran hydrogels

have been investigated for tissue-engineering applications as 3D scaffolds to support and promote regeneration of tissue,

mainly due to their capacity to be designed to mimic the mechanical properties and water content of native tissues [2].

Incorporation of crosslinkable moieties (e.g. methacrylic groups -MA) into dextran structure allows to obtain derivatives

capable for crosslinking initiated by UV or ionizing radiation. The radiation technique is very efficient, versatile and clean tool

for modifying polymers in general. Unquestionable advantages of using radiation include possibility of processing materials

in any physical state, at a convenient temperature (usually room temperature), typically with no need of application of

additional initiators, catalysis, crosslinking agents nor other chemicals [3]. Moreover, if sufficient dose is applied (usually 25

kGy) the sterilization can take place simultaneously. In our recent study we have demonstrated possibility of radiation

synthesis of hydrogels based on biocompatible dextran methacrylate [4].

The current work was aimed to synthesize a dextran derivative having substituents capable of covalent crosslinking (Dex-MA

– dextran methacrylate), and to develop conditions suitable for formation of macroscopic and nano/micro-hydrogels with use

of clean techniques. Dextran derivatives has been synthesized by coupling glycidyl methacrylate with this polysaccharide,

yielding Dex-MA of the degree of methacrylate substitution (DS) ensuring solubility in water. The main goal was detailed

study on synthesizing dextran-based hydrogels by radiation-initiated crosslinking. A series of Dex-MA (DS ~ 0,1–1) solutions

has been treated by the beam of accelerated electrons in different concentration, and wide range of doses. The crosslinking of

Dex-MA in aqueous solutions was found to be an efficient process and the effect of crosslinking (intra- or intercrosslinking)

is dependent on the DS and the concentration applied. Macroscopic hydrogel synthesized from higher concentration (3 and

5%) were thoroughly characterized – the gel fraction (GF) and the equilibrium degree of swelling (EDS) were determined.

Moreover, for selected samples cytotoxicity tests were performed. It was shown, that the hydrogels of Dex-MA of DS below

1 were cytocompatible. The irradiation of Dex-MA in lower concentrations resulted in intracrosslinked forms, i.e. nano- and

microgels, which dimensions were dependent on used dose and concentration.

The collected results and observations made so far suggested that research in the field of radiation processing of Dex-MA is

extremely interesting, and demonstrated that both inter- and intramolecular crosslinking is feasible. Obtained final form of

hydrogels, both macroscopic and submicron hydrogels, can be anticipated as potential biomaterials used either in regenerative

medicine and as DDS.

Literature:

[1] Dumitriu S., Polysaccharides: structural diversity and functional versatility, CRC Press, Boca Raton FL (2005)

[2] G. Sun, et.al. Engineering dextran-based scaffolds for drug delivery and tissue repair, Nanomedicine, 7(11), 1771-1784

(2012)

[3] The Radiation of Chemistry of Polysaccharides, International Atomic Energy Agency, IAEA, Vienna (2016)

[4] Szafulera, K. et.al. Radiation synthesis of biocompatible hydrogels of dextran methacrylate, Radiat. Phys. Chem. 142; 115–

120 (2018)

25

Pullulan-based microneedles for transdermal delivery of

pharmaceutical ingredients Daniela F. S. Fonseca 1, *, @ , Carla Vilela 1, @ , Armando J. D. Silvestre 1, @ , Carmen S. R. Freire 1, @

1 : CICECO – Aveiro Institute of Materials, Department of Chemistry, University of Aveiro

3810-193 Aveiro, Portugal - Portugal * : Corresponding author

Microneedles (MNs), first conceptualized in 1976 (1), arise as micron-sized needles designed to disrupt the stratum corneum of

the skin, creating simple conduits through which external molecules can passively diffuse. Therefore, transdermal drug

delivery efficiency is improved and the number of drugs delivered by this route is significantly increased (2). These minimally

invasive devices have typical lengths ranging from 25 to 2000 μm (3), long enough to penetrate the SC, but short and narrow

to avoid stimulation of nerve fibers or puncture the blood vessels in the dermis. MNs can be fabricated using a plethora of

polymers, either from natural or synthetic origin and are usually classified accordingly to their performance in vivo as

dissolvable, biodegradable or swellable devices. In particular, dissolvable MNs are made from water-soluble polymers that

dissolve within a few minutes upon skin insertion, quickly releasing the preloaded cargoes (2).

In this context, MNs fabricated using dissolvable polymers, composed of pullulan (4), an exopolysaccharide produced by

several yeast species, were investigated. Pullulan-based MNs were successfully fabricated by micromolding using solvent

casting and polydimethylsiloxane molds. Appropriated mechanical evaluation showed that these MNs do not break but bend

under an axial force and therefore have sufficient mechanical force to allow skin insertion in vivo. The incorporation of

macromolecules (as insulin) within the pyramidal structure of these MNs, envying their rapid and efficient transcutaneous

delivery will be also discussed in this communication.

Acknowledgements: This work was developed within the scope of the project CICECO-Aveiro Institute of Materials, POCI-

01-0145-FEDER-007679 (UID/CTM/50011/2013), financed by national funds through the FCT/MEC and when appropriate

co-financed by FEDER under the PT2020 Partnership Agreement. The Portuguese Foundation for Science and Technology

(FCT) is also acknowledged for the doctoral grant to D.F.S. Fonseca (PD/BD/115621/2016), post-doctoral grant to C. Vilela

(SFRH/BPD/84168/2012) and contract under Investigador FCT to C.S.R. Freire (IF/01407/2012).

References:

(1) Gerstel, M. S.; Place, V. A. Drug Delivery Device, June 22, 1976.

(2) Larrañeta, E.; Lutton, R. E. M.; Woolfson, A. D.; Donnelly, R. F. Microneedle Arrays as Transdermal and Intradermal

Drug Delivery Systems: Materials Science, Manufacture and Commercial Development. Materials Science and Engineering

R: Reports 2016, 104, 1–32.

(3) Donnelly, R. F.; Singh, T. R. R.; Woolfson, A. D.; Raj Singh, T. R.; Woolfson, A. D. Microneedle-Based Drug Delivery

Systems: Microfabrication, Drug Delivery, and Safety. Drug delivery 2010, 17, 187–207.

(4) Singh, R. S.; Kaur, N.; Rana, V.; Kennedy, J. F. Pullulan: A Novel Molecule for Biomedical Applications. Carbohydrate Polymers, 2017, 171, 102–121.

26

Functional and Material Properties of a Novel

Microcrystalline Cellulose for Drug Delivery Lalduhsanga Pachuau 1, @

1 : Assam University Silchar, Assam 788011, Inde - India

Introduction: Microcrystalline cellulose (MCC) is an excellent directly compressible biomaterial that is listed as GRAS by

the FDA. The characteristics and functionality of MCC are found to be influenced significantly by the source of the cellulose

fibers and its processing conditions. The present study isolates MCC from Ensete glaucum pseudostem (E-MCC), a sustainable

and renewable bioresource and investigates its functionality to determine its suitability as drug delivery biomaterial.

Method: MCC was isolated from the pseudostem of E. glaucum. The degree of polymerization (DP), pH, moisture content

and ash value along with various micromeritic properties were determined. The particle size and shapes were studied through

optical microscopic method and data were analyzed using T-capture software. DSC and FTIR analysis were performed and

compared with standard Avicel PH 101. The compressibility and compactibility of the newly prepared E-MCC were also

evaluated through Kawakita plots and Heckel equation.

Results: The yield of MCC was found to be 33 %. FTIR and DSC studies indicate that the newly synthesized E-MCC and the

standard Avicel PH 101 exhibit similar characteristics. Moisture content, DP, pH, and the ash content were found to be within

pharmacopoeial limit. The equivalent diameter of E-MCC and Avicel PH101 were found to be 47.6 µm and 35.33 µm

respectively. The aspect ratio (b/l) were found to be 0.37 and 0.53 respectively for E-MCC and Avicel. From Kawakita plot

E-MCC was found to rearrange and pack slightly better than the Avicel while their cohesiveness was found to be almost

similar. From Heckel Plot, the yield value (Py) for E-MCC and Avicel was found to be 153.84 and 99.01 respectively.

Conclusion: From the present study, the performance and functionality of the newly synthesized E-MCC from a novel source were found to be comparable to the well established Avicel PH 101 standard.

27

Isolation and purification of high molecular weight chitin

from shrimp shells using deep eutectic solvents Bojana Bradic 1, @ , Uroš Novak 1, *, @ , Blaz Likozar 1, @

1 : National institute of Chemistry

Hajdrihova 19,1000 Ljubljana - Slovenia * : Corresponding author

Isolation and purification of high molecular weight chitin from shrimp shells using deep eutectic solvents

Bojana Bradić, Uroš Novak*, Blaž Likozar

National institute of chemistry, Department of Catalysis and Chemical Reaction Engineering, Hajdrihova 19, 1000,

Ljubljana, Slovenia

Global shellfishery waste generation is from 6 to 8 million metric tons annually.1 Chitin, the second most plentiful natural

polymer after cellulose is a linear amino polysaccharide composed of β-(1→4)-linked 2-acetamido-2-deoxy-β-D-glucose units

and can be isolated from the outer skeleton of crustaceans.2 Its bioactivity, biocompatibility, and low toxicity make it suitable

for controlled drug release formulations, cosmetics, food preservation, fertilizers, or biodegradable packaging materials, while

its ability to absorb both metal ions and hydrophobic organic compounds make it useful in wastewater processing and other

industrial applications3. Green technology actively seeks new solvents to replace common organic solvents that present

inherent toxicity and have high volatility, leading to evaporation of volatile organic compounds to the atmosphere.4 In this

work the new approach for recovery of chitin from shrimp shells using deep eutectic solvents (DESs) consisting of the mixtures

of Choline Chloride-Lactic Acid (CCLA), Choline Chloride-Malonic Acid (CCMA), Choline Chloride-Urea (CCU) and

Choline Chloride-Citric Acid (CCCA) is presented. The fractionation of the shrimp shell biomass with DESs was carried out

in a stirred reactor at different temperatures. The process selectivity in dissolution was followed on-line using FTIR and FBRM

spectroscopy probes submerged in DESs. The physiochemical properties and molecular mass of isolated chitin were compared

to chitin obtained by conventional methods. The results show that CCLA as the least viscous solvent has the best properties

for extraction of chitin, wherein the yield of the resulting chitin is higher than 18% with purity higher than 80%. Moreover,

CCMA and CCU have a positive effect on elimination minerals and proteins while CCCA shows the least capability for chitin

isolation from the shrimp shells.

References:

1 Xiaoyun Gao, Xi Chen, Jiaguang Zhang, Weimin Guo, Fangming Jin, and Ning Yan, Transformation of chitin and waste

Shrimp Shells into Acetic Acid and Pyrrole, Sustainable Chemistry Engineering, 2016, 4, 3912-3920.

2 Samuel M. Hudson, David W. Jenkins, Chitin and Chitosan.Encyclopedia of Polymer Science and Technology, 2001, 22,

52-54.

3 P.Rajasulochana , V.Preethy , Comparison on efficiency of various techniques in treatment of waste and sewage water – A

comprehensive review, Resource-Efficient Technologies, 2016, 4, 175-184.

4 Yuntao Dai Japvan, Sprosen Geart-Jan Witramp, Robert Verporte, Young Hae Choi, Natural deep eutectic solvents as new potential media for green technology, 2013, 766, 61-68

28

Thermodynamic study of the interaction of various salts

with cellulose nanocrystals Salvatore Lombardo 1, @ , Wim Thielemans 1, *, @

1 : Renewable Materials and Nanotechnology Research Group, Department of Chemical Engineering, KU Leuven

Campus Kulak Kortrijk, Etienne Sabbelaan 53, 8500 Kortrijk, Belgium - Belgium

* : Corresponding author

Isothermal Titration Calorimetry (ITC) is a promising technique to elucidate the thermodynamics of nanoparticle interactions.

In this study we used ITC to study the interactions of differently charged species with functionalized cellulose nanocrystals

(CNCs). Both anionic and cationic species were employed in this study. The binding of charged molecules to cellulose

nanocrystals was found to depend on the charge displayed on both components. Molecules bearing different amounts of

carboxylate anions were readily adsorbed onto positively charged nanocrystals. Similarly, cations were adsorbed onto

negatively charged CNCs. For all systems the binding mechanism between the CNCs nanocrystals and other species was found

to be endothermic and driven by an increase in entropy upon adsorption of the anions due to the release of surface bound water.

The stoichiometric interaction ratios determined were found to be lower than the values relative to processes involving ions in

solution, suggesting a more complex mode of interaction, most likely involving hydrogen-bonding and bridge formation.

However, the number of adsorbed ions was still directly correlated with the amount of surface graft. This makes it possible to

control the amount of surface interactions directly using the degree of substitution on the nanocrystal surfaces.

29

Surface treatment of chitosan fibers with polypyrrole Elena Rosova 1, *, @ , Elena Dresvyanina 2, 3, *, @ , Vladimir Yudin 1, 2 , Ekaterina Maevskaya 2 , Olga

Moskalyuk 3 , Elena Ivan'kova 1, 2

1 : Institute of Macromolecular Compounds RAS

Bolshoy pr. 31, 195251, Saint-Petersburg - Russia

2 : Peter the Great Saint-Petersburg Polytechnic University

Polytechnicheskaya, 29, 195251, Saint-Petersburg, - Russia

3 : Saint-Petersburg State University of Industrial Technologies and Design

B. Morskaya, 18, 191186, Saint-Petersburg - Russia

* : Corresponding author

Keywords: chitosan, fiber, wet spinning, polypyrrole, electrical conductivity, nerve tissue

Recently materials based on the natural polysaccharide chitosan are used for biomedical and medical applications, including

cell replacement technologies, tissue engineering, preparing wound dressing due to positive medical properties of chitosan.

Modifying chitosan-based materials with other kind of polymers or nanoparticles can contribute to the expansion of their

application areas. Electroconducting polymers (in particular, polypyrrole and polyaniline) are promising materials for use in

electronic area. Besides, polypyrrole is allowed for use in medicine. Deposition of these polymers on the surface of polymer

matrix leads to the formation of composites with a good mechanical properties and impart to them new properties, one of

which is electroconductivity. Polymer composites consisting of chitosan fibers and conducting polymer layers were elaborated

and investigated within this study. Conducting layers of polypyrrole (PPy) were formed by oxidative polymerization of

monomers onto chitosan fibers in situ from gaseous phase.

Fibers were spun from 4% chitosan solution in 2% acetic acid solution by coagulation method. The obtained fibers were first

saturated with an oxidant (ferric chloride solution in methanol and in water) and then they were put in a reaction vessel

containing pyrrole vapours at room temperature. The surface structures, morphology, electrical conductivity and mechanical

properties of composites depending on the oxidant solution, exposition in the oxidizer and polymerization time were studied.

Acknowledgment: Financial support of this work by RSF № 14-33-00003 is gratefully acknowledged.

Future perspective in polysaccharide research: The obtained results allow using of the chitosan-polypyrrole fibers as the matrices for the creation nerve tissue in replacement technologies.

30

Mimicking biological mechanical behavior by a bioactive

lactose-modified chitosan Franco Furlani 1, @ , Pasquale Sacco 1, @ , Michela Cok 1, @ , Fioretta Asaro 1, @ , Eleonora

Marsich 1, @ , Dan Cojoc 2, @ , Sergio Paoletti 1, @ , Ivan Donati 1, @

1 : University of Trieste

Piazzale Europa, 1, 34128 Trieste - Italy

2 : CNR-IOM [Trieste] National Research Council - Institute of Materials, Area Science Park, Basovizza, Trieste, ITALY - Italy

Mechanical factors are able to influence biological processes according to a mechanism termed mechanotrasduction.(1) There

is a growing effort to recreate mechanical properties of natural tissues by exploiting synthetic polymers.(2) CTL60 (also termed

as Chitlac) is a lactose-modified chitosan, which showed interesting biological and physical-chemical features; for instance it

was found to form highly homogeneous colloidal coacervates.(3) Its bioactivity was demonstrated vs. different cell types such

as chondrocytes,(4) osteoblasts(5) and neural cells.(6) The biological significance of CTL60 traced back to its interaction with

Galectin-1, which bridges polymer chains and cell surface integrins.(7) Rheological behavior of CTL60 upon treatment with

boric acid (used as cross-linking agent) was explored and an uncommonly high dependence in the scaling law between the

zero-shear viscosity and the concentration of CTL60 emerged, pointing to interesting potential implications in the field of

viscosupplementation.(8) When CTL60 was treated with boric acid, strain hardening effects and non-linear response to stress

were also noticed. Such trends are considered as hallmarks of cytoskeletal and biopolymer networks.(9-10) Resulting matrices

pointed at hybrid sol-gel samples and showed rheological properties similar to collagen and neurofilaments.(9) The elastic

modulus was found to markedly increase after stimulation at constant stress and frequency for few hours. Mechanical

properties of the solicited sample were higher than the non-stimulated sample; the stimulated sample behaved like a weak gel

and, therefore, a stress induced reticulation occurred. By NMR it was possible to identify the interaction sites of boric acid

binding to polymer. Mannitol was selected as competitor for boric acid binding to slow down gelation kinetics. Surprisingly,

mechanical properties were slightly higher by using a certain mannitol concentration.

Optical Tweezers were used as micro-rheology technique on dilute polymer solutions; experimental findings showed that

dynamic viscosity of the polymer treated with boric acid was about 20% higher than polymer alone. Giving the peculiar

properties of the obtained system, bioactivity of CTL60 could be linked to a mechanotrasduction mechanism mediated by the

presence of cross-linking agents.

References 1. Hoffman, B. D., et al. Nature 475, 316–323 (2011).

2. Varnosfaderani, M. et al. Nature 549, 497–501 (2017).

3. Furlani, F., et al. Carbohydr. Polym. 174, 360–368 (2017).

4. Donati, I. et al. Biomaterials 26, 987–98 (2005).

5. Travan, A. et al. Biomacromolecules 11, 583–592 (2010).

6. Medelin, M. et al. submitted

7. Marcon, P. et al. Biomaterials 26, 4975–4984 (2005).

8. Sacco, P., Furlani, F. et al. Biomacromolecules 18, (2017).

9. Storm, C., et al. Nature 435, 191–194 (2005). 10. Chaudhuri, O., et al. Nature 445, 295–298 (2007).

31

Electrospun cellulose acetate nanofibrous mats for

detection of pH in the wound bed Natalija Virant 1, @ , Manja Kurečič 1, 2, 3 , Silvo Hribernik 1, 2 , Mitja Kolar 4 , Tina Maver 1 , Alenka

Ojstršek 1, 2 , Uroš Maver 5, 6 , Lidija Gradišnik 5 , Karin Stana-Kleinschek 1, 2, 3

1 : Laboratory for Characterization and Processing of Polymers (LCCP), Faculty of Mechanical Engineering, University of

Maribor

Smetanova 17, 2000 Maribor - Slovenia

2 : Institute of automation, Faculty of Electrical Engineering and Computer Science, University of Maribor

Koroška cesta 46, 2000 Maribor - Slovenia

3 : Institute for Chemistry and Technology of Materials (ICTM), Graz University of Technolog

Stremayrgasse 9, 8010 Graz - Austria

4 : Faculty of Chemistry and Chemical Technology, University of Ljubljana

Večna pot 113, 1000 Ljubljana - Slovenia

5 : Institute of Biomedical Sciences, Faculty of Medicine, University of Maribor

Taborska ulica 8, 2000 Maribor - Slovenia

6 : Department of Pharmacology, Faculty of Medicine, University of Maribor Taborska ulica 8, 2000 Maribor - Slovenia

Keywords: electrospinning, benzocaine, cellulose acetate, nanofibers, drug release kinetics, pH-indicator

Abstract: Novel multifunctional bio-based nanofibrous mats, which contains active pain release substance is highly interesting in life

science application (e.g., wound healing). It is of great importance to ensure, a controlled release of active substances. One of

the promising techniques for preparation of nanofibrous material, with high surface area enabling the controlled release is

electrospinning. [1] Electrospinning is a method where electrostatic forces are used for producing continuous fibres with the

diameter from tens of nanometres to some micrometres with exceptionally large active surface area per mass unit. [2]

This study presents a highly simplified procedure to prepare a novel multifunctional nanofibrous material based on cellulose

acetate (CA) incorporated with benzocaine (BZC) and pH-change indicator dye bromocresol green (BCG) by electrospinning

process. We have studied the influence of solution parameters and electrospinning process parameters on formation of

nanofibres. Electrospun nanofibers were characterized by SEM and FTIR analysis, swelling behaviour and contact angle were

also investigated.

Smooth nanofibers with diameters ranging from 400 to 900 nm were electrospun from a 17 wt. % CA solution in 85 % acetic

acid. Optimal electrospinning parameters were 160 mm distance between the electrodes and 75 kV voltage. Electrospun CA

nanofibers were high hydrophobic (water contact angle: 134°) and also showed a tremendous water absorption capacity (1657

%). The addition of BZC and BCG in the spinning formulation did not affect the fiber formation. Results showed that the

release kinetics of BZC is pH-controllable and a maximum release is observed at pH 9.0, corresponding to the pH of infected

wound bed. The shift in colour of encapsulated BCG from yellow to blue is noticeable within a few seconds by naked eye

upon pH change from acidic to alkaline; illustrating its capacity as an in-situ pH-detecting system. Finally, the biocompatibility

test of multicomponent CA nanofibrous mesh with the human derived fibroblast assay showed no toxicity followed by

improved proliferation of cells, demonstrating its potential use as an active and beneficial material in wound care applications.

Acknowledgments The authors would like to acknowledge the financial support for this research received from the Slovenian Research Agency

(grant numbers: P2-0118, P3-0036, L2-5492, Z2-8168, I0-0029 and P1-0153).

References: [1] Rogina A. Electrospinning process: Versatile preparation method for biodegradable and natural polymers and biocomposite

systems applied in tissue engineering and drug delivery. Applied Surface Science, 296, 221–230, 2014. [2] Kurečič M., Sfiligoj Smole M. Electrospinning: Nanofibre Production Method. Tekstilec, 56 (1), 4-12, 2013.

32

Development of cellulose wound dressing materials with

rutin and polyrutin Tanja Pivec 1, @ , Rupert Kargl 2, 3 , Uroš Maver 4 , Silvo Hribernik 1, 3 , Matej Bračič 1 , Tamilselvan

Mohan 1, 5 , Karin Stana-Kleinschek 1, 2, 3, *, @

1 : Laboratory for Characterization and Processing of Polymers (LCPP), Faculty of Mechanical Engineering, University of

Maribor

Smetanova ulica 17, 2000 Maribor, Slovenia - Slovenia

2 : Institute for Chemistry and Technology of Materials (ICTM), Graz University of Technology

Stremayrgasse 9, 8010 Graz, Austria - Austria

3 : Institute of automation, Faculty of Electrical Engineering and Computer Science, University of Maribor

Koroška cesta 46, 2000 Maribor, Slovenia - Slovenia

4 : Institute for Biomedical Sciences, Faculty of Medicine, University of Maribor

Taborska ulica 8, 2000 Maribor, Slovenia - Slovenia

5 : Institute of Chemistry, University of Graz

Heinrichstrasse 28, 8010 Graz, Austria - Austria * : Corresponding author

Keywords: cellulose thin film, cellulose non-woven, rutin, polyrutin, antioxidant activity, release study.

Abstract: One of the systemic therapies (e.g. per os use) for the treatment of chronic leg ulcers is the use of micronized

purified flavonoid fraction (MPFF). Although studies have demonstrated its effectiveness, side effects in systemic treatment

are associated with gastric problems and neurological disorders [1, 2]. Also, such systemic flavonoid therapy has a drawback

related to the poor absorption of the formulation in the gastrointestinal tract [3]. In order to improve the efficacy of such and

similar flavonoid therapies, as well as to reduce the occurrence of unwanted side effects related to systemic therapy, we studied

the interaction of flavonoid rutin and enzymatically polymerized rutin (polyrutin) with cellulose surfaces with the aim of

creating a novel cellulose wound dressing material for the topical treatment of chronic leg ulcers. The interaction studies of

the cellulose materials with rutin and polyrutin were performed on model and real wound healing systems. The cellulose films

spin coated on the sensors of a quartz crystal microbalance (QCM-D) were used as a model wound dressing systems. The

influence of pH, salt concentration, and rutin/polyrutin concentration on the interaction with cellulose thin films was evaluated

by means of a QCM-D. The knowledge obtained through interaction studies on model wound healing systems was transferred

to the application of the coatings on real wound healing systems i.e. cellulose non-wovens. The surface morphology was

further characterised on model and real wound healing systems. The antioxidant activity and release kinetics were investigated

for a real wound healing system. The main results showed that a higher solubility of polyrutin at low ionic strength contributes

to the formation of continuous layers of polyrutin on cellulose surface, while the low solubility of rutin and reduced solubility

of polyrutin at higher ionic strengths contribute to deposition of particles of rutin and polyrutin on the cellulose surface. The

presence of particles on the surface of non-woven cellulose fibres led to a faster initial release of rutin and polyrutin. On the

contrary, a continuous layer of the well soluble polyrutin contributes to a prolonged release. Namely, adsorption of the water

soluble polyrutin at pH 2 without the addition of salt results in higher masses of attached polyrutin that release slower and over

longer time periods. Since wound dressing materials for chronic leg ulcers often require a lower frequency of dressing change,

the latter could provide an efficient therapeutic approach to their treatment.

Acknowledgements: The research work was financially supported by the Slovenian Research Agency in the frame of

programme groups P2-0118 and P3-0036, as well through the research training programme for Junior researchers.

References: 1. Micronised purified flavonoid fraction: a phlebotropic agent that is useful in the treatment of chronic venous insufficiency

and venous ulcer.Drugs & Therapy Perspectives, 2003. 19(11): p. 1-4.

2. Lyseng-Williamson, K.A. and C.M. Perry, Micronised Purified Flavonoid Fraction. Drugs, 2003. 63(1): p. 71-100.

3. Garner, R.C., et al., Comparison of the absorption of micronized (Daflon 500 mg) and nonmicronized 14C-diosmin tablets

after oral administration to healthy volunteers by accelerator mass spectrometry and liquid scintillation counting. J Pharm Sci, 2002. 91(1): p. 32-40.

33

Tuesday 15th of May 2018

ROOM FRANA MIKLOŠIČA

InnoRenew CoE Renewable Materials and Healthy

Environments Research and Innovation Centre of

Excellence Črtomir Tavzes 1, @ , Andreja Kutnar 1, @

1 : InnoRenew CoE Renewable Materials and Healthy Environments Research and Innovation Centre of Excellence

Abstract: The InnoRenew CoE is an interdisciplinary research institute located in Slovenia. The InnoRenew CoE aims to be

a world leader in the application and implementation of renewable materials and sustainable building research by focusing on

wood modification and restorative environmental and ergonomic design (REED).

The InnoRenew CoE is currently designing a brand new research building with infrastructure and equipment to explore a wide

variety of topics critical to the advancement of renewable materials research. A growing team of researchers will study how

human health is affected by the built environment; integrate computer science and IT into building and product design and

support forest sector companies with digital strategies and technologies; examine the fundamentals of wood modification and

apply those findings to industrial applications; study new renewable materials composites; and investigate and find solutions

for creating healthier, more sustainable buildings from renewable materials.

34

Monosaccharide Chemistry Martin Thonhofer 1, *

1 : Laboratory for Characterization and Processing of Polymers (LCCP), Faculty of Mechanical Engineering, University of

Maribor

* Corresponding author

Abstract: Carbohydrates (sugars or saccharides) are the most widely distributed naturally occurring organic compounds on

earth. Nonetheless, due to a number of reasons, considerably little attention has been drawn to carbohydrate chemistry over

the last decades. Although there are approximately two hundred monosaccharides found in nature, they only differ from each

other in a few structural features. The chemical complexity of carbohydrates exacerbates their synthesis as well as their

analytical characterization, when compared to other biomolecules. Thus, due to their high level of functionalization, even low

molecular weight derivatives may provide difficult problems in terms of synthesis and analytics. In this context, simple considerations regarding typical problems as well as fundamental synthetic strategies will be presented and discussed.

35

The influence of zinc oxide nanorods on chitosan-based

film properties for food packaging Zélia Alves 1, @ , Paula Ferreira 1, @ , Cláudia Nunes 1, @

1 : Universidade de Aveiro Campus Universitário de Santiago 3810-193 Aveiro - Portugal

The increased use of non-biodegradable plastics as food packaging materials, mostly derived from petroleum-based materials,

is causing huge environmental problems. A good alternative, to meet the increasing demand for sustainability, can be the use

of biodegradable and renewable resources, as polysaccharides. Chitosan has a good film forming capability in addition to its

antioxidant and antimicrobial activity. Therefore, this polysaccharide has active properties adequate to food packaging

materials [1]. However, mechanical and barrier properties of chitosan films are not suitable for food packaging, then a strategy

to improve these properties is the incorporation of inorganic materials as metal oxide nanoparticles in polysaccharide matrix

[2]. Besides, zinc oxide has antimicrobial activity and UV-light protection. In this study, zinc oxide nanorods were produced

by solvothermal process using ethanol. The effect of ZnO nanofiller addition in different loadings on the crystalline structure,

physicochemical, and mechanical properties of bionanocomposite films is investigated and will be discussed in order to show

the viability of these bionanocomposites for active food packaging.

References [1] Fernandez-Saiz P. Chitosan polysaccharide in food packaging applications. Multifunct. Nanoreinforced Polym. Food

Packag., Woodhead Publishing; 2011, p. 571–93.

[2] Espitia PJP, Otoni CG, Soares NFF. Zinc Oxide Nanoparticles for Food Packaging Applications. Antimicrob. Food

Packag., San Diego: Academic Press; 2016, p. 425–31.

Acknowledgement FCT/MEC for the financial support to CICECO-Aveiro Institute of Materials (Ref. FCT UID/CTM/50011/2013 and POCI-

01-0145-FEDER-007679), through national founds and where applicable co-financed by the FEDER, within the PT2020

Partnership Agreement. ZA, CN and PF thank FCT for the grants (PD/BD/117457/2016, SFRH/BPD/100627/2014 and IF/00300/2015, respectively). This work was also supported by BIOFOODPACK project (M-ERA.NET2/0019/2016)

36

The influence of neutralization on the properties and

structure of chitosan films Urška Jančič 1, *, @ , Silvo Hribernik 1, 2 , Tamilselvan Mohan 1 , Rupert Kargl 1, 2, 3 , Karin Stana-

Kleinschek 1, 2, 3 , Mojca Božič 2, 1

1 : Laboratory for Characterization and Processing of Polymers (LCCP), Faculty of Mechanical Engineering, University of

Maribor

Smetanova 17, 2000 Maribor - Slovenia

2 : Institute of automation, Faculty of Electrical Engineering and Computer Science, University of Maribor

Koroška cesta 46, 2000 Maribor - Slovenia

3 : Institute for Chemistry and Technology of Materials (ICTM), Graz University of Technology

Stremayrgasse 9, 8010 Graz - Austria * : Corresponding author

Keywords: chitosan film, neutralization, mechanical properties, barrier properties

Abstract: Chitosan is one of the most abundant biopolymers after cellulose. Chitosan-based materials have been widely applied in

various fields for their biological and physical properties of biocompatibility, biodegradability, antimicrobial ability, and easy

film forming ability [1]. Along with the advances in the nanotechnology and polymer science, different strategies have been

employed to prepare chitosan-based films with multiple functionalities such as solution casting, coating, dipping, layer-by-

layer assembly, and extrusion [2]. Chitosan is not soluble in pure water, but has certain solubility in different acids (i.e. acetic,

hydrochloric, formic, lactic, propionic acids, etc.), which leads to the film-forming ability. Due to unique property of increased

viscosity upon hydration, chitosan polymer may be used as edible and degradable films or coatings. Uses for chitosan films

have been limited because of their high moisture permeability and mechanical problems. However, the properties of chitosan

films can be modified to improve mechanical and functional properties by controlling the film forming solution pH or acids.

In this work we investigated the effect of chitosan film forming solution pH on the film properties before and after surface

neutralization, such as microstructure, chemical structure, crystallinity, mechanical performance, and barrier properties (water

vapor barrier property and oxygen transmission rate property). The chitosan film preparation included following steps: (i)

dissolving chitosan in acid solution at pH 2, (ii) adjusting chitosan solution to planned pH 4 and 6, (iii) solution casting, (iv),

drying, (v), film neutralization with 1 M NaOH, (vi) film washing with distillated water and (vii) drying. For chitosan

morphology characterization scanning electron (SEM) and atomic force microscope (AFM) were used. The change in

morphology roughness before and after films neutralization can be observed in Figure 1. A relatively high amount of micro-

voids can be seen in chitosan film prepared from chitosan solution at pH 2. By increasing pH of chitosan solution to 4 and 6,

films became smoother without voids. Post film neutralization additional smoothed the film surface. Mechanical and barrier

properties were improved by increasing the chitosan solution from pH 2 to 6. Post film neutralization influenced the

intramolecular and intermolecular interactions and consequence improved all examined properties.

Acknowledgments The authors would like to acknowledge the financial support received in the frame of M-era.NET program (NanoElEm -

Designing new renewable nano-structured electrode and membrane materials for direct alkaline ethanol fuel cell

- http://nanoelmem.fs.um.si/, grant number C3330-17-500098).

Future perspective in polysaccharide research: Future developments in chitosan films should be considered in the following

aspects: (i) different chitosan derivatives and additive materials are needed to be explored and produced to meet special

requirement and (ii) new technologies are required for the facilely mass production of the chitosan films with desired properties

to meet industry demands.

References: [1] Leceta I., Guerrero, P., de la Caba, K., Carbohydrate Polymers. 2013, 93, 339–346.

[2] Wang H., Qian J., Ding F., Journal of Agricultural Food Chemistry. 2018, 66, 395−413.

37

Physical, antioxidant and antimicrobial properties of

chitosan-based films incorporated with hop extract Marijan Bajić 1, @ , Helena šeme 2, @ , Uroš Novak 1, @ , Gregor Kosec 2, @ , Blaž Likozar 1, @

1 : Department of Catalysis and Chemical Reaction Engineering, National Institute of Chemistry

Hajdrihova 19, SI-1001 Ljubljana - Slovenia

2 : Acies Bio Tehnološki park 21, SI-1001 Ljubljana - Slovenia

Chitosan, a polysaccharide derived from naturally renewable and abundantly present chitin becomes a prominent candidate

capable of replacing synthetic polymers in many applications.[1] Thanks to its biocompatibility and non-toxicity, chitosan-

based films are attracting a remarkable attention as active food packaging materials.[2] These films are usually further

improved by incorporation of plant extracts that have antimicrobial and antioxidant activity.[3] Regarding that, one of the most

promising natural extracts that deserves attention is a hop (Humulus lupulus) extract.[4]

This work deals with the development and functional characterization of chitosan-based films incorporated with a supercritical

carbon dioxide hop extract (HE). Namely, films with different concentration of HE were prepared by the casting method and

analyzed regarding their physical, morphological as well as antioxidant and antimicrobial properties.

Preliminary results have revealed that obtained films have up to 30% of water as well as sufficient mechanical and chemical

stability. Besides, it has been shown that the antioxidant capabilities are increasing, while the solubility in water and swelling

degree are decreasing, along with the addition of HE. Such results make chitosan-based films incorporated with HE very

suitable for the possible utilization as active food packaging materials.

Keywords: chitosan-based films, hop extract, food packaging

Literature

Muxika, A., Etxabide, A., Uranga, J., Guerrero, P., & de la Caba, K. (2017). Chitosan as a bioactive polymer: processing,

properties and applications. International journal of biological macromolecules.

Van den Broek, L. A., Knoop, R. J., Kappen, F. H., & Boeriu, C. G. (2015). Chitosan films and blends for packaging

material. Carbohydrate polymers, 116, 237-242.

Hafsa, J., ali Smach, M., Khedher, M. R. B., Charfeddine, B., Limem, K., Majdoub, H., & Rouatbi, S. (2016). Physical,

antioxidant and antimicrobial properties of chitosan films containing Eucalyptus globulus essential oil. LWT-Food Science

and Technology, 68, 356-364.

Rój, E., Tadić, V. M., Mišić, D., Žižović, I., Arsić, I., Dobrzyńska-Inger, A., & Kostrzewa, D. (2015). Supercritical carbon

dioxide hops extracts with antimicrobial properties. Open Chemistry, 13(1).

38

Starch films reinforced with broccoli by-products with

antioxidant activity Sónia S. Ferreira 1, *, @ , Idalina Gonçalves 1, 2, @ , Susana M. Cardoso 1, @ , Dulcineia Ferreira

Wessel 3, @ , Manuel A. Coimbra 1, @

1 : QOPNA, Department of Chemistry, University of Aveiro

Campus Universitário de Santiago 3810-193 Aveiro, Portugal - Portugal

2 : CICECO - Aveiro Institute of Materials, Department of Materials and Ceramic Engineering, University of Aveiro

Campus Universitário de Santiago 3810-193, Aveiro, Portugal - Portugal

3 : CI&DETS, Polytechnic Institute of Viseu – Agrarian Higher School

Quinta da Alagoa, Estrada de Nelas 3500-606, Viseu, Portugal - Portugal

* : Corresponding author

Starch films represent an alternative to non-biodegradable synthetic materials. However, their inherent water hydrophilicity

and poor mechanical properties are disadvantageous [1]. Therefore, in this work, starch films were reinforced with broccoli

by-products to evaluate the impact in water contact angle and mechanical properties. Furthermore, due to the known

antioxidant compounds present in broccoli by-products [2], the antioxidant activity by inhibition of 2,2′-azinobis-3-

ethylbenzothiazoline-6-sulfonic acid (ABTS) radical was also evaluated.

The starch was obtained from potato washing slurries. Broccoli by-products were obtained from frozen-food industry and were

used fresh, after dehydration, and after dehydration and water extraction. Starch suspensions (4 % w/v) were stirred for 5-10

min with 1.2 g of glycerol, as plasticizer, and with 0.5%, 1%, or 2% w/w of starch of broccoli by-product or without it as

control. The resulting suspensions were gelatinized at 95ºC, for 30 min, with stirring. Afterwards, they were filtered, degassed,

and films were produced by solvent casting.

The water contact angles with the up and down surfaces of control film were 43.1±2.1º and 43.7±0.4º, respectively. The

addition of broccoli by-products allowed to obtain films with hydrophobic surfaces (angle higher than 90º). Control starch film

had a thickness of 76.0±2.7, presented a tensile strength of 21.9±1.0 MPa, a Young's modulus of 1.28±0.03 GPa, and an

elongation at break of 2.42±0.24%. The incorporation of broccoli by-products led to more resistant, rigid, and flexible films.

An increase of ABTS radical inhibition was also observed.

These results show that the incorporation of broccoli by-products in starch films improved water hydrophobicity and

mechanical properties, and allowed to obtain starch films with antioxidant activity, showing a potential application on the

packaging field.

[1] Jiménez, A., Fabra, M. J., Talens, P., & Chiralt, A. (2012). Edible and biodegradable starch films: a review. Food and

Bioprocess Technology, 5(6), 2058-2076.

[2] Ferreira, S. S., Passos, C. P., Cardoso, S. M., Wessel, D. F., & Coimbra, M. A. (2018). Microwave assisted dehydration of

broccoli by-products and simultaneous extraction of bioactive compounds. Food Chemistry, 246, 386-393.

39

Development of chitosan/graphene oxide composites for

potential application as anion-exchange membranes in

fuel cells Barbara Kaker 1, *, @ , Silvo Hribernik 1, 2, @ , Tamilselvan Mohan 1, @ , Rupert Kargl 1, 2, 3, @ , Karin

Stana-Kleinschek 1, 2, 3, @ , Egon Pavlica 4, @ , Mojca Božič 1, 2, @

1 : Laboratory for Characterization and Processing of Polymers (LCCP), Faculty of Mechanical Engineering, University of

Maribor

Smetanova 17, 2000 Maribor - Slovenia

2 : Institute of automation, Faculty of Electrical Engineering and Computer Science, University of Maribor

Koroška cesta 46, 2000 Maribor - Slovenia

3 : Institute for Chemistry and Technology of Materials (ICTM), Graz University of Technology

Stremayrgasse 9, 8010 Graz - Slovenia

4 : Laboratory of Organic Matter Physics, University of Nova Gorica

Ajdovščina - Slovenia * : Corresponding author

Keywords: chitosan, graphene oxide, ethanol fuel cells, anion-exchange membrane

Abstract: Alkaline fuel cells (AFC) are electrochemical devices that continuously convert chemical energy of fuel into electricity. The

so-called direct alcohol fuel cells (DAFC) are a group of AFCs, containing alcohol fuel which shows a variety of advantages

in comparison to hydrogen as fuel. An anion exchange membrane (AEM) is the core of DAFC and is formed by sandwiching

a multi-layered structure (i.e. anode catalyst or diffusion layer and AEM) between the anode and cathode. Chitosan (CS), as a

biopolymer, is one of the promising membrane materials and could produce more economical fuel cells. To form alkaline

AEMs, CS membrane composites can be modified with quaternary ammonium groups. A novel cross-linked quaternized CS

AEMs could exhibit conductivity up to 7.3 ± 0.22 × 10-3 S cm-1 with a maximum current density of about 65 mA cm-2 [1]. In

our work the CS composite membranes were prepared by using 1 M NaOH for chitosan solution neutralization, with further

addition of graphene oxide (GO) and benzyltrimethylammonium chloride (BTMAC) for quaternization. Procedure for CS-GO

membranes preparation was the following: 1.0 wt % of CS (90 % deacetylated chitosan) was dissolved (addition of 1 M HCl)

at pH 2.0, followed by adding 1 M NaOH to reach pH 6.0, and later addition of a certain amount of graphene oxide (GO-

Sigma) and/or BTMAC. Solution casting technique was used for membrane formation that were oven-dried at 40 °C. The

membrane was afterwards neutralized with 1 M NaOH, thoroughly washed and dried on air.

For membrane morphology characterization scanning electron (SEM) and atomic force microscope (AFM) were used.

Hydrophilicity/hydrophobicity was determined by contact angle measurements, mechanical properties (tensile strength, etc.)

by mechanical testing and ionic conductivity by alternating current impedance method. Further on, swelling ratio/KOH uptake

and ethanol permeability were measured. SEM images show the surface morphologies for pristine CS and CS-0.01 wt % GO

membrane (Figure 1). The change in morphology roughness can be observed. GO sheets are uniformly dispersed along the CS

membrane. Contact angle results indicated on relatively hydrophobic membranes with contact angles of around 99.5°. Newly

produced membranes have high ionic conductivity up to 59 ± 8 × 10-3 S/cm and low ethanol permeability of around 1.8 × 10-

7 cm2/s. Obtained results revealed that newly produced membranes are potentially applicable for ethanol fuel cells.

Acknowledgments The authors would like to acknowledge the financial support received in the frame of M-era.NET program (NanoElEm -

Designing new renewable nano-structured electrode and membrane materials for direct alkaline ethanol fuel cell

- http://nanoelmem.fs.um.si/, grant number C3330-17-500098).

Future perspective in polysaccharide research: Newly produced modified chitosan composite membranes have been proven

to be cost-effective approach and provides fuel cell´s operating reliability.

References: [1] Wan Y., Peppley B., Creber K., Bui V. and Halliop E., J. Power Sources. 2008, 185,183–187.

40

Novel chitosan-based silica-coated magnetic

nanocomposites as a potential adsorbent for heavy metals Olivija Plohl 1, *, @ , Urban Ajdnik 1, @ , Sašo Gyergyek 2, 3, @ , Irena Ban 3, @ , Alenka Vesel 2, @ , Tjaša

K. Glaser 1, @ , Lidija Fras Zemljič 1, @

1 : University of Maribor, Faculty of mechanical engineering, Laboratory for characterization and processing of polymers

Smetanova ulica 17, Maribor - Slovenia

2 : Jozef Stefan Institute [Ljubljana, Slovenia]

Jamova cesta 39, 1000 Ljubljana Slovenia - Slovenia

3 : University of Maribor, Faculty of chemistry and chemical technology, Laboratory for inorganic chemistry

Smetanova ulica 17, 2000 Maribor - Slovenia

* : Corresponding author

Olivija Plohl1,*, Urban Ajdnik1, Sašo Gyergyek2,3, Irena Ban3, Alenka Vesel4, Tjaša K. Glaser1, Lidija Fras Zemljič1

1University of Maribor, Faculty of mechanical engineering, Laboratory for characterization and processing of polymers,

Maribor, Slovenia

2Jožef Stefan Institute, Department for materials synthesis, Ljubljana, Slovenia

3University of Maribor, Faculty of chemistry and chemical technology, Laboratory for inorganic chemistry, Maribor,

Slovenia

4Jožef Stefan Institute, Department of surface engineering and optoelectronics, Ljubljana, Slovenia

*olivija.plohl@um.si

Abstract:

The sludge from municipal and industrial water-treatment plants can be due to its pollution regarded as a big problem.

Especially the presence of metals need to be reduced or eliminated to be able to reuse these sludge as a material with new

added value, e.g. as a fertilizer [1]. Thus, the development of the nanocomposites with strongly covalently attached amino-

biosorbent for effective heavy metal removal from waste sludge is an important issue. For this purpose, we synthesized

magnetic nanocomposites from ~13 nm-sized magnetic maghemite core [2], coated with the around 7 nm thick silica layer

(i.e. MNPs@SiO2) [3]. To achieve strong bond formation, the abundant silanol groups on silica coating were chemically

coupled with amino-biopolymer carboxy-methyl chitosan (CMC) using the principle of carboimide chemistry. The crystal

structure of MNPs was determined with X-ray powder diffraction (XRD), while the morphology, size and homogeneous silica-

shell thickness were analysed with transmission electron microscopy (TEM). The successful chemical coupling of silica-coated

MNPs with CMC was confirmed with infrared spectroscopy (ATR-FTIR). The quantification of amino-biopolymers on

MNPs@SiO2 was performed with termogravimetric analysis (TGA), while the magnetic properties were measured with

vibrating-sample magnetometer (VSM). To study the effect of the chemical stability, the efficiency of the CMC covalent

bonding was tested at alkaline pH value (for simulation of sludge conditions and the stability of biopolymer) using indirect

(i.e polyelectrolyte titration) analysis. For their application in heavy metal removal, the amino-biopolymer-based silica-coated

MNPs can represent an efficient and stable novel adsorbent.

References: [1] B. Bratina, A. Šorgo, J. Kramberger, U. Ajdnik, L. F. Zemljič, J. Ekart, and R. Šafarič, “From municipal/industrial

wastewater sludge and FOG to fertilizer: A proposal for economic sustainable sludge management,” J. Environ. Manage., vol.

183, pp. 1009–1025, 2016.

[2] S. Campelj, D. Makovec, and M. Drofenik, “Preparation and properties of water-based magnetic fluids,” J. Phys. Condens.

Matter, vol. 20, no. 20, p. 204101, 2008.

[3] S. Kralj, D. Makovec, S. Čampelj, and M. Drofenik, “Producing ultra-thin silica coatings on iron-oxide nanoparticles to

improve their surface reactivity,” J. Magn. Magn. Mater., vol. 322, no. 13, pp. 1847–1853, 2010.

Acknowledges: This work was financially supported by the Ministry of Education, Science and Sport under contract C3330-17-529004 and

by the Slovenian research agency within program P2-0118.

41

Anisotropic Diffusion and Phase Behaviour of Cellulose

Nanocrystal Suspensions Jonas Van Rie 1, @ , Salvatore Lombardo 1, @ , Alican Gencer 1, @ , Christina Schütz 2, @ , Kyongok

Kang 3, @ , Wim Thielemans 2, *, @

1 : Renewable Materials and Nanotechnology Research Group, Department of Chemical Engineering, KU Leuven

Campus Kulak Kortrijk, Etienne Sabbelaan 53, 8500 Kortrijk, Belgium - Belgium

2 : Université de Luxembourg

Avenue de la Faïencerie, 1511 Luxembourg - Luxembourg

3 : Forschungszentrum Jülich GmbH

Wilhelm-Johnen-Straße, 52428 Jülich - Germany

* : Corresponding author

Cellulose nanocrystals (CNCs) are biodegradable polymers built up from glucose units, bearing hydroxyl groups which can

be modified with a variety of possible functional groups, making these nanomaterials very interesting for the assembly with

other (inorganic) particles. Ever since the first description by Gray and co-workers of the formation of a nematic liquid

crystalline phase, researchers started to investigate self-assembly in the nematic phase. However, many forces influence the

quality of the final material, and their diffusion has never been investigated in detail for more concentrated systems. We used

dynamic light scattering in polarized and depolarized mode to determine the rotational and translational diffusion coefficients

of 1-5 wt% CNC suspensions. Interestingly, the presence of the phase transition was clearly present in the translational

diffusion data: two different regimes were found starting around 3 wt%, the starting point for the formation of nematic domains.

The behaviour of parallel and perpendicular diffusion coefficients was furthermore found to be concentration dependent: upon

phase transition, rods start to align and available space increases resulting in a higher parallel translational diffusion coefficients

at increasing CNC concentrations around the transition point due to increased translational entropy upon CNC alignment. We quantified diffusion for aqueous CNC suspensions and will explain the role of interparticle effects.

42

Water vapor diffusivity estimation in a polydisperse

sample of micrometric size cellulose particles Valentin Thoury 1, @ , Hélène Angellier-Coussy 1, @ , Valérie Guillard 1, @ , David

Legland 2, @ , Sébastien Gaucel 3, *, @

1 : Ingénierie des Agro-polymères et Technologies Émergentes

Université de Montpellier : UMR1208

2 place Pierre Viala - France

2 : Unité de recherche sur les Biopolymères, Interactions Assemblages

Institut National de la Recherche Agronomique : UR1268

rue de la Géraudière - France

3 : Ingénierie des Agro-polymères et Technologies Émergentes

Institut National de la Recherche Agronomique : UMR1208

2 place Pierre Viala - France * : Corresponding author

Abstract In order to develop reliable mathematical models able to predict mass transfer properties in biocomposites, it is necessary to

accurately characterize mass transfer properties in each constituent. This still remains a bottleneck in the case of micrometric

size lignocellulosic particles. In this context, the present study aimed at showing the importance of considering the whole

particle size distribution instead of summary descriptors (mean, median, mode) to estimate water vapor diffusivity in a

polydisperse cellulose sample. The morphology of cellulose particles was characterized by 2D image analysis by measuring

the major and minor axes lengths of the fitted ellipse of cellulose particles. These lengths were assimilated to the length and

the diameter of 3D cylinders. Water vapor sorption kinetics were performed at 25°C using a quartz crystal microbalance

(QCM) coupled with an adsorption/desorption system. QCM accessed mass variation per unit area as a function of time by

recording alteration in frequency of a quartz resonator. Water vapor uptake was measured at 8 successive steps of relative

humidity to obtain sorption kinetics. The impact of the elongation factor (ratio between the major and the minor axis) of

cellulose particles on water vapor diffusivity was studied by considering two contrasted morphologies of particles, i.e. a small

elongation factor (<2) and a medium elongation factor (=10).Mathematical model based on analytical solution of the 2nd Fick's

law for diffusion in a finite cylinder was used to estimate the apparent water vapor diffusivity in cellulose. This solution was

considered in a non-linear regression procedure, based on least squares minimization, to perform numerical identification of

the diffusion coefficient. Considering the 2D size distribution, average diffusivities of 6.8x10-13 ± 1.1x10-12 m².s-1 and

9.3x10-13 ± 9.5x10-12 m².s-1 were obtained for small and medium elongation factors, respectively. In contrast, the use of

median values for major and minor axes underestimates diffusivities with relative errors of 68% and 55% for small and medium

elongation factors, respectively. It was thus concluded that the use of a 2D size distribution was necessary to achieve an

accurate representation of the estimated parameter.

Keywords: Cellulose, 2D size distribution, Water vapor diffusivity, Mass transfer

43

Nanofibrillated cellulose stabilized Pickering emulsion as

templates for thermal superinsulating materials Clara Jimenez Saelices 1, @ , Bastien Seantier 2 , Yves Grohens 2 , Isabelle Capron 1, @

1 : INRA

Institut National de la Recherche Agronomique - INRA (FRANCE)

RUE DE LA GERAUDIERE - France

2 : IRDL

IRDL

Centre de recherche Huygens - BP 92116 - 56321 Lorient cedex - France

Thermal insulation is a key technology for energy conservation in the 21st century. Aerogels are highly porous materials which

have attracted much attention as thermal insulators. The use of polysaccharides to develop bioaerogels with low environmental

impact has seen an increased interest. In this area, nanocelluloses have shown a particular interest in research and industries.

However, practically nothing is known about thermal conductivity of bioaerogels, with only few publications reporting

examples of insulating aerogels. The thermal conductivity of aerogels can be tuned by their morphology. In this work, we

describe a new process to prepare an ecofriendly porous aerogel with high mechanical and thermal superinsulating properties.

Pickering emulsions were prepared and characterized using nanofibrillated celluloses as unique stabilizers. The control of

emulsion's architecture allows the preparation of aerogels with a hierarchical morphology involving three levels of porosity.

We performed a detailed analysis of the bioaerogels' morphology and we specifically highlight its influence in the mechanical

and thermal insulating properties.

44

Making bio-based materials from microalgae: solvent

and plasticization routes Nicolas Le Moigne 1, @ , Florian Delrue 2, @ , Jean-Francois Sassi 3, @ , Guilhem Arrachart 4, @

1 : Centre des Matériaux des Mines d'Alès (C2MA) - Website

Ecole Nationale Supérieure des Mines d'Alès

6 avenue de clavières 30319 Alès - France

2 : Commissariat à l'Energie Atomique et aux Energies Alternatives (CEA) - Website

CEA

CEA - Direction de la Recherche Technologique Centre de Cadarache - Cité des Energies 13108 SAINT PAUL LEZ

DURANCE - France

3 : Commissariat à l'Energie Atomique et aux Energies Alternatives

CEA - Direction de la Recherche Technologique Centre de Cadarache - Cité des Energies 13108 SAINT PAUL LEZ

DURANCE - France

4 : Institut de Chimie Séparative de Marcoule

Université Montpellier 2 - Sciences et Techniques, Commissariat à l'énergie atomique et aux énergies alternatives, Ecole

Nationale Supérieure de Chimie de Montpellier, Université de Montpellier, Centre National de la Recherche Scientifique :

UMR5257 30207 BAGNOLS SUR CEZE CEDEX - France

The research on microalgae currently shows a strong worldwide development. Although existing productions and commercial

applications mainly concern the food industry and the pharma- nutraceuticals and cosmetic, the capacity of microalgae to

efficiently use solar energy and CO2 to produce lipids, proteins and carbohydrates as well as unique products like antioxidants,

fatty acids, peptides, sterols... make them promising sources of energy, intermediate chemicals and materials. The present

research work aims to prepare bio-based polymer materials from microalgae. Two main processing strategies are investigated:

(i) the dissolution of microalgae to prepare biopolymer based solutions and (ii) the direct plasticization of microalgae to prepare

biopolymer blends. To this aim, a screening on various freshwater and seawater microalgae exhibiting different biochemical

composition and cellular structures, was conducted. Furthermore, growing conditions of microalgae were controlled so as to

investigate the possibility to enrich cells in biopolymers of interest (especially starch). The dissolution of microalgae was

achieved in Ionic liquids (ILs) with controlled hydrophilic/hydrophobic balance, due to their high ability to solvate organic

compounds and their environmental compatibility compared to chemical extraction methods involving organic solvents. The

plasticization of microalgae was achieved by twin screw extrusion with glycerol as a plasticizer, and biopolymer blends

composed of plasticized microalgae with fractions of Poly(butylene Succinate) (PBS) were prepared. First microalgae based

objects were produced in the form of gels, foams and bulk materials (See Figure). This set of results opens interesting perspectives about the use of microalgae for producing bio-based polymer materials.

45

Insights in electrostatic interactions between cationic

modified cellulose and microalgae An Verfaillie 1, 2, @ , Jonas Blockx 1, 2, @ , Wim Thielemans 1, *, @ , Koenraad Muylaert 2, *, @

1 : Renewable Materials and Nanotechnology Research Group, Department of Chemical Engineering, KULeuven, Campus

Kulak Kortrijk

Etienne Sabbelaan 53 8500 Kortrijk - Belgium

2 : Laboratory for Aquatic Biology, Department of Biology, KULeuven, Campus Kulak Kortrijk

Etienne Sabbelaan 53 8500 Kortrijk - Belgium

* : Corresponding author

Our group introduced cationic cellulose nanocrystals (CNCs) as new flocculants in microalgae harvesting. Although

microalgae form a green alternative as a source for biomass, the high cost and energy demand in downstream processing,

especially harvesting, hinders global commercialization. Flocculation offers a low-cost solution for harvesting microalgae.

The interactions between the negatively charged algal cells and positively charged CNC flocculants are mainly electrostatic

in nature and depend directly on the degree of positive surface charges on the flocculant. We modified the CNCs with

varying amounts of pyridinium and methylimidazolium groups to gain insights into the interaction mechanisms between the

negative charged algal cells and the cationic CNCs. Flocculation experiments were performed with the different cationic

CNCs, at different pH's (pH 6, 8 and 10). A higher degree of substitution led to a lower dose required to obtain a high

flocculation efficiency (above 80%) for pyridinium modified CNCs. This pattern was less clear for methylimidazolium

modified cellulose. At the highest obtained degree of substitution (DS surf ≈ 1), no restabilisation of the electrostatic

interaction between flocculant and algae cells was observed. Cationic cellulose nanocrystals resulted in high flocculation

efficiency, requiring a lower dose compared to alternative molecular polysaccharides (e.g. chitosan).

46

Cellulose metal sulfide based nanocomposite thin films Michael Weißl 1, @ , David Reishofer 1 , Bruno Alonso 2 , Emmanuel Belamie 3 , Heinz

Amenitsch 4 , Armin Zankel 5 , Thomas Rath 6 , Josef Innerlohinger 7 , Harald Plank 5 , Gregor

Trimmel 6 , Stefan Spirk 1, *

1 : Institute of Paper, Pulp and Fibre Technology, Graz University of Technology,

Inffeldgasse 23, 8010 Graz - Austria

2 : Institut Charles Gerhardt Montpellier

University of Montpellier

rue de l′Ecole Normale, 34296 Montpellier Cedex - France

3 : Institut Charles Gerhardt Montpellier, UMR 5253 CNRS/UM/ENSCM, ENSCM-8

University of Montpellier

rue de l′Ecole Normale, 34296 Montpellier Cedex - France

4 : Institute for Inorganic Chemistry, Graz University of Technology

Stremayrgasse 9, 8010 Graz - Austria

5 : Institute for Electron Microscopy and Nanoanalysis, Graz University of Technology and Centre for Electron Microscopy

Steyrergasse 17, 8010 Graz - Austria

6 : Institute for Chemistry and Technology of Materials, Graz University of Technology

Stremayrgasse 9, 8010 Graz - Austria

7 : Lenzing AG

Werkstraße 2, 4860 Lenzing - Austria * : Corresponding author

Cellulose, a major biopolymer on earth, exhibits interesting properties and in the past years significant efforts have been

performed to increase the value of cellulose based materials. Particularly, the use of nanoscale cellulosic materials such as

nanofibrillated and nanocrystalline cellulose as well as the introduction of concepts from polymer thin film technology offers

a wide range of opportunities to exploit cellulose in advanced applications such as optoelectronic devices, transistors and solar

cells. (1,2)

Here, we present different strategies to realize cellulose based nanocomposite thin films by spin coating having metal sulfides

as active component. Two strategies are followed, namely to create an interpenetrated network of metal sulfide nanoparticles

in a cellulose based thin film as well as to prepare sandwich type structures where the metal sulfides are deposited in between

the cellulose layers. In both cases, metal xanthates are used as precursors which are either added to the spin coating solution

or to deposit these onto the cellulose thin films by spin coating. After a heating step, the xanthates decompose accompanied

by the formation of volatile by-products and metal sulfides in or on a cellulose based thin film are formed.

In addition to state of the art characterization techniques for the films (XRD, AFM, SEM), we also studied the formation of

the metal sulfide particles using synchrotron assisted GISWAXS measurements. In the end of the presentation we show our

recent results concerning the use of such nanocomposites for the creation of conductive patterns and in optoelectronic

devices.(3,4,5)

1) Nordic Pulp & Paper Research Journal, 2015, 30, 006-013

2) Cellulose, 2015, 22, 717-727

3) ACS Sustainable Chemistry and Engineering, 2017, 5, 3115-3122

4) Carbohydrate Polymers, 2017, 164, 294-300

5) Cellulose, 2018, 25, 711-721

47

Nanocellulose from citrus peel residue: A sustainable

biorefinery approach Eduardo M. De Melo 1, @ , Avtar Matharu 1, @ , James Clark 1, @

1 : University of York [York, UK] Heslington, York, YO10 5DD - United Kingdom

A sustainable approach for the production of nanocellulose and nanocellulose-based materials using citrus peel residue as

feedstock is presented. Nanocellulose is a robust biobased material derived from lignocellulosic biomass presenting

outstanding physicochemical properties. Yet, its production has been hampered by the high costs of conventional feedstock

(wood pulp) and processing energy consumption. In this context, the aim of this work was: i., to incorporate the production of

nanocellulose in an acid-free microwave-assisted hydrothermal treatment (MAHT) of depectinated orange peel residue

(DOPR); ii., to produce and characterise nanocellulose-based hydrogels and films. Nanocellulose was produced by MAHT at

several temperatures ranging from 120 to 220 °C. Hydrogels were formulated at different concentrations (0.5 – 3 wt.%)

followed by ultrasound-assisted dispersion and films were produced by solvent-casting from 0.2 wt.% dispersions. All

materials were characterised by several techniques including CP-MAS 13C NMR, ATR-IR, TGA, CHN, N2 adsorption

porosimetry, SEM, TEM, GPC and XRD. The production of nanocellulose from DOPR was successfully in all temperatures,

with dry basis yields varying from 69 wt.% (at 120 °C) to 27 wt.% (at 220 °C). The nanocellulose material presented high

thermostability (Td ca. 360 °C), high crystallinity index (32 – 62 %) and high water holding capacity values (10 – 33 g H2O/g

sample), which are much higher than the precursor or literature-based values. The average Mw of nanocellulose ranged from

1123 to 133 KDa, where major decrease happens for nanocellulose produced above 180 °C (a drop of almost 10-fold) due to

the removal of hemicellulose and amorphous-like cellulose regions from the cellulosic matrix. Moreover, the nanocellulose

material was found to be mesoporous (pore size of 3 – 48 nm), with improved BET surface area (10 – 30 m2 g-1) when

compared to the non-porous precursor material. The hydrogels formed a strong fibre-network at 2 - 3 wt.% concentration,

presenting shear-thinning, which is an important property for rheological applications. SEM micrographs showed that the films

presented a lamellar structure with low porosity, which are important properties for photonic, and oxygen-barrier materials. In

sum, the production of nanocellulose from a cheap and widely available agroindustrial waste using a clean energy-efficient

processing was demonstrated feasible. Furthermore, as a proof-of-concept, the produced nanocellulose showed excellent

formation of hydrogels and films, with self-assembled structures, at low concentrations.

48

From structure to functionality: an initial approach

towards the application of the galactomannans extracted

from Prosopis affinis Pilar Vilaró 1, 2, @ , Eliana Budelli 3, @ , Guillermo Moyna 4, @ , Luis Panizzolo 5, @ , Fernando

Ferreira 6, @

1 : Pilar Vilaró

pilar.vilaro@cut.edu.uy - Uruguay

2 : Centro Universitario de Tacuarembó, Universidad de la República

Ruta 5 km 386,5. Tacuarembó, Uruguay, C.P. 45000. - Uruguay

3 : Departamento de Reactores, Facultad de Ingeniería, UdelaR

Herrera y Reissig 565, 11200 Montevideo - Uruguay

4 : Departamento de Química del Litoral / Centro Universitario Región Litoral Norte, UdelaR

Ruta 3 Km 363, Paysandu 60000, Uruguay - Uruguay

5 : Departamento de Ciencia y Tecnología de Alimentos, Facultad de Química, UdelaR

Avenida General Flores 2124, Montevideo, Uruguay, C.P. 11800. - Uruguay

6 : 4Laboratorio de Carbohidratos y Glicoconjugados, Departamento de Química Orgánica, Facultad de Química, UdelaR

Dr. Alfredo Navarro 3051, Montevideo C.P. 11600. - Uruguay

Galactomannans (GM) are valuable water-soluble nonionic polysaccharides, used in the food and pharmaceutical industry. In

the last years, the industry has made efforts to obtain new products that satisfy consumers interest towards natural products,

especially renewable, produced at low cost. Leguminous seeds are a well-known source of GM, used in the pharmaceutical

and food industries depending on each specific phyicochemical properties. As part of our bioprospection program for the

valorization of Uruguayan native woodlands we have isolated and characterized the galactomannan present in the seeds

of Prosopis affinis Spreng (Leguminosae, Mimosaceae).

Mature pods from P. affinis were collected from an experimental field (EEMAC, Paysandú). Galactomannans were isolated

at room temperature and 80°C from the endosperm of P. affinis pods and purified. The methylation analysis showed three

types of partially methylated alditols acetates, that in accordance to the obtained NMR spectra by 1D-TOCSY and 2D-HSQC-

TOCSY confirms a (1→4)-mannopyranosidic main chain branched every second mannose residue with a galactosyl residue

connected to the C-6 of mannose.

The molecular weight distribution was analyzed by SEC-HPLC/MALLS/IR (Wyatt Dawn 8+) on an Agilent SEC-5 column.

A Physica MCR 301 rheometer with concentric cylinder configuration and double gap geometry was used for the determination

of the intrinsic viscosity, that was calculated according to Fedors equation. Afterwards, the viscosity-average molecular weight

(Mv) was estimated from the intrinsic viscosity using the MHS equation with parameters obtained for several sources of

galactomannans by Picout and Ross-Murphy (2007). The parameters obtained both from intrinsic viscosity an SEC-HPLC

were consistent within each other, showing that the determination of Mw by diluted viscometry is still a proper methodology

for the comparison of macromolecular properties.

Finally, the rheology of the samples was studied among a semi-diluted concentration, showing a limit concentration parameter

(c*) in the range of those found by Busch et.al., 2017. The shear rates profiles were studied, showing a good fit to the

Williamson model, with parameters depending on the extraction procedure.

The structural and physicochemical characterization of the galactomannans obtained from P. affinis demonstrated that it

represents a new promising biomaterial that can be produced from the native flora in a sustainable way.

References

Busch, V., Delgado, J., Santagapita, P., Wagner, J., & Buera, M. (2017). Rheological characterization of vinal gum, a

galactomannan extracted from Prosopis ruscifolia seeds. Food Hydrocolloids, 74,333–341.

Picout, D. R., & Ross-Murphy, S. B. (2007). On the Mark-Houwink parameters for galactomannans. Carbohydrate Polymers, 70,145-148.

49

Identification and characterisation of Micro-fibrillated

cellulose (MFC) from pea fibre food waste. Jade Phillips 1, @ , Bill Macnaughtan 1, @ , Umar Zainudin 2, @ , Tim Foster 1, @

1 : The University of Nottingham

Sutton Bonington Campus, Sutton Bonington, Loughborough LE12 5RD - United Kingdom

2 : PepsiCo Beaumont Park, 4 Leycroft Rd, Leicester LE4 1ET - United Kingdom

This work will investigate the utilisation of food waste from pea plant biomass, created after harvest, for the sole purpose of

recycling it back into the food chain for direct human consumption. Different chemical and or mechanical pre-treatments were

investigated on their ability to fibrillate the Pisum Sativum, which contains a mixture of polysaccharides and biopolymers.

This work focuses on alternative methods for fibrillation compared to the usual high pressure / high-energy mechanical

methods and non-food grade chemical pre-treatments usually performed on cellulosic materials. The aim was to ascertain

which alternative method was optimal for creating Micro-fibrillated Cellulose (MFC) that can be applied to a food product, as

a functional food ingredient. In order for a material to be classed as fibrillated, the majority of the fibres within a suspension

must be classified as microfibrils or nanofibrils (Carrasco, G.C., 2012). Once modified MFC typically has similar properties

to gelling and/or thickening agents. The current problem with fibrillation is most techniques are non-food grade and the ability

to prove/classify MFC is problematic and still open to debate (Carrasco, G.C 2012). This work characterises the food grade

and non-food grade created pea plant MFC by using microscopy (TEM and SEM), sedimentation and crystallinity. Rheological

suspensions of the MFC colloidal dispersions are also measured to test whether the recycling of natural food waste through

fibrillation may be a viable option for the creation of new food structuring materials.

References

Carrasco, G.C. (2011). Cellulose fibres, nanofibrils and microfibrils: The morphological sequence of MFC components from

a plant physiology and fibre technology point of view. Nanoscale Research letters. 6(11), 417-423.

50

ROOM BORISA PODRECCE

Tailor-Made Polysaccharides with Defined Substitution

Pattern by Enzymatic Polymerization of Arabinoxylan

Oligosaccharides Deborah Senf 1, @ , Colin Ruprecht 1 , Aleksandar Matic 1 , Fabian Pfrengle 1, *, @

1 : Max Planck Institute of Colloids and Interfaces

Am Mühlenberg 1, 14476 Potsdam - Germany

* : Corresponding author

Polysaccharides from plant biomass are explored extensively as renewable resources for the production of materials and fuels.

A major component of plant cell walls is the hemicellulose xylan. Although the structure of xylans varies between plant

species, they all possess a common backbone consisting of b-1,4-linked xylopyranoses that may be decorated with different

substituents. An important subclass of xylans are arabinoxylans that carry arabinofuranosyl residues attached to the backbone

in different positions [1].The heterogeneous nature of the substitution pattern makes it difficult to correlate the molecular

structure with macroscopic properties. To study the impact of specific structural features of the polysaccharides on e.g.

crystallinity [2] or affinity to other cell wall components [3], collections of polysaccharides with defined repeating units are

required. Here, we report a chemo-enzymatic approach towards artificial arabinoxylan polysaccharides with systematically

altered branching patterns. The polysaccharides were obtained by glycosynthase-catalyzed polymerization of glycosyl

fluorides [4] derived from arabinoxylan oligosaccharides that were procured either chemically, chemo-enzymatically, or from

a commercial source. The presented strategy of combining sophisticated carbohydrate synthesis with glycosynthase technology

offers access to artificial polysaccharides for structure-property relationship studies that are not accessible by other means.

[1] A. Ebringerová, T. Heinze, Macromol. Rapid Commun. 2000, 21, 542-556. [2] Köhnke, T.; Östlund, Å.; Brelid,

H., Biomacromolecules 2011, 12, 2633-2641. [3] Bosmans, T. J.; Stépán, A. M.; Toriz, G.; Renneckar, S.; Karabulut, E.;

Wågberg, L.; Gatenholm, P., Biomacromolecules 2014, 15, 924-930. [4] Mackenzie, L. F.; Wang, Q.; Warren, R. A. J.;

Withers, S. G., J. Am. Chem. Soc. 1998, 120, 5583-5584; Ben-David, A.; Bravman, T.; Balazs, Y. S.; Czjzek, M.; Schomburg, D.; Shoham, G.; Shoham, Y., ChemBioChem 2007, 8, 2145-2151.

51

Investigations towards the Synthesis of Bismuth-sugar

conjugates Martin Thonhofer 1, *, @ , Roland Fischer 2, @ , Rupert Kargl 1, @ , Carina Sampl 2, @ , Stefan

Spirk 3, @ , Karin Stana-Kleinschek 1, @

1 : University of Maribor

Smetanova ulica 17, 2000 Maribor - Slovenia

2 : TU Graz

Stremayrgasse 9, 8010 Graz - Austria

3 : TU-Graz

Inffeldgasse 23A, 8010 Graz - Austria

* : Corresponding author

Contrast agents used in magnetic resonance imaging are commonly based on Gadolinium compounds. In search of novel and

“smart” contrast agents, several hydrophobic organobismuth compounds have become of interest. Additionally, carbohydrates

are the most widely distributed naturally occurring organic compounds on earth and due to the constant improvement in the

field of glyco-chemistry, a powerful resource in material sciences, pharmacy and medicine. Reflecting these findings, the

development and synthesis of a new compound class, namely bismuth-sugar conjugates, was deemed important. For this

purpose, three different approaches leading to various saccharides bearing covalently bonded triaryl-bismuth moieties were

investigated. In preliminary studies, several derivatives of monosaccharides were chosen as staring materials in the desired

reactions with the corresponding bismuth compounds. These researches provided a fundamental knowledge of the kinetics and

selectivity of the performed conversions. Furthermore, the efficiency of the developed “general procedure for the introduction

of bismuth ligands” had to be proven on other and larger systems. Therefore, partially protected cyclodextrines served as

suitable starting materials. Recent results in the scope and limitations of these reactions will be presented.

52

Polysaccharide Carbonates as Intermediates for Modular

Synthesis Approaches Martin Gericke 1, 2, @ , Lars Gabriel 3 , Marcus Fischer 3 , Thomas Heinze 3

1 : Friedrich Schiller Universität Jena, Institute of Organic Chemistry and Macromolecular Chemistry, Center of Excellence

for Polysaccharide Research - Website

Humboldtstraße 10, D-07743 Jena - Germany

2 : Thuringian Institute of Textile and Plastics Research e.V.

Breitscheidtstr. 97, D-07407 Rudolstadt - Germany

3 : Friedrich Schiller Universität Jena, Institute of Organic Chemistry and Macromolecular Chemistry, Center of Excellence

for Polysaccharide Research Humboldtstraße 10, D-07743 Jena - Germany

Polymer analogue chemical modification of polysaccharides (PS) provides access to functional biomaterials with tailored

physical, chemical, and biological properties. Homogeneous conversions provide high reaction efficiencies and yield PS

derivatives with well-defined molecular structures. Modular synthesis approaches are of particular interest in this regard.

Starting from a few key intermediates, it is possible to prepare a broad variety of functional compounds for different

applications with little effort.

The present work describes the synthesis of two types of activated PS derivatives; xylan phenyl carbonates (XPC) and agarose

phenyl carbonates (APC). Using different homogeneous reaction media, it was possible to achieve high degrees of substitution

(DS) up to a full functionalization of all available hydroxyl groups. Ionic liquids in combination with a co-solvent proofed to

be the most efficient reaction medium. It is also demonstrated that PS phenyl carbonates can be converted with nucleophilic

amines to yield the corresponding carbamates with high reaction efficiency and yield.

XPC proofed to be superior intermediates for the preparation of functional PS carbamates when compared to the corresponding

cellulose phenyl carbonates. They showed neither cross-linking, which is usually observed at low starting DScarbonate, nor

drastic cleavage of the activated carbonate groups, which can occur when employing high DScarbonate. Interestingly, XPC

can also self-assemble into spherical nanoparticles (NP). These reactive XPC-NP can be further functionalized, e.g., with dyes

and drugs, under aqueous conditions without previous activation. APC were converted with different ionic amines to obtain

derivatives with a tunable charge density. These derivatives were directly converted into hydrogels by a facile thermoreversible

gelation process. It was possible to tune the release of nucleotide-like drugs by variation of the type and amount of ionic moieties.

53

Efficient solvent-free preparation of amidified

carboxymethyl cellulose derivatives: study of the

structure-properties relationships Asja Pettignano 1, @ , Etienne Fleury 1 , Aurélia Charlot 1

1 : Ingénierie des Matériaux Polymères - Site INSA Lyon

Institut National des Sciences Appliquées de Lyon : UMR5223 17, Av. Jean Capelle 69621 Villeurbanne Cedex - France

In the context of sustainable development, chemical modification of polysaccharides represents a fundamental tool for biomass

valorisation, as the access to novel polysaccharide derivatives and alternative synthesis paths enables to extend the possible

applications of natural polymers. Carboxymethyl cellulose (CMC) is one of the most widely manufactured cellulose

derivatives, commonly employed in a variety of industrial applications as viscosity modifier, thickener, emulsion stabilizer,

etc (Kono, 2013). Compared to cellulose, the presence of a carboxylate function not only allows achieving a large water

solubility but also enables further functionalization, making the modification of CMC highly attractive. In this background,

the present work explores the potential offered by the inherent reactivity of CMC in order to generate new derivatives and to

design promising CMC-based materials. Amidation of CMC, at high temperature and in heterogeneous conditions, has been

selected as synthetic tool for grafting aromatic and aliphatic amines on CMC backbone. In the present protocol, the reaction is

successfully carried out in absence of solvents, catalysts and coupling agents, providing an eco-friendly and efficient

alternative to conventional amidation procedures (Montalbetti & Falque, 2005). Suitable characterizations of the obtained

amidified products allowed the investigation of their structure-properties relationships, with particular attention to their thermal

properties. The thermal behaviour of the modified polysaccharides was found to be highly dependent on the amine grafting,

highlighting the substantial effects of the substituent employed and the degrees of grafting obtained.

Kono, H., Carbohydrate polymers, 2013, 97(2), 384-390. Montalbetti, C. A., Falque, V., Tetrahedron, 2005, 61(46), 10827-10852.

54

Polysaccharide based 3D scaffolds: preparation,

characterization, and application Andreja Dobaj štiglic 1, * , Sanja Potrč 1, * , Silvo Hribernik 1, * , Matej Bračič 1, * , Manja

Kurečič 1, * , Rupert Kargl 1, 2, * , Lidija Gradišnik 3, * , Uroš Maver 3, * , Karin Stana-

Kleinschek 1, 2, * , Tamilselvan Mohan 1, 4, *, @

1 : Laboratory for Characterization and Processing of Polymers (LCPP), Faculty of Mechanical Engineering, University of

Maribor

Smetanova 17, 2000 Maribor - Slovenia

2 : Institute for Chemistry and Technology of Materials, Graz University of Technology

Stremayrgasse 9, 8010 Graz - Austria

3 : University of Maribor, Faculty of Medicine, Institute of Biomedical Sciences

Taborska ulica 8, SI-2000 Maribor - Slovenia

4 : Institute of Chemistry, University of Graz

Heinrichstraße 28, 8010 Graz, Austria - Austria * : Corresponding author

In tissue engineering, 3D scaffolds which show tunable interconnected porosity, hydrophilicity, and are made of natural

polymers are particularly of interest since they are often biocompatible and biodegradable. These scaffolds act as a template

for cellular infiltration and give physical support for mediating the growth, differentiation, and proliferation of cells which

are seeded on it. Despites their many advantages over synthetic scaffolds, poor mechanical stability limit the use of these

materials. Although this issue is addressed in several reports, only a few studies have been devoted to the development of

stable cell-supporting matrices from ionically cross-linked polysaccharides. In this talk, ionically cross-linked 3D scaffolds

from oppositely charged polysaccharides, investigation of their physicochemical and mechanical properties and their

interaction with cells will be presented.

55

Functionalization of never-dried Nanocelluloses Marco Beaumont 1, @ , Antje Potthast 2, @ , Thomas Rosenau 2, 3, *, @

1 : University of Natural Resources and Life Sciences [Vienna]

University of Natural Resources and Life Sciences, Vienna (BOKU), Department of Chemistry, Division of Chemistry of

Renewable Resources, Konrad-Lorenz-Straße 24, A-3430 Tulln - Austria

2 : University of Natural Resources and Life Sciences [Vienna]

University of Natural Resources and Life Sciences, Vienna (BOKU), Department of Chemistry, Division of Chemistry of

Renewable Resources, Konrad-Lorenz-Straße 24, A-3430 Tulln - Austria

3 : Johan Gadolin Process Chemistry Centre, Åbo Akademi University

Johan Gadolin Process Chemistry Centre, Åbo Akademi University, Porthansgatan 3, Åbo/Turku FI-20500,

Finland. - Finland * : Corresponding author

Cellulose nanofibrils feature an open-porous structure and a fibrillar nanohierarchy, and have high surface areas. In addition

to that, they are biodegradable, biocompatible, renewable and environment-friendly. In order to influence their properties and

to increase functionality by chemical means, it is mandatory to introduce new functional groups onto the cellulose surface.

However, it is a major challenge to achieve this goal without causing reactivity losses and undesired changes of the

nanostructure. Appropriate functionalization procedures have to be mild, heterogeneous and should be in agreement with the

principles of sustainable and green chemistry. In this contribution, we demonstrate functionalization strategies based on an

aqueous silanization protocol to introduce azide, thiol and vinyl groups onto the cellulose surface to act as click synthons. The

silanization protocol can be also applied to other cellulosic materials and is an elegant and sustainable avenue to a variety of

functionalized nanostructured celluloses.

56

The potential of electrochemical methods in analysis of

natural polysaccharides Slađana Strmečki Kos 1, *, @ , Marta Plavšić 1, @ , Lora Pereža 1, @

1 : Ruđer Bošković Institute

Bijenička cesta 54, 10000 Zagreb - Croatia * : Corresponding author

Natural polysaccharides (PSs) constitute a major part of organic matter present in the hydrosphere where they are involved in

the carbon cycle, speciation of trace metal ions, aggregation and sedimentation processes, etc. From electroanalytical point of

the view, PSs are electroinactive molecules that could not be oxidized nor reduced. But, recently it was reported that PSs

carrying sulfate groups such as carrageenans [1] or amino groups such as chitosan [2] produce in buffered solution well-

developed “peak Hps” using chronopotentiometric stripping (CPS) method. Peak Hps is due to the catalytic hydrogen evolution

reaction at hanging mercury drop electrode (HMDE). Concerning PS detection in seawater where they are naturally present,

peak Hps was observed only if an ex situ procedure of adsorptive transfer (AdT) is performed [3].

Here we report about detection of amino PS chitosan in seawater applying AdT procedure as direct CPS in seawater gave no

peak Hps even for 100 mg/L of chitosan. AdT included adsorption of chitosan in seawater onto the HMDE surface, transfer

of the modified HMDE into the buffer (without PS) followed by CPS detection of peak Hps. The layer of adsorbed chitosan

on the HMDE surface was very stable even 20 min after the transfer. An increase of the peak Hps height at higher buffer

concentration (0.01-0.10 M) and at lower pH (5-8) confirmed faradaic catalytic nature of the electrode process. The effect of

CPS parameters (accumulation potential, accumulation time and stripping current) as well as other experimental conditions

(type and concentration of the buffer, pH, and ionic strength) on the peak Hps height and peak potential of chitosan were

evaluated and defined. Nanomolar concentrations of chitosan in seawater was determined at moderate accumulation times

and/or stripping currents.

Accordingly, our results highlight the capacity of electrochemical CPS technique for characterisation of natural

polysaccharides carrying sulfate and/or amino groups in the structure, not only in the medium where they are naturally present

(such as seawater), but in any buffered electrolyte using HMDE that are suitable for detection of catalytic peak Hps.

References

[1] S. Strmečki, M. Plavšić, B. Ćosović, V. Ostatna, E. Paleček, Constant current chronopotentiometric stripping of sulphated

polysaccharides, Electrochem. Commun. 11 (2009) 2032-2035.

[2] E. Paleček, L. Rimankova, Chitosan catalyzes hydrogen evolution at mercury electrodes, Electrochem. Commun. 44 (2014)

59-62.

[3] S. Strmečki, M. Plavšić, Adsorptive Transfer Chronopotentiometric Stripping of Sulphated Polysaccharides, Electrochem. Commun. 18 (2012) 100-103.

57

Responsive chitosan/surfactant complexes for different

applications Leonardo Chiappisi 1, 2, *, @

1 : Technische Universität Berlin

Stranski-Laboratorium für Physikalische und Theoretische Chemie Institut für Chemie Sekretariat TC 7 Strasse des 17.Juni

124 D-10623 Berlin Germany - Germany

2 : Institut Laue-Langevin

ILL

6, rue Jules Horowitz BP 156 38042 Grenoble Cedex 9 - France * : Corresponding author

Polysaccharides constitute an important, renewable and abundant resource with unique characteristics. Their use as building

blocks allows to design eco-friendly smart materials. More importantly, the amphiphilic nature of the saccharidic units, the

large number of possible hydrogen bonds, and the stiffness of the polymeric backbone, make their self- and co-assembly with

other colloidal particles particularly interesting, opening the way for the preparation of new materials. The abovementioned

properties, for instance strongly affect the ionic co-assembly of charged polysaccharide with oppositely charged macroions

(surfactant micelles, proteins, etc).

Herein, we present the complex co-assembly behaviour of the cationic polysaccharide chitosan and weakly anionic alkyl

oligoethyleneoxide carboxylic acid (CiEjCH2COOH) micelles and vesicles. These mixtures were extensively characterized

by scattering methods (light, neutrons, and X-rays). The polymer/surfactant interactions were probed via isothermal titration

calorimetry (ITC) and densitometry.

These compounds co-assemble into very different structures, depending on the molecular architecture of the surfactant, i.e.

number of ethyleneoxide units and alkyl chain length[1-2]. The self-assembled structures are not only of a surprisingly large

variety, but strongly react to external stimuli, such as small changes in the acidity of the solution or to the application of

hydrostatic pressure. Understanding the complex interactions governing the behaviour of these systems also allowed to develop

smart-functional materials. On the one hand, the strong pH-responsiveness was exploited for the selective removal and/or

release of target molecules. On the other hand, the structures formed by spontaneous self-assembly of the components in bulk

can be transferred onto solid substrates. This approach offers an elegant and facile route for the preparation of responsive

multilayered coatings.

In summary, this work provides a comprehensive understanding of polysaccharide/surfactant co-assembly leading to

interesting applications in very different fields.

References

[1] Chiappisi, L.; Prévost, S.; Grillo, I.; Gradzielski, M. Langmuir 2014, 30 (7), 1778–1787. [2] Chiappisi, L.; Prevost, S.; Grillo, I.; Gradzielski, M. Langmuir 2014, 30 (35), 10608–10616.

58

The impact of the hemicellulose acetylation on

interactions with model cellulose surfaces: a QCM-D

study Zahraa Jaafar 1, *, @ , Alexandre Boissière 1 , Ana Villares 1, @ , Jacqueline Vigouroux 1, @ , Sophie Le

Gall 1, @ , Nadège Beury 1, @ , Céline Moreau 1, @ , Marc Lahaye 1, @ , Bernard Cathala 1, @

1 : INRA

Institut National de la Recherche Agronomique

Unité Biopolymères Interactions et Assemblages - Rue de la Géraudière – BP 71627 44316 Nantes cedex 3 - France

* : Corresponding author

Cellulose is the most abundant biopolymer on earth and the major component of plant cell wall. It occurs as semi-crystalline

microfibers embedded within a network of hemicelluloses and pectins forming the primary plant cell wall.1 Hemicelluloses

represent a group of various polysaccharides traditionally extracted by alkaline treatment from plant cell walls. These

polysaccharides are based on a β-(1-4) linked backbone of xylose or glucose and/or mannose, forming xyloglucans, xylans,

mannans and glucomannans families.1 They demonstrate large variations in composition and structure according to the

botanical origin, the tissue type and developmental stage particularly with regard to their backbones substitution.2Acetyl

esterification is ubiquitous substitution among hemicelluloses families but the role of these decorations remain poorly

understood since acetyl esters are usually lost during classical hemicelluloses alkaline extractions. Nevertheless, they can be

retained when extraction is achieved by DMSO doped by lithium chloride.3

Understanding the role of acetyl decorations on hemicelluloses interaction with cellulose and the consequence on cell wall

architecture and properties remain key questions with regard to plant development and uses. In this work, acetylated

galactoglucomannan and xylan-enriched fractions were extracted by DMSO-LiCl from apple pomace and their adsorption on

cellulose model surfaces was monitored using quartz crystal microbalance with dissipation (QCM-D) prior and after de-

acetylation. QCM-D is a highly effective mass sensing technique based on piezzolectric properties of quartz crystal. It has

been successfully used to monitor hemicellulose adsorption onto cellulose solid model surfaces since it affords information of

the mass adsorbed upon time, and therefore the kinetic behavior of the adsorption process.4 It is also an efficient method for

screening the mechanical behavior of the adsorbed layer through the dissipation factor.

The results obtained are discussed in terms of kinetic parameters of the association between hemicelluloses and cellulose,

which confirmed different adsorption regimes as a function of hemicelluloses structure and the acetylation degree. Thus, this

study provides more insight into the functional roles of the broad biological diversity of hemicelluloses in nature.

1. Scheller, H. V.; Ulvskov, P., Hemicelluloses. In Annual Review of Plant Biology, Vol 61, Merchant, S.; Briggs, W. R.; Ort,

D., Eds. 2010; Vol. 61, pp 263-289.

2. Melton, L. D.; Smith, B. G.; Ibrahim, R.; Schröder, R., Mannans in primary and secondary plant cell walls.New Zealand J.

Forestry Sci. 2009, 39, 153-160.

3. Quemener, B.; Vigouroux, J.; Rathahao, E.; Tabet, J. C.; Dimitrijevic, A.; Lahaye, M., Negative electrospray ionization

mass spectrometry: a method for sequencing and determining linkage position in oligosaccharides from branched

hemicelluloses. Journal of Mass Spectrometry 2015, 50 (1), 247-264.

4. Villares, A.; Moreau, C.; Dammak, A.; Capron, I.; Cathala, B., Kinetic aspects of the adsorption of xyloglucan onto cellulose nanocrystals. Soft Matter 2015, 11 (32), 6472-6481.

59

Formation of Ethyl Cellulose Particles: Influence of

Different Surface Active Polysaccharide Derivates and

Particle Formation Methods Doris Tkaučič 1, @ , Mojca Božič 1, *, @ , Rupert Kargl 1, @ , Thomas Elschner 2, @ , Silvo

Hribernik 1, @ , Karin Stana-Kleinschek 1, @ , Matej Bračič 1, @

1 : Laboratory for Characterization and Processing of Polymers (LCCP), Faculty of Mechanical Engineering, University of

Maribor

Smetanova 17, 2000 Maribor - Slovenia

2 : Papiertechnische Stiftung

Pirnaer Straße 37, 01809 Heidenau - Germany * : Corresponding author

In this work we focus on understanding the influence of different surface active polysaccharide derivates and particle formation

methods on the systematic production of the ethyl cellulose (EC) particles. In particular, the role of one ionic - carboxymethyl

cellulose (CMC), one nonionic - hydroxyethyl cellulose (HEC) a high and a low molecular weight methyl cellulose (MC-

HMw and MC-LMw) on EC particle formation was investigated. We have established how individual surface active

polysaccharides with varying concentration from 0.1 to 3.0 wt.% affect particle size and its distribution, particle shape, surface

charge, and particle morphology. The interdependencies between surfactant nature and concentration at constant processing

parameters and the subsequent nano- to micro-particle characteristics are discussed. It was determined that the particle size,

morphology, supramolecular structure and surface properties of EC particles can be effectivelycontrolled by the type and

concentration of used polysaccharide surfactant yielding spherical particles sizes from 170 nm to the micrometer level with

smooth surfaces or remarkably a wrinkled surface morphology or “particle on particle” structures. However, significant

differences of the particle phisicochemical properties can observed by varying the particle formation methods. The dialysis

method produced less uniform particles of small diameters with a rather low yield, while the solvent evaporation method produces more uniform particles of larger diameters with a high process yield.

60

Investigation of the decomposition process of cellulose

during oxidation with ammonium persulfate Inese Filipova 1, *, @

1 : Latvian State Institute of Wood Chemistry

Dzerbenes Street 27, Riga, Latvia, LV-1006 - Latvia * : Corresponding author

Keywords: ammonium persulfate, oxidation, cellulose, nanocellulose

Cellulose is one of the most abundant biomass-based polysaccharide, available in large quantities all over the world.

Nanocellulose is extremely promising product of cellulose and is obtained in chemical and/or mechanical deconstruction

process. Chemical treatment with ammonium persulfate (APS) of cellulose is used as an alternative to sulphuric acid hydrolysis

of cellulose (Rozenberga et al. 2016; Leung et al. 2011); however less attention is devoted to detailed investigation of the

decomposition process. The aim of presented research was to investigate the effect of APS oxidation on the structural and

chemical changes of cellulose.

Bleached birch Kraft cellulose was heated at 70°C for 4 hours with APS water solution with continuously stirring. APS to

cellulose mass ratio was changed in range from 1:1 to 1:10. After reaction obtained oxidised cellulose was washed to pH

neutral with water, the excess of water was drained and material was frieze dried. The reaction yield and length of fibres was

determined using gravimetric calculations and Fiber tester, respectively. Microscopy and scanning electron microscopy (SEM)

was used to visualise the deconstruction of cellulose. The degree of polymerisation (DP) was determined using Rheotek RPV-

1.

The yield of oxidised cellulose during APS oxidation reaction decreased from 98 % to 43 % with increasing APS to cellulose

mass ratio. Average length of fibres decreased from 0.9 mm to 0.3 mm with increasing APS to cellulose ratio. The decrease

of DP and microscopy results confirmed that the gradual decomposition of cellulose in smaller pieces by APS occurred. It was

concluded that the level of decomposition was significantly dependant on APS to cellulose ratio.

The obtained results can be used to predict optimal conditions of APS pretreatment before further mechanical disintegration

of cellulose in order to obtain nanocellulose.

Acknowledgement

The work has been financed by the Post-doctoral Research Aid Project No.1.1.1.2/VIAA/1/16/211 (1.1.1.2/16/I/001) “Study

of novel method for nanocellulose isolation from biomass and its residues”.

References

Leung A., Hrapovich S., Lam E. 2011. Characteristics and properties of carboxylated cellulose nanocrystals prepared from

novel one-step procedure. Small. 7, 302-305.

Rozenberga L., Vikele L., Vecbiskena L., Sable I., Laka M., Grinfelds U. 2016. Preparation of nanocellulose using ammonium persulfate and method's comparison with other techniques. Key Engineering Materials. 674, 21-25.

61

RELATIONSHIP BETWEEN DEGREE OF

SUBSTITUTION AND VISCOSITY OF CATIONIC

STARCH Denys Zalyvchyi 1, 2, *, @ , Iryna Marchenko-Sorochak 2, @

1 : Taras Shevchenko National University of Kyiv

64/13, Volodymyrska Street, Kyiv, Ukraine, 01601 - Ukraine

2 : Interstarch-Ukraine, LLC

29a, Elektrykiv Street, Kyiv, Ukraine, 04176 - Ukraine * : Corresponding author

Starch is a carbohydrate produced by green plants like corn, potatoes, wheat, cassava. To give the starch specific properties,

including high viscosity, emulsifying capacity, freeze/thaw stability, stability at low pH etc., native starch is modified

chemically, physically or enzymatically. Modified starches found application both in food and non-food industry.

Cationic starches are usually prepared in alkaline environment with cationic nitrogenous reagent, which carries amine groups.

Cationic starches are widely used in paper industry as wet and additives.

The degree of substitution (DS) is the determining parameter for cationic starches performance. DS is usually estimated using

Kjeldahl method, which is rather long and time consuming.

The aim of these research is to develop express lab method of cationic starches evaluation by conventional lab methods of

starch properties measurements, such as viscosity. Since the cationization influences the starch properties greatly, there can be

a correlation between DS and the viscosity of cationic starches. We investigated waxy corn cationic starches with DS of up to 0.05 and carried out a correlation between the previously specified parameters.

62

Coupling of alginate isolation with alternative method for

polyphenol extraction from brown seaweed Laminaria

Hyperborea Miša Mojca Cajnko 1, *, @ , Uroš Novak 1 , Blaž Likozar 1

1 : National Institute of Chemistry, Department of Catalysis and Chemical Reaction Engineering

Hajdrihova 19, 1000 Ljubljana - Slovenia * : Corresponding author

Macroalgae are an abundant and potentially renewable resource that is currently being investigated as a novel and sustainable

biomass based source of compounds for medical, cosmetic and nutritional applications. The cell walls of brown seaweed

contain mostly cellulose, alginates, sulfated fucans and proteins. Alginates are a dominant structural polysaccharide found in

the cellular wall matrix of brown seaweed (Phaeophyceae) and are composed of β-(1→4)-D-mannuronic and α-L-guluronic

acid blocks in heterogeneous proportions. The industrial applications of alginate are numerous. It is widely used as a thickener

and stabilizing agent in ice cream, emulsifier, mayonnaise, for whey separation in milk industries, microencapsulating agent

in medical science and as microsphere vector for drug delivery. One of the problems that arise in the process of alginate

isolation is the toxicity of formalin which is used for removal of polyphenols. In our current work we used stipes and leaves

from brown seaweed Laminaria hyperboreaand compared alginate extraction with formalin (yield and purity) to three different

alternative solvents, ethanol, methanol and acetone. We used either pure solvent or 50/50 solvent/water solutions. We also

tested these alternative solvents for their ability for polyphenol removal by determining the dry weight of the extract and by

measuring the total polyphenol content. Based on yield and purity measurements, the alternative solvents used in this study

showed great potential as suitable alternative in the alginate isolation process. Also, these solvents were very effective in

extracting polyphenols which can potentially be used as antioxidants in cosmetic and food industry.

63

Does mannan interact with arabinogalactan proteins and

impact wheat endosperm development? Yves Verhertbruggen 1, @ , Axelle Bouder 2 , Marlayna Sterner 2 , Xavier Falourd 2 , Camille

Alvarado 2 , Mark Wilkinson 3 , Sylviane Daniel 2 , Sophie Le-Gall 2 , Rowan Mitchell 3 , Loic

Foucat 2 , Fabienne Guillon 2 , Anne-Laure Chateigner-Boutin 2 , Luc Saulnier 2

1 : INRA

INRA (French Institute for Agricultural Research) : UR1268

BIA, rue de la Géraudière, 44300 Nantes - France

2 : INRA

Institut national de la recherche agronomique (INRA) : UR1268

BIA, rue de la Géraudière, 44300 Nantes - France

3 : Rothamsted Research West Common, Harpenden AL5 2JQ - United Kingdom

In wheat endosperm, the two major cell wall polysaccharides, arabinoxylans and b-glucans, have been extensively studied. By

contrast, mannan, the third most abundant polysaccharide, is still poorly documented. Nevertheless, this hemicellulosic

polysaccharide might have a determinant role in wheat grain development since, in Arabidopsis thaliana, mutants with a

reduced amount of mannan show an altered seed development. Our project aims to decipher the biochemical structure and the

biological function of mannan in wheat endosperm. We have extracted this polysaccharide to determine its fine structure.

Former studies have speculated that the class of mannan present in wheat endosperm was glucomannan. However, our data

suggest that, in mature wheat endosperm, this class of hemicelluloses is only represented by short unsubstituted chains of 1,4

linked D-mannose residues. Co-precipitations and co-elutions of mannan with arabinogalactan-proteins (AGPs) suggest the

two cell wall components might interact together in the cell walls of wheat endosperm. To confirm this, we are examining the

possible presence of linkages in between mannan and AGPs. To study the biological function of mannan, we have studied its

occurrence during wheat grain development. The detection of mannan using monoclonal antibodies show that the deposition

of this hemicellulosic polysaccharide starts at an intermediate step of endosperm cellularization. Mutant lines targeting genes

involved in the mannan synthesis are being generated to further investigate the biological function of mannan. Our current

results raise questions regarding the structure of mannan in wheat endosperm, its possible interactions with other cell wall

components and its contribution to cell wall formation.

64

Kraft lignin as a modifier and binder: Esterification of

lignin Matej Bračič 1, @ , Mojca Božič 1, 2, @ , Manja Kurečič 1, 2, 3, @ , Silvo Hribernik 1, @ , Karin Stana-

Kleinschek 2, 4, 5, @

1 : Laboratory for Characterization and Processing of Polymers (LCCP), Faculty of Mechanical Engineering, University of

Maribor

Smetanova 17, 2000 Maribor - Slovenia

2 : Institute of automation, Faculty of Electrical Engineering and Computer Science, University of Maribor

Koroška cesta 46, 2000 Maribor, Slovenia - Slovenia

3 : Graz University of Technology

Stremayrgasse 9, 8010, Graz - Austria

4 : Laboratory for Characterization and Processing of Polymers (LCPP), Faculty of Mechanical Engineering, University of

Maribor

Smetanova ulica 17, 2000 Maribor, Slovenia - Slovenia

5 : Institute for Chemistry and Technology of Materials (ICTM), Graz University of Technology Stremayrgasse 9, 8010 Graz, Austria - Austria

The annual world wood harvest exceeds 3 billion cubic meters and the wood is used in a variety of different branches form

construction, paper industry, energy supply, and many more. All this processes produce tons of waste wood biomass which is

mostly used as an energy supply or lands in landfills. In the paper industry, lignin is such a biomass waste which so far hasn't

been utilised to its full potential. If used, the waste lignin mostly serves as an alternative energy supply to fossil fuels, but

lignin offers interesting physicochemical properties which make it useful far beyond energy supply. It has shown potential to

be used as a modifier or binder in asphalt, a marine antifouling coating or a protection coating for metals to name a few. It is

sometimes necessary to alter the chemical properties of lignin if one wants to mix it with other materials and use it as a

modifier. Esterification reactions are commonly performed on lignin to alter its chemical structure, as it contains lots of

phenolic hydroxyl groups. In this work, a commercially available alkali lignin and a kraft process lignin liquid were esterified

with a hydrophobic substance commonly used in the paper industry to make paper hydrophobic. A simple and cost effective

approach was designed to make the lignin soluble in organic solvents and compatible with hydrophobic materials. The lignin

was ultrafiltrated prior to esterification and the filtrated fractions were characterised with high-performance liquid

chromatography, and pH potentiometric titrations. The esterified products were characterised by means of infrared

spectroscopy, gas chromatography, contact angle and pH potentiometric titrations.

The authors would like to acknowledge the financial support received in the frame of Slovenian smart specialization program (CELLCYCLE - http://celkrog.si/?lang=en, grant number C3330-16-529004).

65

POSTER PRESENTATIONS

ROOM ANTONA TRSTENJAKA

Fractionation and structural analysis of polysaccharides

from Chlorella vulgaris G11 biomass Leonid Sushytskyi 1, *, @ , Jana Copikova 1, @ , Peter Capek 2 , Roman Bleha 1, @ , Andrej Sinica 1, @

1 : University of Chemistry and Technology Prague

Technická 5166 28 Prague 6 – Dejvice - Czech Republic

2 : Institute of Chemistry, Centre for Glycomics, Slovak Academy of Sciences

Dúbravská cesta 9, 845 38 Bratislava - Slovakia * : Corresponding author

During last decades biomass from microalga Chlorella vulgaris obtained numerous practical applications and still induces

interest among scientific and industrial communities as the source of proteins and polysaccharides with biological activities,

food supplement and biofuels. Partially, some algal polysaccharides demonstrated antiviral, immunomodulatory, anticoagulant

and cosmetic effects, and also numerous effects as part of common food. Aqueous extracts from microalgal biomass, which

are rich in proteins and polysaccharides, are interesting in testing on living models. A lutein rich chlorophyll deficient

mutant Chlorella vulgaris G11 was cultivated in heterotrophic conditions and referred medium. Both heterotrophic incubation

and modified protein synthesis may influence composition and structure of cell wall polysaccharides.

This study was aimed on fractionation and further structural study of polysaccharides represented in water extracts of Chlorella

vulgaris G11 biomass. Preparative chromatography with tempered column filled with Biogel P-100 gel (Bio-rad) was used to

establish molecular weight distribution of the biopolymer components in aqueous extracts obtained at different temperatures

(20, 60 and 100°C). Obtained fractions were lyophilized and characterised by FTIR and FT Raman

spectroscopy. Monosaccharide composition and linkage sugar analyses were established by GC chromatography coupled with

FID and MS detection, respectively. It was found, that boiling water extracts has high amount of carbohydrates compared to

proteins. By contrast, extractions at lower temperatures led to fractions having significant amounts of proteins. Further removal

of proteins yielded purified polysaccharides. Rhamnose, galactose, and xylose were the main monosaccharide units, while

glucose, fucose, arabinose, and mannose were found in smaller amounts. According to NMR analysis, this fraction could be a

mixture of several polysaccharides including galactofuranan and xylorhamnan. Preparative size exclusion

chromatography showed at least two polysaccharide sub-fractions, which were lyophilized and characterised by spectroscopic

and chromatographic methods.

This work was supported by specific university research (MŠMT No 20-SVV/2017) and by the Slovak Grant Agency VEGA

(grant no. 2/0051/18).

P1

Redesign of collagen sausage casings for high quality

performance using food grade polysaccharides Motolani Sobanwa 1, @ , Tim Foster 2, @ , Nicholas Watson 3, @ , Gordon Paul 4, @

1 : Motolani

Division of Food Science, School of Biosciences, The University of Nottingham, Sutton Bonington Campus, Loughborough,

LE12 5RD - United Kingdom

2 : Tim Foster

Division of Food Science, School of Biosciences, The University of Nottingham, Sutton Bonington Campus, Loughborough,

LE12 5RD - United Kingdom

3 : Nicholas Watson

Department of Chemical and Environmental Engineering, The University of Nottingham, University Park Campus, NG7

5RD - United Kingdom

4 : Gordon Paul Devro Plc, Moodiesburn, Chryston, Scotland, G69 0JE - United Kingdom

There is a growing interest in the application of collagen casings as an alternative to casings made from animal intestines for

processed meat products such as sausages. Currently, collagen type 1 extracted from the hide of cattles is reconstituted into a

paste and formed into a casing through an extrusion process1. Collagen casings have different properties to casings made from

animal intestines hence there is a need to investigate how collagen casings can be adapted to provide new properties, beyond

that of casings made from animal intestines. One potential approach which can be used to modify the properties of collagen

casings is to incorporate natural biopolymers such as polysaccharides which acts as fillers. The aim of this work is to investigate

how polysaccharides can impact the structure and functionality of collagen paste for the development of collagen casings with

new and desirable properties. Cellulose suspensions with different aspect ratios were added to collagen paste in order to

evaluate the effects this has on the thermal and rheological properties of the collagen paste. The viscoelastic properties of the

different pastes were characterised using a controlled stress rotational rheometer equipped with a parallel-plate geometry while

the denaturation temperature of the pastes was estimated using the Differential Scanning Calorimetry. Our results revealed

that the addition of cellulose fibers as fillers has significant effects on the rheological properties of the collagen paste. Also,

the viscoelastic properties of the collagen paste was not dependent on the cellulose aspect ratios when added at the same

dispersed phase volumes. DSC thermograms showed that the addition of the cellulose fibers had no effect on the denaturation

temperature of the collagen paste. In conclusion, our results suggest that by using polysaccharides, the rheological properties of collagen pastes can be modified to create collagen casings with improved properties.

P2

Chitin as a renewable source for the production of smart

food packaging materials Bojana Bradic 1, @ , Marijan Bajic 1, *, @ , Uroš Novak 1, @ , Blaz Likozar 1, @

1 : National institute of Chemistry

Hajdrihova 19,1000 Ljubljana - Slovenia * : Corresponding author

Chitin is considered as one of the most plentiful organic resource on the Earth, present in various organisms such as marine

invertebrates, insects, fungi and yeast.[1] This biopolymer is composed of N-acetyl glucosamine and its deacetylation gives

chitosan, which is composed from N-acetyl glucosamine and glucosamine units. Chitosan shows a better aqueous solubility

compared to chitin, and consequently broader application in many areas .[2] Due to it, as well as its renewability,

sustainability, and biodegradability, chitosan has been attracting a growing interest in the development of biopolymers over

the past few years.[3]

This study deals with the whole process, from the isolation of shrimp chitin to its utilisation for the preparation of chitosan-

based films as smart food packaging materials. After isolation of chitin using a deep eutectic solvent that consists of different

combinations of salts under unequal reaction conditions, it was deacetylated using sodium hydroxide solutions at elevated

temperatures and time in order to obtain chitosan with a high deacetylation degree. Afterwards, chitosan-based films were

prepared by casting method from previously isolated and deacetylated chitin and further evaluated regarding their functional

properties as potential food packaging material. The samples were characterized by several techniques, such as FTIR

spectroscopy, Scanning electron microscope (SEM) and Energy dispersive spectroscopy (EDS).

Keywords: Chitin, Chitosan, Extraction, Biofilms, Antioxidants

References:

[1] David L Kaplan , Biopolymers from Renewable Resources, 1998.

[2] Islem Younes , Marguerite Rinaudo, David Harding and Hitoshi Sashiwa, Chitin and Chitosan Preparation from Marine

Sources. Structure, Properties and Applications, Marine Drugs, 2015, 13, 1133-1174.

[3] Maher Kammon, Manel Haddar, Tasnim Kossentini Kallel, Mohamed Dammak, Adel Saya, Biological properties and

biodegradation studies of chitosan biofilms plasticized with PEG and glycerol, International Journal of biological

Macromolecules , 2013, 62 , 433-438.

P3

Gelatin/PAN as a polymer blend for electrospinning Daria Wehlage 1, *, @ , Robin Böttjer 1 , Timo Grothe 1, *, @ , Andrea Ehrmann 1, *, @

1 : Bielefeld University of Applied Sciences

Interaktion 1, 33619 Bielefeld - Germany * : Corresponding author

Due to their large inner surface, nanofiber mats are often used in tissue engineering and biotechnology. Especially gelatin is

an interesting biopolymer for electrospinning, because of the high availability and usability, e.g. as substrate for adherent cell

growth. But electrospinning gelatin without a spinning agent is difficult due its low molecular weight.

This series of experiments focused on co-spinning gelatin with polyacrylonitrile (PAN) as spinning agent to investigate the

morphology of the produced nanofiber mats with different gelatin and PAN concentrations. In addition, the mats were watered

to study the stability of the gelatin part in the nanofiber mats and were optically examined before and after soaking. This poster depicts the influence of the gelatin content on nanofiber diameters and the solubility of the nanofiber mat in water.

P4

Influence of xylan on ions of 1-ethyl-3-

methylimidazolium acetate solution Wafa Ezzawam 1, @

1 : University of Leeds Woodhouse Lane, Leeds LS2 9JT - United Kingdom

Cellulose and xylan are the world's most abundant naturally occurring biopolymers, found in plants; and these carbohydrates

are potentially an unlimited resource to lessen our dependence on fossil fuels. This work uses ionic liquids, designer green

solvents, to dissolve and therefore process cellulose with. We are looking at the interactions between plant polymers, here

xylan with cellulose, with the aim to form novel materials. Solutions of cellulose and xylan in the ionic liquid 1-ethyl-3-

methylimidazolium acetate [C2mim] [OAc] were examined using NMR spectroscopy, diffusion, relaxation and viscosity at

various temperatures (20 °C - 60 °C). We observed that the dissolution of xylan in [C2mim] [OAc] is similar to that for

cellulose, though cellulose preferentially reduces the diffusion coefficient of the anion more than that of xylan. The dissolution

mechanism of cellulose and xylan in [C2mim] [OAc] can be examined via the mobility of the ions. We proposed that the

number of accessible OH groups belonging to the carbohydrates is reduced at certain xylan-cellulose blend compositions,

showing that at these concentrations there are significant interactions between the two biopolymers. The data of intrinsic viscosity [η] of xylan / [C2mim] [OAc] solutions were determined and from this a viscosity master curve was produced.

P5

MATUROLIFE - Metallisation of Textiles to make

Urban living for Older people more Independent and

Fashionable Alenka Ojstršek 1, @

1 : University of Maribor, Faculty of Mechanical Engineering, Institute of Engineering Materials and Design

Smetanova 17, 2000 Maribor - Slovenia

The overall objective of MATUROLIFE project is to adopt and inter-disciplinary and co-creation approach combining material

science, electronics/sensors, social science, creative and artistic design for development of 3 Assistive Technology (AT)

prototypes (clothing, furniture and footwear) that will make urban living for older people easier, more independent, fashionable

and comfortable.

The population of older people in Europe is increasing, and a key European societal challenge is to ensure that older people

live independently and secure as long as possible. This can be provided by AT as proposed in a project, e.g. discreet

incorporation of sensors to alert for movements, vital signs and dehydration, wearing alarms and tracking devices around the

arm or neck to alert carers to falls or their location if they wander, etc. Despite availability of AT, there are significant issues

in terms of user and acceptance. AT development often doesn't involve the end-user in the design process resulting in

dissatisfaction and abandonment rates as high as 75% (e.g. due to aesthetics and unattractive appearance). Thus, the project

will integrate creative artists and fashion designers into the research team to facilitate design-driven innovation. This will

ensure high uptake and retention of AT, create a strong market for the products and lead to a high social and economic impact

across Europe particular for the large number of SMEs involved in this consortium.

The project will build on existing technological advances in materials which have produced a highly innovative selective

metallisation process that utilises nanotechnology, electrochemistry and materials science to encapsulate fibres in textiles with

metal and thereby provide conductivity and electronic connectivity. In this way, better integration of electronics and sensors

into fabrics and textiles will be possible. This will give the fashion designers and artists the tools to produce AT for older

people that is not only functional but is more desirable and appealing as well as being lighter and more comfortable.

This ambitious project started in January 2018 under coordination of Coventry University, United Kingdom (dr. Andrew

Cobley). MATUROLIFE brings together 20 partners from 9 countries: 11 SMEs, RTDs, NGOs and academics in a 6 million

EUR, 36 month project. University of Maribor, as a WP5 leader, is responsible for activities pertaining to passivation of

conductive tracks, which main aim is to ensure the protection of metallised textiles against external factors (e.g. sweat, water).

More: http://maturolife.eu/

“This project has received funding from the European Union's Horizon 2020 research and innovation program under grant agreement No 760789”.

P6

Oil encapsulation in core-shell alginate capsules using

droplets based millifluidic Mariana Pereda 1, 2, *, @ , Joelle Davy 1 , Denis Poncelet 3 , Denis Renard 1

1 : INRA UR 1268 Biopolymères Interactions Assemblages

Institut National de la Recherche Agronomique

F-44300 Nantes - France

2 : INTEMA- Consejo Nacional de Investigaciones Científicas y Técnicas

Avda. Rivadavia 1917 - CP C1033AAJ - Cdad. de Buenos Aires - Argentina

3 : ONIRIS

Process Engineering for Environment and Food laboratory, ONIRIS

F-44322 Nantes - France * : Corresponding author

Oils are widely applied in the formulation of foods, pharmaceutical and cosmetic products; however, they are often volatile,

labile and sensitive to environmental factors such as heat, light, water and oxygen [1]. An efficient strategy to decrease their

sensitivity towards environmental conditions consists of its encapsulation in inert polymer matrix (alginate) using

gelation/emulsification technique [2-4]. Specifically, the inverse gelation approach consists in adding drops of calcium

chloride/oil emulsions into an alginate bath [5-7], leading to core-shell capsules with a high oil loading. Based on previous

results of our group [8], the droplets millifluidic device, where a dispersed phase is introduced through a capillary or needle

into the co-flowing continuous phase, allows the easy production of highly controlled and uniform microcapsules from W/O

emulsions. The objective of the present work is, therefore, to take advantages of the new droplets millifluidic/inverse gelation

based process to produce core-shell alginate milli-capsules and to analyze the effect of varying the gelation time on the final

properties of the obtained capsules. Alginate was selected as the microcapsules shell given the non-toxic biocompatible and

biodegradable properties of the gel easily formed once it reacts with divalent cations like Ca2+. It was first found as expected

that alginate membrane thickness increased with gelation time in the collecting bath. Surprisingly, it was found that alginate

membrane thickness was inversely related to its mechanical properties, i.e. the thicker membrane, the lower surface Young

modulus. Surface Young's modulus ranged from 61 to 26 N/m at gelation times of 3 and 45 minutes respectively. Oil loading

was quite high with 80wt% for dry capsules whatever the conditions used.

P7

Using phenolics from potato peels for the production of

active starch-based films Joana Lopes 1, @ , Idalina Gonçalves 1, 2, @ , Cláudia Nunes 1, 2, @ , Paula Ferreira 1, @ , Manuel A.

Coimbra 2, @

1 : CICECO - Aveiro Institute of Materials, Department of Materials and Ceramic Engineering, University of Aveiro

Campus Universitário de Santiago 3810-193, Aveiro, Portugal - Portugal

2 : QOPNA, Department of Chemistry, University of Aveiro Campus Universitário de Santiago 3810-193 Aveiro, Portugal - Portugal

The development of active biobased packaging materials is of major concern to food industry. Herein, starch, an abundant

polysaccharide in nature, accomplish all the main features, making it a promising raw material for edible coatings/films [1,2].

However, starch leads to quite brittle and hydrophilic materials [3] without active properties and, therefore many efforts have

been carried out to fulfill these features [4,5]. In this work phenolic compounds were recovered from potato peels and combined

with starch aiming to produce films with antioxidant capacity.

The starch size distribution, granular surface and calorimetry were determined. In addition, the total phenolic content and the

antioxidant profile (ABTS method) of the recovered phenolic extract (by Soxhlet extraction with ethanol) were measured. The

influence of phenolic extract concentration (0.1%, 0.5% and 1% w/w related to starch weight) on color, wettability, water

solubility, mechanical and antioxidant properties of starch films was evaluated.

The starch presented oval granules with medium size of 43 µm and ability to form transparent and colorless films, showing a

gelatinization temperature around 60 ºC. By adding the phenolic extract, a yellowish coloration is conferred to starch films.

Moreover, an improved of the starch films surfaces hydrophobicity and a slightly decrease of their water solubility were

observed. Phenolic extract also promoted a plasticizing effect on starch films as observed by the decrease of tensile strength

and Young's modulus and the increase of elongation properties. As expected, combining phenolics with starch formulations

led to films with higher antioxidant capacity, being this effect more pronounced for 1% of phenolic extract (more 50% than

pristine starch film, after 48 h). These results revealed that potato industry byproducts possess compounds with potential for

the development of active starch-based materials with improved surface, mechanical and antioxidant performance, opening

applications on the food packaging field.

P8

Development and characterization of novel electrospun

matrices with embedded CNC for air filtration Manja Kurečič 1, 2, 3, @ , Tanja Pivec 4, @ , Mojca Božič 2, 3, @ , Silvo Hribernik 2, 3, @ , Karin Stana-

Kleinschek 1,2, 4, @

1 : Institute for Chemistry and Technology of Materials (ICTM), Graz University of Technology

Stremayrgasse 9, 8010 Graz, Austria - Austria

2 : Institute of Automation, Faculty of Electrical Engineering and Computer Science, University of Maribor

Koroška cesta 46, 2000 Maribor, Slovenia - Slovenia

3 : Laboratory for Characterization and Processing of Polymers (LCCP), Faculty of Mechanical Engineering, University of

Maribor Smetanova 17, 2000 Maribor - Slovenia

4 : Laboratory for Characterization and Processing of Polymers (LCPP), Faculty of Mechanical Engineering, University of

Maribor Smetanova ulica 17, 2000 Maribor, Slovenia - Slovenia

Solid particles represents nowadays one of the largest risks for human health and state of the environment. Therefore, an urgent

need for development of bio-based filtering materials was induced. Removal and immobilization of increasingly small particles

is currently the major concern of the filtering sector, due to requirement of novel material with small pore size and enhanced

surface area.

Presented research work is a part of a national research and development program Cel.Cycle (http://celkrog.si/?lang=en),

aiming at constructing materials with a hierarchical porous structure and increased active surface by using novel technologies

(e.g. electrospinning). For preparation of composite materials with improved filtration properties cellulose derivative (e.g.

cellulose acetate) combined with embedded active component (cellulose nanocrystals – CNC) were used. Developed

composite CA/CNC nanofibrous material shows improved filtration efficiency by 90% compared to pure CA nanofibrous mat.

Acknowledgement:

Slovenian smart specialization program (CELLCYCLE, grant number C3330-16-529004) Slovenian Research Agency

(Program Group: Textile chemistry (P2-0118))

P9

A comparative study of sample preparation for staining

and immunodetection of plant cell walls by light

microscopy Yves Verhertbruggen 1, 2, 3, @ , Jesse Lee Walker 2, 4 , Fabienne Guillon 5 , Henrik Vibe Scheller 2, 3, 4

1 : INRA

INRA (French Institute for Agricultural Research) :UR1268 BIA, rue de la Géraudière, 44300 Nantes - France

2 : Joint BioEnergy Institute

Lawrence Berkeley National Laboratory, Emeryville, CA - United States

3 : Environmental Genomics and Systems Biology Division

Lawrence Berkeley National Laboratory, Berkeley, CA - United States

4 : University of California

Berkeley, CA - United States

5 : INRA Institut national de la recherche agronomique (INRA) : UR1268

BIA, rue de la Géraudière, 44300 Nantes - France

Staining and immunodetection by light microscopy are methods widely used to investigate plant cell walls. The two techniques

have been crucial to study the cell wall architecture in planta, its deconstruction by chemicals or cell wall-degrading enzymes.

They have been instrumental in detecting the presence of cell types, in deciphering plant cell wall evolution and in

characterizing plant mutants and transformants. The success of immunolabeling relies on how plant materials are embedded

and sectioned. Agarose coating, wax and resin embedding are, respectively, associated with vibratome, microtome and

ultramicrotome sectioning. Here, we have systematically carried out a comparative analysis of these three methods of sample

preparation when they are applied for cell wall staining and cell wall immunomicroscopy. In order to help the plant community

in understanding and selecting adequate methods of embedding and sectioning for cell wall immunodetection, we present here the advantages and limitations of these three methods.

P10

A comprehensive approach to the analysis of

anhydrosaccharides in wood pyrolysis products Kristine Meile 1, @ , Aivars Zhurinsh 1, @ , Nadezda Iljina 1, @

1 : Latvian State Institute of Wood Chemistry 27 Dzerbenes, Riga, LV-1006 - Latvia

Pyrolysis is a practical thermochemical destruction process which can be applied to various biomass feedstock, requiring

relatively low capital investment and it is easy to scale-up [1]. Pyrolysis of wood – lignocellulosic biomass – produces char,

gasses and condensable or liquid products. These pyrolysis liquids contain hundreds of individual compounds, among which

anhydrosaccharides are one of the most interesting group. Anhydrosaccharides are the products of the pyrolysis of cellulose,

but despite the fact that cellulose is a very ‘'simple'' polymer consisting of the same β(1→4) linked D-glucose units, several

different anhydrosaccharides (isomers and oligomers) can be obtained by its pyrolysis [2,3]. The challenges in analysing these

anhydrosaccharides arise from 1) unavailability of commercial standards; 2) structural similarities of isomers, for example,

1,6-anhydro-β-D-glucofuranose, 1,6-anhydro-β-D-glucopyranose, 1,6-anhydro-β-D-galactopyranose all are C6H10O5

anhydrosaccharides. In our work we used not only preparative column chromatography with chemical analysis, but also size

exclusion chromatography and ultra-high performance chromatography with mass spectrometry to characterise the

anhydrosaccharides obtained by birch wood pyrolysis. Among the identified compounds were levoglucosan, cellobiosan and

1,6-anhydro-β-D-glucofuranose.

The study was supported by the National Research Programme “Forest and earth entrails resources: research and sustainable

utilization – new products and technologies” (ResProd) Project Nr.3 “Biomaterials and products from forest resources with versatile applicability''.

P11

Fungal biomass polysaccharides: extraction of side

stream from enzyme production Ida Nikkilä 1, *, @ , Maija Tenkanen 1, @ , Kirsi Mikkonen 1, @

1 : Department of Food and Nutrion, University of Helsinki, Finland

P.O. Box 66, FI-000014 Helsinki - Finland * : Corresponding author

The need to replace fossil resources and advance sustainability in today's industry has increased biopolymer research.

Polysaccharides form a large group of biopolymers with diverse chemical structures and functional properties. Polysaccharides

are non-toxic, biodegradable, and renewable materials that are widely utilized e.g., in the fields of food and materials science.

Research is mainly focusing in plant-based polysaccharides, but new renewable sources for biopolymers such as

polysaccharides are actively sought.

Enzyme industry is broadly using fungi to produce enzymes, and fungal cell biomass is produced as side stream. The fungal

cell wall is composed of polysaccharides, glycoproteins, and phospholipids, where the polysaccharides consist mainly of chitin,

mannans, and glucans. The specific structures of fungal cell wall polysaccharides are poorly known. Our aim is to extract and

characterize polysaccharides from enzyme production side stream. First part of the study is extraction and fractionation of

water-soluble polysaccharides. As an approach to extracting these fungal polysaccharides different extraction conditions such

as temperature, time, and concentration are being varied. Several extractions are made yielding fractions that contains

polysaccharides with different solubility. In future studies fractions are purified, and polysaccharides are characterized. This side stream fungal biomass could be an interesting option for novel bioresources.

P12

Gas chromatographic-mass spectrometric determination

of selected monosaccharides in wood hemicellulose

samples Mitja Kolar 1, @ , Katja Čuš 2 , Milena Ivanović 2 , Maša Islamčević Razboršek 2

1 : University of Ljubljana, Faculty of Chemistry and Chemical Technology

Večna pot 113, SI-1000 Ljubljana - Slovenia

2 : University of Maribor, Faculty of Chemistry and Chemical Engineering Smetanova 17, SI-2000 Maribor - Slovenia

A gas chromatographic – mass spectrometric (GC/MS) method for the simultaneous separation, identification and

determination of monosaccharides (arabinose, glucose, xylose, galactose, mannose and rhamnose) in wood hemicellulose

samples was developed. Hydrolysis/methanolysis of the hemicellulose samples was performed using: H2O, 2M HCl/H2O, 2M

HCl/MeOH or 5M HCl/MeOH (the temperature was maintained at 100°C for 3.5 h). The resulting monosaccharide units were

then trimethylsilylated (TMS) using MSTFA as derivatization reagent by heating at 80°C for 60 min. The compounds were

identified and quantified by comparison of their retention times and EI mass spectra¢s with those of pure standards. Phenyl β-

D-glucopyranoside was used as an internal standard (ISTD). The linearity of the method was tested within the concentration

range 20−200 mg L-1. Method was linear with the correlation coefficients (r2) in the range from 0.9934 to 0.9999. We proved

that the method was repeatable (precise) (RSD<3,9%) and accurate. Arabinose, xylose and rhamnose were not identified in

the hemicellulose samples. The average contents of other monosaccharides varied between 4% and 50% of dry weight

hemicellulose samples. The results confirmed that the highest concentrations of glucose (15%), mannose (47%) and galactose

(26%) were present in the sample where hemicellulose was methanolysed with 5 M HCl/MeOH. Relatively high concentrations

of glucose (12%), mannose (38%) and galactose (16%) were determined in the hydrolysate prepared using 2 M HCl/H2O. The

lowest contents of glucose (4.5%), mannose (29%) and galactose (16%) were determined in the methanolysate prepared with

2 M HCl/MeOH. In the samples of hemicellulose extracted using only water the studied compounds were not detected. Key words: hemicellulose, monosaccharides, GC/MS, hydrolysis, methanolysis.

P13

Lytic polysaccharide monooxygenases (LPMOs) as novel

tools for the preparation of innovative nanocelluloses Amani Chalak 1, 2, *, @ , Ana Villares 1, *, @ , Céline Moreau 1, *, @ , Mireille Haon 2, *, @ , Sacha

Grisel 2, *, @ , Aurore Labourel 2, *, @ , Jean-Guy Berrin 2, *, @ , Bernard Cathala 1, *, @

1 : Unité de recherche sur les Biopolymères, Interactions Assemblages

Institut National de la Recherche Agronomique : UR1268

44300, Nantes - France

2 : Biodiversité et Biotechnologie Fongiques

Ecole Centrale de Marseille : UMRA1163, Aix Marseille Université : UMRA1163, Institut National de la Recherche

Agronomique : UR1163

163 Avenue de LuminyCP92513288 Marseille Cedex 9France - France * : Corresponding author

Cellulose is the most abundant biopolymer on Earth. It has been used for centuries for paper, textile and chemicals production

(Klemm et al., 2005). Nowadays, efficient breakdown of cellulose is taking on a new importance as it constitutes a promising

source for biofuels and advanced bio-based products such as nanocelluloses. Nanocelluloses arise from the fractionation of

the cellulose fibers by chemical hydrolysis (cellulose nanocrystals) (Ranby, 1951) or mechanical delamination (cellulose

nanofibers, NFC). In the case of NFC production, to pass from the macroscale to the nanoscale, mechanical treatments require

high energy inputs that hinder efficient production of NFC. Lytic polysaccharide monooxygenases (LPMOs) are recently

discovered oxidative enzymes that belong to the AA9 family within the CAZy database. When applied to cellulosic fibers,

LPMOs facilitate the defibrillation down to nanoscale, opening the road for a new pretreatment process (Villares et al,2017;

Bennati Granier et al., 2015). The objective of this study is to understand the LPMO action on cellulosic fibers. For this goal,

the LPMO9H from Podospora anserina was produced in Pichia pastoris with and without its carbohydrate binding module

(CBM), and the purpose of this work is to investigate the contribution of the CBM domain in the activity of this LPMO. In

order to depict the level of hierarchy on which LPMOs act, two nanocellulosic materials were used as substrates: Bacterial

cellulose nanocrystals (BCNCs) as a crystalline cellulose substrate, and regenerated cellulose as an amorphous cellulosic

substrate. The action of LPMO was investigated, in combination with cellobiohydrolase, by high performance anionic

exchange chromatography (HPAEC) and quartz crystal microbalance with dissipation (QCM-D). Revealing the mechanism

of action of LPMO is a key building block for their application in the production of novel nanocellulosic materials in a way

that respects the environment.

Bennati-Granier C., Garajova S., Champion C., Grisel S., Haon M., Zhou S., Fanuel M., Ropartz D., Rogniaux H.,

Gimbert I., Record E., and Berrin J-G Biotechnology for Biofuels 2015, 8:90

Klemm D., Heublein B., Fink H.P., and Bohn A. Angewandte Chemie International Edition 2005, 44 : 3358 – 3393

Ranby B. G., Discuss. Faraday Society., 1951

Villares A., Moreau C., Bennati-Granier C., Garajova S., Foucat L., Falourd X., Saake B., Berrin J.G. & Cathala B. Scientific Reports 2017, 7:40262

P14

The improvement of wet spinning of chitosan fibers Ekaterina Maevskaia 1, @ , Elena Elena Dresvyanina 1, 2 , Alexandra Alexandra Yudenko 2 , Vladimir

Vladimir Yudin 1, 3

1 : Peter the Great Saint-Petersburg Polytechnic University

Polytechnicheskaya, 29, 195251, Saint-Petersburg, Russia - Russia

2 : Saint-Petersburg State University of Industrial Technologies and Design

B. Morskaya, 18, 191186, Saint-Petersburg, Russia - Russia

3 : Institute of Macromolecular Compounds RAS Bolshoy pr. 31, 195251, Saint-Petersburg, Russia - Russia

Keywords: Chitosan, fiber, wet spinning, molecular mass, nonwoven hemostatic material

Abstract:Chitosan, a natural polysaccharide polymer is well-known for its unique properties, including biocompatibility,

biodegradation, lack of cytotoxicity and hemostatic effect. Due to such properties chitosan-based materials find a lot of

applications in biotechnology and medicine.

The method of wet spinning of chitosan fibers from an aqueous solution of 2% acetic acid is described in [1-3], it was shown

that spinning conditions can have a significant effect on the properties of the wet spun fibers [3]. In the present work we

investigated the molecular mass effect of chitosan on the fiber processing as well as on the rheological and mechanical

properties of spun monofilaments. The viscosity of solutions increases with increasing molecular mass, at the same time the

optimum concentration of the polymer in solution for fibers processing decreases with increasing molecular mass. The

monofilaments with the highest factor of orientation drawing (λ=100-120%) were prepared from chitosan with the highest

molecular mass, these fibers had the best mechanical. Taking into account the received data the method of spinning of chitosan-

based polyfilament was developed, the number of monofilaments in the polyfilament was varied from 12 to 100, the diameter

of monofilaments was 10-30 μm. These polyfilaments were subsequently used to prepare a nonwoven hemostatic material.

The studies of its efficiency were carried out.

References:

Dresvyanina E.N., Dobrovol'skaya I.P., et al. Influence of spinning conditions on properties of chitosan fibers. Fibre

chemistry. 2013, 5 (4), pp. 280-283.

Yudin V.E., Dobrovolskaya I.P., et al. Wet spinning of fibers made of chitosan and chitin nanofibrils. Carbohydrate

Polymers. 2014, 108, pp. 176-182.

Elena Dresvyanina, Alexandra Yudenko, Irina Dobrovolskaya, Vladimir Yudin, Pierfrancesco Morganti Preparation and

properties of Fibrous Materials based on chitosan // 2nd International EPNOE Junior Scientists Meeting “Future perspectives

in polysaccharide research”. – Sophia Antipolis, France, 2016, October 13-14, P 44.

Acknowledgment: Financial support of this work by RSF № 14-33-00003 is gratefully acknowledged.

Future perspective in polysaccharide research: The knowledge of the influence of molecular mass and spinning conditions on the properties of chitosan fiber is essentially to

control the fiber processing and the quality of ready-made fibers. Chitosan-based fibers and filaments can be promising materials for surgery, including biodegradable surgical suture materials and hemostatic materials.

P15

Comparison of bacterial cellulose yield in two strains of

Gluconacetobacter xylinus in Hestrinn-Schramm and

molasses media Ceren Sagdic Oztan 1, @ , Sezin Yilmaz 1 , Tuba Karaalp 1 , Melek Tuter 2, *, @ , Nevin Gul

Karaguler 1, @

1 : Istanbul Technical University Department of Molecular Biology-Genetics and Biotechnology

Faculty of Science and Letters, 34469, Maslak, Istanbul - Turkey

2 : Istanbul Technical University, Chemical Engineering Department

Chemical and Metallurgical Engineering Faculty, 34469, Maslak, Istanbul - Turkey * : Corresponding author

Bacterial cellulose (BC) has been an attractive bio-material due to its superior features such as mechanical strength,

biocompatibility, purity and lack of toxicity. However, the high production cost of BC in the conventional medium makes it

an unfavorable material. There has been great effort to find alternative media where BC can be produced with high yields and

low cost. In this study, two strains of Gluconacetobacter xylinus are compared in terms of their efficiency to use simple sugars

-glucose, sucrose, fructose, mannitol and lactose- in Hestrin-Schramm (HS) medium and to use molasses as the only medium.

Results show that DSM 2325 strain uses fructose the most effectively with 3.7 g/L BC yield, where DSM 2004 uses sucrose

the most efficiently with 3.5 g/L BC yield in HS medium. In the second part of the study, the same strains are cultivated in 20,

40, 60, 80 g/L molasses concentrations. Both strains gave the highest BC yield in 20 g/L molasses concentration with 0.974

g/L BC for DSM 2325 and 1.132 g/L BC for DSM 2004. It indicates that the strain choice is an important factor to produce BC in alternative media. These results are going to be further tested in another strain of G. xylinus - ATCC 53582.

P16

Thin Films from Acetylated Lignin Stefanie Müller 1, @ , Krisztina Zajki-Zechmeister 2, @ , Werner Schlemmer 1, @ , Harald

Plank 2, @ , Stefan Spirk 1, *, @

1 : Graz University of Technology, Institute for Paper-, Pulp- and Fibre Technology (IPZ),

Inffeldgasse 23a, 8010 Graz - Austria

2 : Institute of Electron Microscopy and Nanpoanalysis (FELMI)

Steyrergasse 17, 8010 Graz - Austria * : Corresponding author

Lignin is a highly abundant biopolymer, however, the varying sources and complexity in composition make the utilization

challenging. The solubility and reactivity of lignin can be strongly affected by chemical modification such as acetylation,

making it available to various additional applications. Acetylation can be achieved by a microwave assisted reaction with

acetanhydride. The obtained acetylated lignin (AcL) was further used to prepare thin films by spin coating with tuneable

thicknesses in the nanometer range depending on the AcL concentration. The films were characterized by different surface

sensitive techniques, such as contact angle determination, ATR-IR spectroscopy, atomic force microscopy and profilometry.

The preparation of defined thin films from acetylated lignin forms a good foundation for further research, especially in the

field of nanostructured biomacromolecules.

P17

Coated Cellulose Interface as Substrate for Dynamic

Observation of Protein Adhesion and Coupling Processes

with Liquid Atomic Force Microscopy Krisztina Zajki-Zechmeister 1, 2, @ , Stefan Spirk 2, *, @ , Harald Plank 1, *, @

1 : Graz University of Technology, Institute of Electron Microscopy and Nanpoanalysis (FELMI)

Steyrergasse 17, 8010 Graz - Austria

2 : Graz University of Technology, Institute for Paper-, Pulp- and Fibre Technology (IPZ),

Inffeldgasse 23a, 8010 Graz - Austria * : Corresponding author

Flat biopolymer substrates, such as cellulose thin films, enable a way to study interactions of biological systems. For this

purpose, different immobilization tools can be employed to selectively tune the interaction of certain biological

macromolecules such as proteins. In particular, coating with cellulose derivates and specific immobilization molecules result

in strong binding of a protein on the surface. In order to monitor the underlying mechanisms, liquid mode Atomic Force

Microscopy (Liquid-AFM) is used. This method facilitates the possibility to observe dynamic processes such as antibody-

antigen interactions in situ in aqueous conditions. Protein coated cellulose substrates are measured in real time in an antigen

enriched liquid, to monitor the adsorption/interaction behaviour of the antibodies and antigens. The possibility to coat different

proteins onto such films could give rise to an easily accessible biosensor, which could be used in a wide range of life science or medical applications.

P18

Determination of Surface Fractions of Cellulose Thin

Films Carina Sampl 1, 2, @ , Katrin Niegelhell 3 , Katri Kontturi 4 , Ulrich Hirn 1, 2, @ , Stefan Spirk 1, 2, *, @

1 : Institute of Paper, Pulp and Fibre Technology

Inffeldgasse 23 (A), 8010 Graz - Austria

2 : CD-Laboratory for Fiber Swelling and Paper Performance

Inffeldgasse 23(A), 8010 Graz - Austria

3 : Institute for Chemistry and Technology of Materials

Stremayrgasse 9, 8010 Graz - Austria

4 : Department of Forest Products Technology

P.O. Box 16100, 00076 Aalto - Finland * : Corresponding author

Swelling of cellulose is an important parameter in the processing of paper. In order to investigate the swelling behavior,

cellulose thin films are used as model systems. These films can be modified by chemical as well as physical treatments, aiming

at an increase of swelling at the film's surface while the bulk layer keeps its usual swelling behavior. Applying a combination

of surface sensitive techniques, namely “Multi Parameter Surface Plasmon Resonance Spectroscopy” (MP-SPR) and “Atomic

Force Microscopy” (AFM), it became possible to determine the surface fraction which plays a major role in the interaction

processes at the interface in such systems. MP-SPR is a very promising tool to monitor this spatially varied swelling behavior.

By combining AFM and MP-SPR, the cellulose film could be split into a so called interaction or roughness layer occurring at

the surface and a bulk layer. These results can give an explanation of the swelling behavior affecting the different cellulose layers within the film. In combination, these techniques are powerful instruments to solve key questions in material science.

P19

Bacterial cellulose on bioelectronics for the study and

treatment of neurodegenerative disorders Tiago Carvalho 1, @ , Armando Silvestre 1, @ , Pedro Inácio 2, 3, @ , Ana Mestre 2, 3, @ , Henrique

Gomes 2, 3, @ , Carmen Freire 1, *, @

1 : CICECO Aveiro Institute of Materials

University of Aveiro - Portugal

2 : Instituto das Telecomunicações

Instituto Superior Técnico (Lisbon) - Portugal

3 : University of Algarve

Faculdade de Ciências e Tecnologia - Portugal

* : Corresponding author

Brain disorders affect over two billion people worldwide, meaning that it is crucial to better understand them and find new

treatments. Recently, prosthetic electronic transducers have been developed, aiming to measure neuron pattern signals,

decoding and associating them with the brain's specific disease states[1]. Ideally, once the signals are decoded, the transducers

will be able to generate specific signal patterns to help the brain restoring its normal function.

These electroceutical devices[2] must be fabricated on soft and conformable substrates. In this vein, bacterial cellulose (BC)

membranes, has shown high potentialities, because their characteristics proved to facilitate the interaction between the

transducer and the brain cells. The electrophysiological sensing devices were typically prepared by printing a conducting

polymer, poly (3,4-ethylenedioxythiophene) polystyrene sulfonate (PEDOT:PSS), on the BC membranes. The printed

electrodes were used to record electrical signals from tumor neural cells (glioma cells)[3]. It is known that these cells generate

cooperative spikes under acidic environment and may account for epileptic seizures and other neurological side effects in

glioma patients.

However, BC is not biodegradable in vivo because of the absence of cellulases in the human body. To address this issue, we

have also fabricated and characterized BC membranes by means of chemical modification and combination with other

biopolymers, to become bioresorbable within a desired timeframe, while maintaining the most desired features for the proposed

application.

In this communication, the most important results on the use of BC to produce these electronic devices and their application

to record electrical signal from cells and the chemical modification of BC envying the production of bioresorbable membranes

will be presented and discussed.

1. Mestre, A. L. G. et al. Extracellular Electrophysiological Measurements of Cooperative Signals in Astrocytes

Populations. Front. Neural Circuits 11, 1–9 (2017).

2. Famm, K., Litt, B., Tracey, K. J., Boyden, E. S. & Slaoui, M. Drug discovery: a jump-start for electroceuticals. Nature 496,

159–61 (2013).

3. Rocha, P. R. F. et al. Extracellular electrical recording of pH-triggered bursts in C6 glioma cell populations. Sci. Adv. 2, e1600516 (2016).

P20

Bioresorption of porous three-dimensional chitosan-

based matrices Pavel Popryadukhin 1, @ , Galina Yukina 2, @ , Vladimir Yudin 2, @

1 : Institute of Macromolecular Compounds Russian Academy of Sciences

Bolshoy Pr. 31, Saint-Petersburg 199004 - Russia

2 : Peter the Great Saint-Petersburg State Polytechnical University Polytechnicheskaya Str. 29, Saint-Petersburg 194064 - Russia

Intensive development of medicine and tissue engineering requires designing bioengineering preparations that consist of a

polymer matrix and stem or somatic cells. These preparations should serve as functional substitutes for lost organs or their

parts, and should not cause autoimmune rejection. The development of bioengineering preparations allows also abandoning

the use of donor tissues and organs which are necessary in modern transplantology. The matrix material and its structure should

facilitate adhesion, proliferation and differentiation of recipient cells. To achieve this, the matrix should possess a certain

combination of properties (biocompatibility, bioresorbability, porosity, absence of toxicity, relatively high mechanical strength

and elasticity that are necessary for manipulations in liquid media).

Three-dimensional matrices with high porosity were prepared by lyophilization of chitosan solution. The mechanism and rate

of resorption of the resulting materials were studied in vivo. It was shown that resorption was completed in 12 months after

implantation into an animal. The formation of connective tissue was not observed and the surrounding tissue had no signs of

changes or damage. Histological analysis demonstrates that chitosan resorption occurred simultaneously with the formationof

collagen fibers and blood vessels. These results allow us to recommend the obtained chitosanbased porous material for use as

a matrix for tissue engineering and medicine. The authors are grateful to the Russian Science Foundation (grant № 14-33-00003) for financial support

P21

List of participants

last name first name email address Alves Zélia zeliaralves@ua.pt

Bajić Marijan marijan.bajic@ki.si

Beaumont Marco marco.beaumont@boku.ac.at

Bossu Julie juliebossu@hotmail.fr

Božič Mojca mojca.bozic@um.si

Bračič Matej matej.bracic@um.si

Bradič Bojana bojana.bradicbokica@gmail.com

Bratuša Ana ana.bratusa2@um.si

Canjko Miša Mojca misa.cajnko@ki.si

Carvalho Tiago tfc@ua.pt

Chalak Amani Amani.Chalak@inra.fr

David Grégoire gregoire.david@supagro.fr

de Bento Flores Carlos Eduardo carlosflores.ed@gmail.com

de Melo Eduardo emdm500@york.ac.uk

Dresvyanina Elena elenadresvyanina@gmail.com

Elschner Thomas thomas.elschner@ptspaper.de

Ezzawam Wafa pywme@leeds.ac.uk

Feldner Alexander alexander.feldner@ptspaper.de

Feldner Alexander Alexander.Feldner@ptspaper.de

Ferreira Sónia soniasferreira@ua.pt

Filipova Inese inese.filipova@inbox.lv

Fonseca Daniela danielafonseca@ua.pt

Fridrihsone Velta fridrihsone.velta@inbox.lv

Furlani Franco FRANCO.FURLANI@phd.units.it

Ganie Showkat alishowkat443@gmail.com

Gatt Etienne etienne.gatt@ensiacet.fr

Gericke Martin martin.gericke@uni-jena.de

Gimat Alice alice.gimat@orange.fr

Gonçalves Idalina idalina@ua.pt

Gorgieva Selestina selestina.gorgieva@um.si

Gorjanc Marija marija.gorjanc@ntf.uni-lj.si

Grothe Timo timo.grothe@fh-bielefeld.de

Hajj Raymond Raymond.hajj@mines-ales.fr

Hobisch Mathias mathias.hobisch@student.tugraz.at

Hotzel Konrad konrad.hotzel@uni-jena.de

Hribernik Silvo silvo.hribernik@um.si

Innerlohinger Josef j.innerlohinger@lenzing.com

Jaafar Zahraa zahraa.jaafar@inra.fr

Jančič Urška urska.jancic@um.si

Jimenez Saelices Clara clara.jimenez-saelices@inra.fr

Kaker Barbara barbara.kaker@um.si

Kamila Kapusniak kamilajochym@o2.pl

Kargl Rupert rupert.kargl@hotmail.com

Kogler Michaela m.kogler@lenzing.com

Kolar Mitja mitja.kolar@fkkt.uni-lj.si

Kurečič Manja manja.kurecic@um.si

Le Moigne Nicolas nicolas.le-moigne@mines-ales.fr

Lombardo Salvatore salvatore.lombardo@kuleuven.be

Lopes Joana lopesjoana@ua.pt

Maevskaia Ekaterina ma.eka@yandex.ru Marchenko-Sorochak Iryna marchenko.sorochak@upi.com.ua

Milojevic Marko marko.milojevic1@um.si

Massol Sylvie sylvie.massol@mines-paristech.fr

Mautner Andreas andreas.mautner@univie.ac.at

Maver Tina tina.maver@um.si

Meile Kristine kristine.meile@inbox.lv

Mohan Tamilselvan tamilselvan.mohan@um.si

Müller Stefanie stefanie.mueller@student.tugraz.at

Nasr-Eddine Bouhamou nasredine.bouhamou@univ-mosta.dz

Natalija Virant natalija.virant@um.si

Navard Patrick patrick.navard@mines-paristech.fr

Nessi Veronica veronica.nessi@inra.fr

Nikkilä Ida ida.nikkila@helsinki.fi

Ojstršek Alenka alenka.ojstrsek@um.si

Pereda Mariana mariana.pereda@inra.fr

Pettignano Asja asja.pettignano@insa-lyon.fr

Phillips Jade stxjp7@nottingham.ac.uk

Pivec Tanja tanja.pivec@um.si

Plohl Olivija olivija.plohl@um.si

Popryadukhin Pavel pavelpnru@gmail.com

Sagdic Oztan Ceren sagdicc@itu.edu.tr

Sampl Carina carina.sampl@tugraz.at

Schlemmer Werner werner.schlemmer@gmx.at

Senf Deborah deborah.senf@mpikg.mpg.de

Shabunin Anton anton-shab@yandex.ru

Sobanwa Motolani tolasobanwa@gmail.com

Spirk Stefan stefan.spirk@tugraz.at

Stana K Karin karin.stana@um.si

Strätz Juliane juliane.straetz@forst.tu-dresden.de

Strmečki Kos Slađana strmecki@irb.hr

Sushytskyi Leonid sushytsl@vscht.cz

Süßenbacher Michael m.suessenbacher@student.tugraz.at

Szafulera Kamila kszafulera@mitr.p.lodz.pl

Tanja Kos tanja.kos@um.si

Tavzes Črtomir crtomir.tavzes@innorenew.eu

Teh Sue Siang tehsuesiang@yahoo.com

Teichert Gundula teichert@student.tugraz.at

Thonhofer Martin thonhofer@tugraz.at

Thoury Valentin valentin.thoury@supagro.fr

Tkaučič Doris doris.tkaucic@um.si

van der Klis Frits frits.vanderklis@wur.nl

Van Rie Jonas jonas.vanrie@kuleuven.be

Verfaillie An an.verfaillie@kuleuven.be

Verhertbruggen Yves yves.verhertbruggen@inra.fr

Vilaró Pilar pilar.vilaro@cut.edu.uy

Weißl Michael michael.weissl@student.tugraz.at

Weissl Michael michael.weissl@student.tugraz.at

Zajki-Zechmeister Krisztina zajki-zechmeister@student.tugraz.at

Zalyvchyi Denys denyszlv4@gmail.com