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Technical grass lignins engineering with ionic liquids as a method for improving antioxidant activity
No full textInternational audienceWithin the Zelcor European project, INRA applied a newly-developed process in ionic liquids to depolymerise and functionalise lignin (increase the phenol content) to two reference lignin samples (Protobind 1000 from GreenValue and Futurol residue) and their fractions. Advantages of the process are to combine short reaction time (max 40 min) and low temperatures (max 110°C) compared to alternative catalytic processes. The process conditions were selected according to the prior optimisation performed on phenolic model compounds (monomer, dimer and milled wood isolated lignins ). Thioacidolysis, 31P NMR, and SEC were applied to the ethyl acetate soluble and insoluble reaction products so as to assess the degree of depolymerisation and demethylation. The results indicate that: i) a prior extraction of the ethyl acetate soluble compounds is beneficial to the process; ii) up to 30% solubility can be reached after the treatment of insoluble fractions; iii) demethylation occurs for all samples. The samples were then tested for antioxidant properties study to assess whether the process generates fractions with improved performances compared to the lignin samples and fractions already available. In parallel to the technical development of the process, security assessment has been undertaken through close interaction with INERIS to identify possible safety advantages of the process and to check that there is no major obstacle to future industrial development of the process
Niveaux de champs électromagnétiques de type radiofréquences dans l'environnement de deux services de néonatologie
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Estimation multi-annuelle des sources d’aérosols organiques et de leurs propriétés d’absorption de la lumière en région Parisienne
No full textCarbonaceous aerosols, including organic aerosols (OA) and black carbon (BC), are playing important roles on air quality and climate change. Therefore, quantifying contribution of their emission sources, as well as the sources of their gaseous precursors, is needed to implement efficient mitigation measures. Investigating trends in atmospheric composition is also essential to a better knowledge of present and future impacts of airborne particles on global warming. This work aimed at investigating on-line and in situ carbonaceous aerosol measurements performed for more than 6 years at the SIRTA facility (Site Instrumental de Recherche par Télédétection Atmosphérique). This observatory platform is part of the ACTRIS (Aerosols, Clouds, Trace gases Research InfraStructure). It is located 25 km southwest of Paris city center and is representative of background air quality in the Ile de France region. The main sources of submicron OA were discriminated through Positive Matrix Factorization applied to Aerosol Chemical Speciation Monitor (ACSM) data. Light absorption properties of BC and brown carbon (BrC) were obtained from multi-wavelength Aethalometer measurements. Converging results illustrated well-marked seasonal, weekly, and diel cycles of the various primary and secondary carbonaceous aerosol fractions. Primary OA (POA), mainly from wood burning and traffic emissions, were confirmed to dominate submicron OA concentrations during the coldest months (November to February), while Oxygenated OA (OOA) were shown as the major contributors during the rest of the year. Less Oxidized OOA (LO-OOA), possibly with predominant biogenic origins, were found to contribute up to about 60% of total submicron OA on average in summer. Trend analyses indicated slight decreasing features (in the range of 0.05-0.20 µg m-3 yr-1) for every OA fractions over the 6+-year investigated period, except for this LO-OOA factor which showed no significant trend. Regarding absorption properties, BrC - with overwhelming biomass burning origin - was found to have equivalent light absorption impact than BC at near-ultraviolet wavelengths during the winter season. In summer, a mean value of 1.6 was obtained for BC absorption enhancement (Eabs) due to secondary aerosol lensing effect, supporting possible higher BC-related radiative impact than currently expected. Last but not least, More Oxidized OOA (MO-OOA) were shown as the main agent for this Eabs and then appeared as one of the most critical aerosol fraction to be considered within near-future climate models.Les aérosols carbonés, qui incluent les aérosols organiques (AO) et le carbone suie (BC), jouent un rôle majeur sur la qualité de l’air et sur le climat. Il est donc primordial de pouvoir quantifier leurs sources, ainsi que celles de leurs précurseurs gazeux, pour la mise en œuvre de plans d’action appropriés. Les études de tendance sur la composition chimique de l’atmosphère sont également nécessaires afin d’améliorer les connaissances de l’impact des particules sur le réchauffement climatique, actuel et à venir. Ce travail de thèse a permis d’exploiter les mesures automatiques et in situ des aérosols carbonés réalisées au SIRTA (Site de Recherche par Télédétection Atmosphérique) depuis plus de 6 ans. Cet observatoire appartient au programme européen ACTRIS (infrastructure de recherche européenne sur les aérosols, nuages, et espèces gazeuses réactives). Il est situé à 25 km au sud-ouest de Paris et est représentatif de la pollution de fond en région Ile de France. Les principales sources d’AO ont été discriminées à l’aide de l’outil Positive Matrix Factorization appliqué aux données issus d’un Aerosol Chemical Speciation Monitor (ACSM). Les propriétés d’absorption de la lumière de BC et du brown carbon (BrC) ont été mesurées à l’aide d’un aethalomètre multi-longueurs d’onde. L’ensemble des résultats obtenus indiquent des cycles saisonniers, hebdomadaires et journaliers spécifiques aux différentes fractions des aérosols primaires et secondaires. Ils ont confirmé que l’AO primaire (AOP), provenant essentiellement de la combustion de biomasse et du transport routier, est prépondérant sur la période froide (de novembre à février), alors que le reste de l’année est dominé par des aérosols organiques oxygénés. Parmi ces derniers, une fraction moins oxydée, provenant probablement de façon majeure de précurseurs biogéniques, est prépondérante en été (60% de l’AO en moyenne estivale). Les études de tendance ont montré une légère diminution des concentrations (de l’ordre de 0.05-0.20 µg/m3 par an) de toutes les fractions d’AO identifiées au cours de la période étudiée, hormis pour cette fraction d’AO moins oxydée qui ne présente pas de tendance significative. Concernant les propriétés optiques, une contribution moyenne globalement équivalente à celle de BC a été observée pour le BrC dans le proche ultraviolet en hiver. Par ailleurs, il a été mis en évidence une augmentation significative des propriétés d’absorption du BC liée à des interactions avec les aérosols secondaires en mélange interne, en particulier en été (avec une valeur moyenne de 1.6 pour le paramètre Eabs). La fraction organique la plus oxydée a pu être identifiée comme principale responsable de ce phénomène, faisant des aérosols organiques secondaires l’une des fractions des particules les plus importants à considérer par les modèles climatiques
Problématiques de sécurité en lien avec les dangers à caractère physico-chimique lors de la valorisation des composés furaniques biosourcés principalement à partir d'humines
No full textThe present research work was integrated as part of the EU-funded project named HUGS (HUmins as Green and Sustainable precursors for eco-friendly building blocks and materials), involving 5 main partners (Institut national de l'environnement industriel et des risques - France, Avantium - the Netherlands, Institut de Chimie de Nice - France, Universidad De Cordoba- Spain and Leibniz - Institut Fur Katalyse Ev An Der Universitat Rostock- Germany). The project is essentially supported through five European Industrial Doctorate fellowships put in place when the HUGS-MSCA-ITN-2015 program was launched in 2016. The primary objective of the HUGS project was to explore several valorization pathways of so-called “humins” in order to add value and create better business cases. Humins (and similarly lignins) are the side products that may become low-cost feedstock resulting from a number of future biorefineries and sugar conversion processes. Humins are complex residues resulting from the Acid-Catalyzed Dehydration and condensation of sugars, having furan-rings in their polymeric structures. The work presented in this specific part of the HUGS project is essentially focusing on safety-related topics of all components and subsequent applications related to sugar dehydration technology. Priority actions were devoted to a first insight on the characterization of physicochemical safety profiles of the side-product humins and main (parent) furanic products. Some members of this large family of compounds (e.g. RMF and FDCA) have high volume potential which results in opening new doors towards the development of furanbased building blocks and a bio-based economy. Humins are residues or side products which can be burnt for energy. However, its safe and sustainable use in high-value applications could also become a key milestone in the so-called circular economy. In practice, the work has been developed in two main locations: primarily at the INERIS lab, located in Verneuil-en-Halatte and at Avantium, located in Amsterdam. Nearly all experimental research after the production of the components at Avantium was performed at INERIS. This involved the evaluation of physicochemical hazards of both humins (crude industrial humins and humin foams obtained by thermal curing) and a series of furanic compounds. Avantium is involved in the commercialization of humins, furanics and furanic polymers/materials as novel chemicals and materials. The work has encompassed: An extensive bibliographical review of humins, furanics, and their related products (polymers, composites) resulted in the following main conclusions o A lack of physicochemical safety-oriented studies for many furanic compounds and for humins was observed as these products are still in the early stage of development and only a few may be commercialized in the next 5 years.o Despite the limited availability of safety-related data, more studies on toxicity aspects have been conducted for a selected number of furanics than physicochemical safety-related aspects. o A few furanic family members that have been evaluated as biofuel components were found to have given better emphasis on addressing some physicochemical safety attributes. o Every modification of the process for acid-catalyzed sugar dehydration (such as solvent, temperature, residence time and sugar concentration) will result in different humins, which would certainly demand further characterization and safety profiling of the resulting humins. • Analytical development integrating the first examination of flash point distribution versus the Net Heating Values, and analysis of total heats of combustion of furanic compounds. • Design and development of experimental plan addressing the safety-related key parameters such as thermal stability, self-heating risks, fire-risk-assessment and flammability limits depending on the need for specific tests and availability of the test samples.Le travail de recherche présenté dans ce manuscrit fait partie intégrante d’un projet de recherche collaborative financé par l’Union-Européenne (Il s’agit d’un projet H2020 de type « Marie-Curie Action »), dénommé HUGS (pour « HUmins as Green and Sustainable precursors for eco-friendly building-blocks and materials »). Ce projet de recherche implique 5 partenaires (INERIS/UTC, France, Avantium, Pays-Bas, Université de Sophia Antipolis/CNRS, France, l’université de Cordoue, Espagne et le LIKAT de l’université de Rostock en Allemagne). La recherche menée dans ce projet est essentiellement structurée via la mise en place de 5 programmes sous-jacents de doctorat (intitulé « Doctorat industriel européen » dans l’appel d’offre H2020 (H2020-MSCA-ITN-2015) auquel a répondu le consortium de recherche), mis en place lors du lancement du projet « HUGS » en 2016. L’objectif premier du projet HUGS concerne l’étude de divers chemins de valorisation à haute valeur ajoutée des humines. Ces résidus de biomasse, à l’instar des lignines se présentent comme des sources de carbone renouvelable à faible coût, en émergence dans nombre de bioraffineries modernes. Les humines sont des résidus complexes résultant du procédé de déshydratation par catalyse acide des polysaccharides (sucres en C5 et C6) contenus dans la biomasse lignocellulosique, ayant des cycles furaniques dans sa structure polymère. Le travail présenté ici est centré essentiellement sur les questionnements de sécurité soulevés par la phase de développement du projet. De manière plus ciblée, des actions prioritaires ont été définies, à savoir l’obtention d’un premier profilage des risques à caractère physicochimique des humines, ainsi qu’une première évaluation des risques des composés furaniques, lesquels constituent une famille de composés potentiellement très grande et représentent une voie encourageante vers le développement de nouveaux synthons au service d’une économie biosourcée. Les humines étant des résidus fatals, leur réutilisation sure et durable constitue aussi une étape stratégique dans le contexte de l’économie circulaire. De manière opérationnelle, le travail a compris les principaux axes de recherche suivants : • Revue bibliographique continue tout au long du travail de thèse concernant les humines, les composés furaniques et les matériaux associés (polymères) en termes de données relatives à la sécurité et ayant conduit aux principales informations suivantes: o Rareté /absence d’études sur les dangers physiques des humines et nombres de composés furaniques, car ces produits sont souvent au premier stade de leur développement o Malgré une la disponibilité très limitée de données pertinentes sur la sécurité, le constat est fait que les aspects de toxicité (par ingestion) sont le plus souvent le point focal des études, au détriment de l’examen des dangers physiques.o Seuls quelques composés furaniques (ethers, esters) ont spécifiquement fait l’objet de l’étude de certaines caractérisations en lien avec la sécurité (par exemple en termes de stabilité thermique), dans le cas d’application comme composants biosourcés de carburants innovants o De nombreuses variables influent sur les caractéristiques des humines et notamment leur méthode de production : ce qui signifie que les résultats obtenus sur les humines dans le cadre de ce projet (une seule source d’approvisionnement) mériteraient des travaux de consolidation dans le futur • Développements analytiques intégrant un premier examen de la distribution des points d’éclair en fonction des chaleurs de combustion des composés furaniques et une analyse des chaleurs de combustion de ces mêmes composés furaniques
Geomechanical response of an abandoned chalk mine to multi-annual water table fluctuations
No full textInternational audienceThe Paris basin contains 35,000–40,000 mines, most of which are abandoned, having mined chalk, a rock very sensitive to water. Although they have been excavated above the groundwater level, some of the mines can be temporarily or permanently flooded, due to (some) exceptional rainfall events. We have thus instrumented the chalk mine of Estreux (Nord department) to measure the impact of the oscillations of the water table on the stability of one of its pillars. It is a mine dug around 20 m deep by the chambers and pillars method. Now abandoned, it is temporarily flooded when the water table, located a few meters below the mine floor, rises due to heavy precipitation, which occurs on average every 8 years. From 2004 to 2012, a pillar was equipped with a convergence rod and two extensometers. There is a correlation between the vertical and horizontal deformation rates of the pillar and the periodic rise in the water table. Chalk samples were also taken in situ and their geomechanical properties characterized in the laboratory. On this basis, a first 3D mechanical simulation of the behavior of this pillar has been carried out taking into account elasticity, plasticity and creep. The calculated mean values of deformation generally match the measurements, and the model succeeds in reproducing the annual fluctuations of these parameters in relation to those of the level of the water table. However, compared to the measurements carried out in situ, the current model exaggerates the vertical deformations compared to the horizontal deformations. However, with this first model, we can observe that the variations in the water table induce elastic and reversible deformations of the pillar, given the absence of plastification of the chalk. These deformations are complementary to those due to the creep induced by the weight of the overlying grounds. If we want to model the long-term behavior of the pillar, particularly under the effect of the fluctuations of the water table induced by the climate change in progress, it is necessary to improve this model, taking into account the hydromechanical couplings and the flows in unsaturated condition. In conclusion, it is proposed to use these data later in a complete mechanical model, still under development at INERIS
Enhancing the antioxidant activity of technical lignins by combining solvent fractionation and ionic-liquid treatment
No full textInternational audienceA grass soda technical lignin (PB1000) underwent a process combining solvent fractionation and treatment with an ionic liquid (IL), and a comprehensive investigation of the structural modifications was performed by using high-performance size-exclusion chromatography, P-31 NMR spectroscopy, thioacidolysis, and GC-MS. Three fractions with distinct reactivity were recovered from successive ethyl acetate (EA), butanone, and methanol extractions. In parallel, a fraction deprived of EA extractives was obtained. The samples were treated with methyl imidazolium bromide ([HMIM]Br) by using either conventional heating or microwave irradiation. The treatment allowed us to solubilize 28 % of the EA-insoluble fraction and yielded additional free phenols in all the fractions, as a consequence of depolymerization and demethylation. The gain of the combined process in terms of antioxidant properties was demonstrated through 2,2-diphenyl-1-picrylhydrazyl (DPPH.) radical-scavenging tests. Integrating further IL safety-related data and environmental considerations, this study paves the way for the sustainable production of phenolic oligomers competing with commercial antioxidants
: Travaux LCSQA 2017 (Convention n°2201070603)
No full textNote technique rendant compte de l’opportunité d’établir un protocole pour la caractérisation métrologique en laboratoire de micro-capteurs pour la mesure indicative des particules (au sens de la Directive européenne "Qualité de l'air 2008/50/CE")
Hydrolysis of Hemicellulose and Derivatives. A Review of Recent Advances in the Production of Furfural
No full textInternational audienceBiobased production of furfural has been known for decades. Nevertheless, bioeconomy and circular economy concepts is much more recent and has motivated a regain of interest of dedicated research to improve production modes and expand potential uses. Accordingly, this review paper aims essentially at outlining recent breakthroughs obtained in the field of furfural production from sugars and polysaccharides feedstocks. The review discusses advances obtained in major production pathways recently explored splitting in the following categories: (i) non-catalytic routes like use of critical solvents or hot water pretreatment, (ii) use of various homogeneous catalysts like mineral or organic acids, metal salts or ionic liquids, (iii) feedstock dehydration making use of various solid acid catalysts; (iv) feedstock dehydration making use of supported catalysts, (v) other heterogeneous catalytic routes. The paper also briefly overviews current understanding of furfural chemical synthesis and its underpinning mechanism as well as safety issues pertaining to the substance. Eventually, some remaining research topics are put in perspective for further optimization of biobased furfural production
Emerging pollutants in the EU: 10 years of NORMAN in support of environmental policies and regulations
No full textInternational audienceIn 2005, the European Commission funded the NORMAN project to promote a permanent network of reference laboratories and research centers, including academia, industry, standardization bodies, and NGOs. Since then, NORMAN has (i) facilitated a more rapid and wide-scope exchange of data on the occurrence and effects of contaminants of emerging concern (CECs), (ii) improved data quality and comparability via validation and harmonization of common sampling and measurement methods (chemical and biological), (iii) provided more transparent information and monitoring data on CECs, and (iv) established an independent and competent forum for the technical/scientific debate on issues related to emerging substances. NORMAN plays a significant role as an independent organization at the interface between science and policy, with the advantage of speaking to the European Commission and other public institutions with the “bigger voice” of more than 70 members from 20 countries. This article provides a summary of the first 10 years of the NORMAN network. It takes stock of the work done so far and outlines NORMAN’s vision for a Europe-wide collaboration on CECs and sustainable links from research to policy-making. It contains an overview of the state of play in prioritizing and monitoring emerging substances with reference to several innovative technologies and monitoring approaches. It provides the point of view of the NORMAN network on a burning issue—the regulation of CECs—and presents the positions of various stakeholders in the field (DG ENV, EEA, ECHA, and national agencies) who participated in the NORMAN workshop in October 2016. The main messages and conclusions from the round table discussions are briefly presented
Contribution à la caractérisation des émissions de nanomatériaux bâtimentaires
No full textInternational audienceThe intensive use of building nanomaterials lead to an increased risk of nanoparticle exposure. The present document aims to summarize works on nanoparticle emissions in the water, the air and the ageing effects on nanomaterial. A vast literature describes the release in the water and sometimes highlights the implicated quantities. In this case, measurements are expressed in mass concentration of chemical species. In contrast, few study deal with characterization of aerosol containing nanoparticles. Otherwise no study gives rise to the expression of a mass concentration of chemical species in aerosol. A method leading to a chemical speciation expressed as a masse concentration of airborne nanoparticles could be a clear improvement in this field and be directly used in nanotoxicology.L’usage intensif de nanomatériaux entraine un risque d’exposition accrue aux nanoparticules. Le présent document vise à résumer des travaux sur les émissions dans l’eau, l’air et les effets du vieillissement. Une abondante littérature décrit le relargage dans l’eau et met parfois en lumière les quantités en jeu. Les relargages sont fournis en concentration massique d’espèce chimique. En revanche un faible nombre d’étude est observé sur la caractérisation d’aérosols contenant des nanoparticules et aucune ne donne lieu à l’expression d’une concentration massique d’espèces chimiques contenues dans l’aérosol. Une méthode permettant une spéciation chimique de nanoparticules aérosolisées exprimée en masse pourrait être une amélioration significative et être exploitée directement en nanotoxicologie