The purpose of the research was to investigate the potential for converting agricultural by-products, barley hull and flaxseed hull as well as their co-extract, into value-added functional food ingredients. Four varieties of barley hull and 3 types of flaxseed hull were hydrolyzed in calcium hydroxide solution in a water bath at 70°C for 4 hrs with shaking. The major phenolic compounds in barley hull, flaxseed hull and their co-extracts were identified by reversed phase high performance liquid chromatography (HPLC) coupled with photodiode array detection (PAD) and quadrupole - time of flight (Q-TOF) mass spectrometry (LC-MS). Ferulic acid, p-coumaric acid, vanillic acid and vanillin, and four ferulate dehydrodimers were detected in barley hull and their co-extracts. Quantitative analysis was conducted on the phenolic acids using the available standards. However, the phenolic compounds in flaxseed were found to be distinct from that of barley hull. Large amounts of secoisolariciresinol diglucoside (SDG), ferulic acid glucoside (FeAG), p-coumaric acid glucoside (CouAG) were found in flaxseed hull with minor content of caffeic acid glucoside (CAG) and flavonoids herbacitin glucoside (HDG), whereas the phytochemical profile of the co-extract was enriched by combining major phenolic compounds from both barley hull and flaxseed hull.The antioxidant activity of barley hull, flaxseed hull as well as their co-extract was evaluated using DPPH radical scavenging assay while total phenolic content was measured using the Folin-Ciocalteau method. After screening using chemical assays, the representative barley hull extract, flaxseed hull extract as well as their co-extract were tested for their intracellular antioxidant activity and the antiproliferative activity in PC-3 human prostate cancer cells. Both chemical assays and the cell culture assays indicated that barley and flaxseed hull had strong antioxidant activity and antiproliferative activity. Although the co-extract exhibited the strong antioxidant activity in the chemicals assay, it behaved differently in the cell culture assay, which may be attributed to the chemical and biological properties of the major phenolics in the co-extract.Following evaluation of the antioxidant activity and anticancer effect of barley hull extract, flaxseed hull extract as well as their co-extract, each type of extract was incorporated into Chinese steamed bread (CSB). The phytochemical profile of CSB was enriched by incorporating barley hull extract, flaxseed hull extract as well as their co-extract, which resulted in a significant enhancement in the antioxidant activity evaluated by DPPH and ORAC. Therefore, barley hull, flaxseed hull and their co-extract are suggested as promising sources of functional food ingredients.

The object of this study was to identify microscopic differences among six selected cultivars of harakeke traditionally used by Maori in weaving. The cultivars were Arawa, Makaweroa, Paretaniwha, Takaiapu, Takirikau, and Tapamangu. The effectiveness of different microscopy techniques for taking measurements of the dimensions of ultimate fibres using a factorial experimental design was investigated in part A. Constant variables were geographical location, location of specimens along the leaf, season (winter), individual plant, fan, north-facing fan, and age of plant (approximately seven years), and cultivars (Paretaniwha and Tapamangu). Experimental variables were the microscopy techniques used and measurement axis. Techniques selected use on further cultivars in part B were transverse sections of leaf specimens 4 m thick, embedded in Paraplast� and observed using LM, and non-fixed ultimate fibres observed using SEM. In part B the dimensions of ultimate fibres from the six selected cultivars of harakeke were measured, and analysed (ANOVA and Tukey's HSD), and the transverse section shapes of fibre aggregates were observed. Transverse widths of ultimate fibres ranged from 10.15 m (Takaipu) -12.80 m (Paretaniwha). Ultimate fibre lengths ranged from 3735 m (Takirikau) - 4751 m (Makaweroa). The cultivars prizes for muka, Arawa and Makaweroa, had the longest and finest ultimate fibre bundles more uniform in transverse-sectional shape than the other cultivars studied and perhaps this explains their selection for extraction of muka. Takirikau had a high yield of ultimate fibre bundles, and perhaps this makes extraction of muka worthwhile. Paretaniwha differed from the other five cultivars studied having an average number of ultimate fibre bundles per unit width that were narrow and non-uniform in shape, and composed of short, thick, ultimate fibre cells. The microscopic structure of muka from six selected cultivars of harakeke used traditionally for weaving varied and may explain differences perceived by weavers, and that different end uses are preferred for various cultivars.

Bibliography: 136-146 / v, 146 leaves, [9] leaves of plates : ill. (some col.) ; 30 cm. / Title page, contents and abstract only. The complete thesis in print form is available from the University Library. / Thesis (Ph.D.)--Dept. of Agronomy, University of Adelaide, 1987

Cette thèse de doctorat a été réalisée dans le cadre du projet Fiabilin, qui regroupe 15 partenaires industriels et académiques, et vise à structurer une filière industrielle de production de biocomposites polyamide-11/fibres de lin. Ces travaux ont pour objectif de déterminer des performances multi-échelles de ce composite 100% biosourcé, afin d’envisager son usage en substitution de composites pétrosourcés. Nous avons tout d’abord mis en évidence la sensibilité des fibres de lin aux cycles temps-température des procédés de mise en œuvre, tant du point de vue de leurs propriétés mécaniques que de leur structure biochimique. Ensuite, nous avons montré les capacités du système PA11-lin à produire des performances mécaniques en traction compétitives vis-à-vis d’autres composites pétrosourcés. La qualité de l’interface fibre/matrice du biocomposite a également été étudiée à différentes échelles, montrant une compatibilité supérieure à celles de systèmes lin-résines thermodurcissables. La fin de vie du composite PA11-lin a été envisagée à travers le recyclage par broyages et injections successives. Les propriétés mécaniques du biocomposite à fibres courtes ainsi obtenu sont semblables au composite PPgMA-lin, avec une déformation à rupture accrue et qui augmente significativement avec le nombre de recyclages. Une analyse des cycles de production de plusieurs composites révèle les plus faibles impacts environnementaux du PA11-lin lors d’un dimensionnement des pièces en rigidité équivalentes. / This thesis has been carried out as part of the project Fiabilin, which includes 15 different academic and industrial partners, with an aim to develop industrial production of polyamide-11/flax biocomposite. The purpose of this work is to determine multi-scale performances of 100% biosourced composite, in order to substitute composite materials containing glass fibers and/or matrix derived from petroleum. First, we highlighted the flax fiber sensibility toward processing cycles (time and temperature), from mechanical and biochemical structure aspects. Then, we revealed the capacity of PA11-flax association to produce competitive mechanical properties compared to others usual composites. Fiber-matrix interface of the biocomposite was studied at micro and macro scales, showing a higher compatibility than some flax-thermoset resin systems. The end-of-life of the biocomposite was considered by recycling with successive grinding and injections. Then stiffness and strength at break of short fiber biocomposites thus obtained are similar to PPgMA-flax composites, whereas a strong increase of the strain at break according to the number of injection cycles was observed. A life cycle analysis of some composites production steps shows lower environmental impacts of PA11-flax when sizing was made through equivalent material stiffness.

Background, Consumption of marine-based oils high in omega-3 polyunsaturated fatty acids (n3PUFAs), eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) is known to protect against obesity-related pathologies. It is less clear whether traditional vegetable oils with high omega-6 polyunsaturated fatty acid (n6PUFA) content exhibit similar therapeutic benefits. As such, this study examined the metabolic effects of a plant-based n3PUFA, stearidonic acid (SDA), in polygenic obese rodents. Methods, Lean (LZR) and obese Zucker (OZR) rats were provided either a standard westernized control diet (CON) with a high n6PUFA to n3PUFA ratio (i.e., 16.2/1.0) or experimental diet modified with flaxseed (FLAX), menhaden (FISH), or SDA oil that resulted in n6PUFA to n3PUFA ratios of 1.7/1.0, 1.3/1.0, and 1.0/0.8, respectively. Results, After 12 weeks, total adiposity, dyslipidemia, glucose intolerance, and hepatic steatosis were all greater, whereas n3PUFA content in liver, adipose, and muscle was lower in OZR vs. LZR rats. Obese rodents fed modified FISH or SDA diets had lower serum lipids and hepatic fat content vs. CON. The omega-3 index (i.e., ÓEPA + DHA in erythrocyte membrane) was 4.0, 2.4, and 2.0-fold greater in rodents provided FISH, SDA, and FLAX vs. CON diet, irrespective of genotype. Total hepatic n3PUFA and DHA was highest in rats fed FISH, whereas both hepatic and extra-hepatic EPA was higher with FISH and SDA groups. Conclusions, these data indicate that SDA oil represents a viable plant-derived source of n3PUFA, which has therapeutic implications for several obesity-related pathologies.

Cette étude porte sur le comportement à l’impact et post-impact d’un composite 100% biosourcé, à fibres de lin et à matrice Polyamide 11. Une première étape a consisté à optimiser les paramètres de mise en oeuvre par thermocompression de ce composite. Deux types de tissus unidirectionnels de lin (A et B) ont été testés, ainsi que deux conditionnements de la résine PA11 : sous forme de film ou de poudre. Tout d’abord, les niveaux de température et de pression ont été optimisés sur un « premier set » de composites, élaborés à partir de lin A et de poudre de Polyamide 11. Ensuite, un « deuxième set » de composites a été étudié pour optimiser le choix des constituants. L’ensemble des composites fabriqués a été testé en traction, par DMA et par des mesures de taux de porosité. Il a été montré que la configuration optimale était obtenue avec le lin B et le Polyamide 11 sous forme de film, élaborée avec une température de 210°C et des paliers de pression de 25, 40 et 65 bars. Une analyse des endommagements créés en traction dans ce composite a été réalisée en couplant des observations par MEB et des enregistrements par émission acoustique. Il a ainsi été possible d’identifier quatre classes d’endommagement dans les composites [0]4 et [90]4, et cinq classes dans les composites [±45]s. Chacune de ces classes a été associée à une forme d'onde acoustique et à un type d’endommagement observé. La deuxième partie de ce travail a consisté à étudier l’influence d’un impact de 3,6J sur le comportement en traction et en compression de quatre séquences d’empilement : unidirectionnel [0]8, alterné [0/90]2s, sandwich [02/902]s et multidirectionnel [45/0/-45/90]s. Les grandeurs caractéristiques du comportement à l’impact ont tout d’abord été déterminées pour les quatre drapages.Les endommagements créés par l’impact ont été analysés par différentes techniques : observations visuelles,mesures topographiques, C-scan par ultrasons, et micro-tomographie. Les résultats ont montré que les configurations qui s’endommagent le moins à l’impact sont les drapages alterné et multidirectionnel. Les échantillons impactés ont ensuite été sollicités pour déterminer leurs propriétés post-impact, et les comparer aux résultats obtenus sur éprouvettes saines. Des essais de traction et de compression ont été réalisés sur cinq éprouvettes de chaque configuration. Lors de ces essais, les endommagements ont été suivis par émission acoustique, et les champs de déformation ont été mesurés par corrélation d’images. Les résultats ont montré que,grâce à la présence des plis à ±45°, le composite multidirectionnel présente les meilleures propriétés résiduelles.Enfin, un modèle post-impact a été mis en place, permettant, dans une première approche, en appliquant un module dégradé dans la zone impactée, de retrouver globalement les champs de déformations expérimentaux mesurés sur les différents drapages. / This PhD work deals with the impact and post-impact behavior of a fully bio-based composite made of flax fibresand Polyamide 11. The first goal was to optimize the hot press moulding parameters for manufacturing this composite. Two types of unidirectional flax fabrics (A and B) and two forms of Polyamide 11 (powder or film) were tested. At first, the pressure and temperature process values were optimized using a first set of composites made of flax A and Polyamide 11 in the form of powder. Then, an optimization of material components was conducted using a second set of composites. All the manufactured composites were tested by means of tensile tests, DMA and porosity measurements. Finally, an optimum configuration was determined: the composite flax B/PA 11 film manufactured with a temperature value of 210 °C and with gradual levels of pressure until 65 bars. Moreover, damage mechanisms were evaluated by acoustic emission and SEM observations during tensile tests. Four mechanisms were identified for the [0]4 and [90]4 composites and five for [±45]s composites. The second goal of this study was to study the effect of an impact of 3.6 J on the compression and tensile behaviors of four stacking sequences of this composite: unidirectional [0]8, alternated [0/90]2s, sandwich [02/902]s and multidirectional [45/0/- 45/90]s. The damage created by the impact in these four lay-ups was characterized thanks to different techniques: visual observations, topographic and C-scan measurements, and micro-tomography. It has been shown that the configurations with the smallest damage were the alternated and multidirectional composites. Then, impacted composites were tested by tensile and compressive loadings, and results were compared with the properties of non- impacted composites. Acoustic emission and digital image correlation were used to identify the damage and strain mechanisms of each type of composites. The results showed that, thanks to the presence of the ±45° plies, the multidirectional composite has the best post-impact behavior. Finally, a finite element model has been developed for simulating the post-impact behavior. As a first approach, a lower value of modulus has been implemented in the impacted area. It has allowed us to compare numerical and experimental strain fields for the different stacking sequences.

Ces travaux de doctorat ont été menés dans le cadre d'un contrat CIFRE entre l'entreprise Van Robaeys Frères, l'UBS et l'IFREMER. Les travaux visent à mieux comprendre certains paramètres influençant les propriétés de fibres de lin et celles de matériaux composites. Nous avons tout d'abord mis en évidence l'influence du degré de rouissage du lin sur les propriétés mécaniques des fibres de lin et celles de matériaux composites injectés lin/polypropylène. Ensuite, à l'aide d'une étude comparative, nous avons montré qu'il est possible de réaliser des matériaux composites unidirectionnels aux propriétés mécaniques très proches à partir de filasse ou d'étoupes de lin. Puis, l'influence de l'architecture de trois renforts non tissés de lin sur les propriétés mécaniques de composites à matrice thermoplastique a été soulignée. L'anisotropie des propriétés mécaniques de ces matériaux a été mise en évidence. Enfin, la connaissance des propriétés mécaniques de fibres de lin produites par l'entreprise Van Robaeys Frères a été approfondie. On note une relation directe entre les propriétés mécaniques des fibres et celles de composites à renfort unidirectionnel. La relation est plus complexe dans le cas de composites injectés à fibres courtes. / This research study has been carried out during a CIFRE joint project between the Van Robaeys Frères Company, UBS and IFREMER. The work aims to improve understanding of the properties of both flax fibres and composite materials reinforced with flax.First, the influence of the degree of retting of flax fibers on the tensile properties of single fibers and short fiber/polypropylene composites has been shown.Then, the properties of scutched flax and flax tow were compared. We have shown that it is possible to reach similar tensile properties for unidirectional composite materials manufactured from the two products.Moreover, the influence of three different flax nonwoven reinforcements on the mechanical properties of thermoplastic matrix composites was studied. These materials were found to show anisotropy of tensile properties.Finally, the mechanical properties of the flax fibres processed by the Van Robaeys Frères Company were examined. A straightforward relationship was found between the tensile properties of the fibres and the tensile properties of unidirectional composite materials. The relationship is more complex for short fibre injected composites.

The awareness of environmental sustainability drives the composite industry to utilize natural fibres. Natural fibres are a readily available resource with a relatively low price. In this study natural fibre flax reinforced polylactic acid (PLA) biocomposites were made using a new technique incorporating an air-laying nonwoven process. Flax and PLA fibres were blended and converted to fibre webs in the air-laying process. Composite prepregs were then made from the fibre webs. The prepregs were finally converted to composites by compression moulding. The relationship between the main process variables and the properties of the biocomposite was investigated. It was found that with increasing flax content, the mechanical properties increased. As the moulding temperature and moulding time increased, the mechanical properties decreased. The physical, thermal and morphological properties of the biocomposites were also studied. The appropriate processing parameters for the biocomposites were established for different fibre contents. The biodegradability and water absorption properties of the composites were evaluated. The composites were incubated in compost under controlled conditions. The percentage weight loss and the reduction in mechanical properties of PLA and biocomposites were determined at different time intervals. It was found that with increasing flax content, the mechanical properties of the biocomposites decreased more rapidly during the burial trial. The increasing of flax content led to the acceleration of weight loss due to preferential degradation of flax. This was further confirmed by the surface morphology of the biodegraded composites from Scanning Electron Microscope (SEM) image analysis. This study also investigated the manufacturing of 3D PLA/Flax nonwoven prepregs by using a new system of 3D nonwoven web formation, and 3D biocomposite was made using these prepregs. A new mould unit for web and a new aluminium mould for biocomposite were developed. The physical properties of 3D biocomposites were investigated and it was found that there is no significant difference between 2D and 3D biocomposites in density and void content. The effects of fibre content and processing variables on the crushing behaviour, energy absorption and failure mode of 3D shell biocomposites were experimentally studied.

Two experiments determined the effects of flaxseed supplementation on reproductive parameters in sheep. In experiment one, 240 multiparous Rambouillet ewes were assigned to one of two treatments: basal ration alone or basal ration with a Flaxlic® Sheep Tub offered over 35 days. Serum was collected weekly for progesterone (P4). Flaxseed supplementation did not improve progesterone concentration or reproductive parameters (P ≥ 0.26). In experiment two, 120 Rambouillet ram lambs were assigned to one of two treatments: basal ration alone or basal ration with a Flaxlic® Sheep Tub offered over 112 days. Scrotal circumference measurements, serum for testosterone, and semen were collected on day 84 and 112. Day effects were found for select semen measurements, testosterone, weight, and scrotal circumference (P ≤ 0.05). There was no effect of treatment on testosterone concentration (P = 0.99) or any semen quality characteristics (P ≥ 0.33). Overall, tub supplementation did not alter reproductive ability.

Bio-based flax fiber polymer composites (FFPC) have the potential to replace metals and synthetic fibers in certain applications due to their unique mechanical properties. However, the long term reliability of FFPC needs to be better understood. In this study, the fatigue limit was evaluated using mathematical, thermographic, and energy-based approaches. Each approach determined fatigue limits around 45% load of ultimate tensile strength at a loading frequency of 5 Hz. Thermographic and energy-based approaches were also implemented at different loading frequencies (5, 7, 10, and 15 Hz) to define the effect of loading frequency on the fatigue life. Fatigue limit was found to decrease slowly with increasing loading frequency. Moreover, two forms of damage energy (thermal and micro-mechanical) during cyclic loading was separated using an experimental approach to pinpoint the main responsible damage energy for decreasing fatigue limit with increasing loading frequency.