scholarly journals Aminoethyl substitution enhances the self-assembly properties of an aminocellulose as a potential archaeological wood consolidant

2020 ◽  
Vol 49 (8) ◽  
pp. 791-798 ◽  
Author(s):  
Jennifer M. K. Wakefield ◽  
Robert Hampe ◽  
Richard B. Gillis ◽  
Agnes Sitterli ◽  
Gary G. Adams ◽  
...  
Keyword(s):  
Self Assembly ◽  
Molecular Level ◽  
Sedimentation Equilibrium ◽  
Cellulose Derivatives ◽  
Two Stage ◽  
Archaeological Wood ◽  
Reversible Aggregation ◽  
Natural Cellulose ◽  
Film Forming ◽  
Stage Process

AbstractThe 6-deoxy-6-aminocelluloses—or “aminocelluloses”—are a class of synthetic natural cellulose derivatives which are mostly aqueous soluble and have excellent film-forming properties. Recent studies have connected these properties at the molecular level with protein-like self-associative behaviour for a range of aminocelluloses including a 6-deoxy-6-(ω-aminoethyl) aminocellulose AEA-1 with the association being a two-stage process—a reversible oligomerisation followed by further (semi-reversible) aggregation into larger structures. Here, we synthesise and compare a new 6-deoxy-6-(ω-aminoethyl) aminocellulose AEA-1′ with different degree of substitution with one with further alkyl derivatisation, namely 6-deoxy-6-(ω-hydroxyethyl) aminocellulose HEA-1′. As with AEA-1, sedimentation velocity and sedimentation equilibrium in the analytical ultracentrifuge still show a two-stage process for both AEA-1′ and HEA-1′, with the latter giving higher molar masses. The consequences of these properties for use as consolidants for archaeological wood are considered.

scholarly journals Tert-butyldimethylsilyl chitosan synthesis and characterization by analytical ultracentrifugation, for archaeological wood conservation

2020 ◽  
Vol 49 (8) ◽  
pp. 781-789 ◽  
Author(s):  
Jennifer M. K. Wakefield ◽  
Susan Braovac ◽  
Hartmut Kutzke ◽  
Robert A. Stockman ◽  
Stephen E. Harding
Keyword(s):  
Molar Mass ◽  
Analytical Ultracentrifugation ◽  
Monomer Unit ◽  
Sedimentation Equilibrium ◽  
Archaeological Wood ◽  
Water As Solvent ◽  
Stage Process ◽  
Future Work ◽  
Different Sources

AbstractThe Oseberg ship is one of the most important archaeological testimonies of the Vikings. After excavation in 1904, the wooden gravegoods were conserved using alum salts. This resulted in extreme degradation of a number of the objects a hundred years later through acid depolymerisation of cellulose and lignin. The fragile condition of the artefacts requires a reconsolidation which has to be done avoiding water as solvent. We synthesized tert-butyldimethylsilyl (TBDMS) chitosan which is soluble in a 50:50 solution of ethyl acetate and toluene. Measurement of its molecular weight, to anticipate its penetration, provided a challenge as the density difference of the polymer and solvent was too small to provide adequate solute redistribution under a centrifugal field, so a two-stage process was implemented (i) determination of the weight-average molar mass of the aqueous soluble activated precursor, chitosan mesylate, Mw,mc using sedimentation equilibrium with the SEDFIT-MSTAR algorithm, and determination of the degree of polymerisation DP; (ii) measurement of the average degree of substitution DSTBDMS of the TBDMS group on each chitosan monosaccharide monomer unit using NMR, to augment the Mw,mc value to give the molar mass of the TBDMS-chitosan. For the preparation, we find Mw = 9.8 kg·mol−1, which is within the acceptable limit for penetration and consolidation of degraded wood. Future work will test this on archaeological wood from different sources.

scholarly journals Two-Stage Biodiesel Synthesis from Used Cooking Oil with a High Acid Value via an Ultrasound-Assisted Method

Energies ◽  
2021 ◽  
Vol 14 (12) ◽  
pp. 3703
Author(s):  
Ming-Chien Hsiao ◽  
Wei-Ting Lin ◽  
Wei-Cheng Chiu ◽  
Shuhn-Shyurng Hou
Keyword(s):  
Acid Value ◽  
Molar Ratio ◽  
Optimal Conditions ◽  
Two Stage ◽  
Cooking Oil ◽  
High Acid ◽  
Used Cooking Oil ◽  
Biodiesel Synthesis ◽  
Stage Process ◽  
Ultrasound Assisted

In this study, ultrasound was used to accelerate two-stage (esterification–transesterification) catalytic synthesis of biodiesel from used cooking oil, which originally had a high acid value (4.35 mg KOH/g). In the first stage, acid-catalyzed esterification reaction conditions were developed with a 9:1 methanol/oil molar ratio, sulfuric acid dosage at 2 wt %, and a reaction temperature of 60 °C. Under ultrasound irradiation for 40 min, the acid value was effectively decreased from 4.35 to 1.67 mg KOH/g, which was decreased to a sufficient level (<2 mg KOH/g) to avoid the saponification problem for the subsequent transesterification reaction. In the following stage, base-catalyzed transesterification reactions were carried out with a 12:1 methanol/oil molar ratio, a sodium hydroxide dosage of 1 wt %, and a reaction temperature of 65 °C. Under ultrasound-assisted transesterification for 40 min, the conversion rate of biodiesel reached 97.05%, which met the requirement of EN 14214 standard, i.e., 96.5% minimum. In order to evaluate and explore the improvement of the ultrasound-assisted two-stage (esterification–transesterification) process in shortening the reaction time, additional two-stage biodiesel synthesis experiments using the traditional mechanical stirring method under the optimal conditions were further carried out in this study. It was found that, under the same optimal conditions, using the ultrasound-assisted two-stage process, the total reaction time was significantly reduced to only 80 min, which was much shorter than the total time required by the conventional method of 140 min. It is worth noting that compared with the traditional method without ultrasound, the intensification of the ultrasound-assisted two-stage process significantly shortened the total time from 140 min to 80 min, which is a reduction of 42.9%. It was concluded that the ultrasound-assisted two-stage (esterification–transesterification) catalytic process is an effective and time-saving method for synthesizing biodiesel from used cooking oil with a high acid value.

scholarly journals Terpene polyacrylate TPA5 shows favorable molecular hydrodynamic properties as a potential bioinspired archaeological wood consolidant

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Michelle Cutajar ◽  
Fabrizio Andriulo ◽  
Megan R. Thomsett ◽  
Jonathan C. Moore ◽  
Benoit Couturaud ◽  
...  
Keyword(s):  
Molar Mass ◽  
Analytical Ultracentrifugation ◽  
Gel Filtration ◽  
Axial Ratio ◽  
Sedimentation Equilibrium ◽  
Archaeological Wood ◽  
Molecular Hydrodynamic ◽  
Pine Trees ◽  
Minimal Concentration ◽  
Hydrogen Bonding Potential

AbstractThere is currently a pressing need for the development of novel bioinspired consolidants for waterlogged, archaeological wood. Bioinspired materials possess many advantages, such as biocompatibility and sustainability, which makes them ideal to use in this capacity. Based on this, a polyhydroxylated monomer was synthesised from α-pinene, a sustainable terpene feedstock derived from pine trees, and used to prepare a low molar mass polymer TPA5 through free radical polymerisation. This polymer was extensively characterised by NMR spectroscopy (chemical composition) and molecular hydrodynamics, primarily using analytical ultracentrifugation reinforced by gel filtration chromatography and viscometry, in order to investigate whether it would be suitable for wood consolidation purposes. Sedimentation equilibrium indicated a weight average molar mass Mw of (4.3 ± 0.2) kDa, with minimal concentration dependence. Further analysis with MULTISIG revealed a broad distribution of molar masses and this heterogeneity was further confirmed by sedimentation velocity. Conformation analyses with the Perrin P and viscosity increment ν universal hydrodynamic parameters indicated that the polymer had an elongated shape, with both factors giving consistent results and a consensus axial ratio of ~ 4.5. These collective properties—hydrogen bonding potential enhanced by an elongated shape, together with a small injectable molar mass—suggest this polymer is worthy of further consideration as a potential consolidant.

scholarly journals An In-Situ Reaction Route to Molecular Level Dispersed Bisimide and ZnO Nanorod Hybrids with Efficient Photo-Induced Charge Transfer

2021 ◽  
Vol 16 (1) ◽  
Author(s):  
Chunzheng Lv ◽  
Lirong He ◽  
Jiahong Tang ◽  
Feng Yang ◽  
Chuhong Zhang
Keyword(s):  
Charge Transfer ◽  
Electric Field ◽  
Self Assembly ◽  
Molecular Level ◽  
Surface Photovoltage ◽  
Zno Nanorod ◽  
In Situ Reaction ◽  
Perylene Bisimide ◽  
Induced Charge

AbstractAs an important photoconductive hybrid material, perylene/ZnO has attracted tremendous attention for photovoltaic-related applications, but generally faces a great challenge to design molecular level dispersed perylenes/ZnO nanohybrids due to easy phase separation between perylenes and ZnO nanocrystals. In this work, we reported an in-situ reaction method to prepare molecular level dispersed H-aggregates of perylene bisimide/ZnO nanorod hybrids. Surface photovoltage and electric field-induced surface photovoltage spectrum show that the photovoltage intensities of nanorod hybrids increased dramatically for 100 times compared with that of pristine perylene bisimide. The enhancement of photovoltage intensities resulting from two aspects: (1) the photo-generated electrons transfer from perylene bisimide to ZnO nanorod due to the electric field formed on the interface of perylene bisimide/ZnO; (2) the H-aggregates of perylene bisimide in ZnO nanorod composites, which is beneficial for photo-generated charge separation and transportation. The introduction of ordered self-assembly thiol-functionalized perylene-3,4,9,10-tetracarboxylic diimide (T-PTCDI)/ ZnO nanorod composites induces a significant improvement in incident photo-to-electron conversion efficiency. This work provides a novel mentality to boost photo-induced charge transfer efficiency, which brings new inspiration for the preparation of the highly efficient solar cell.

scholarly journals Food behavior change in late-life widowhood: A two-stage process

Appetite ◽  
2015 ◽  
Vol 95 ◽  
pp. 399-407 ◽  
Author(s):  
Elisabeth Vesnaver ◽  
Heather H. Keller ◽  
Olga Sutherland ◽  
Scott B. Maitland ◽  
J.L. Locher
Keyword(s):  
Behavior Change ◽  
Late Life ◽  
Food Behavior ◽  
Two Stage ◽  
Stage Process

High-efficiency CuInSe2 solar cells prepared by the two-stage process

Solar Cells ◽  
1989 ◽  
Vol 27 (1-4) ◽  
pp. 299-306 ◽  
Author(s):  
Bulent M. Basol ◽  
Vijay K. Kapur ◽  
Richard C. Kullberg
Keyword(s):  
Solar Cells ◽  
High Efficiency ◽  
Two Stage ◽  
Stage Process
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