Archaeological Bone from Macro- to Nanoscale: Heat-Induced Modifications at Low Temperatures

2009 ◽  
Vol 8 ◽  
pp. 157-172 ◽  
Author(s):  
Céline Chadefaux ◽  
Ina Reiche
Keyword(s):  
Electron Microscopy ◽  
Low Temperatures ◽  
Type I Collagen ◽  
Bone Structure ◽  
Heating Temperature ◽  
Global Analysis ◽  
Type I ◽  
Scanning Calorimetry ◽  
Bone Material ◽  
X Ray

The present work focuses on the characterization of structural modifications in bone material induced by heating at low temperatures (90 - 250°C). This is of outmost importance when archaeological bone material is concerned. Changes occurring in the structure of the type I collagen and of the mineral-organic arrangement are especially investigated. This precise characterization required the combination of complementary analytical techniques: Differential Scanning Calorimetry (DSC) for global analysis of the collagen state of conservation, Scanning Electron Microscopy coupled with an Energy Dispersive X-Ray system (SEM-EDX), micro-Proton-Induced X-ray and Gamma-ray Emission (micro-PIXE/PIGE) for chemical analysis of the mineral fraction, Infrared microspectroscopy in attenuated total reflectance mode (micro-ATR-FT-IR) combined with curve-fitting for microscopic investigations and Transmission Electron Microscopy (TEM) on ultrathin sections to characterize the modifications in the mineral/organic interface at nanoscale. New criteria characterizing the effect of a thermal treatment at low temperatures on the bone structure from the macroscopic to the nanoscale were determined. There are namely a broadening of the Haversian canals, the inversion of the turns to -sheet ratio in the collagen structure determined by decomposition of the amide I IR band as well as a shift of amide II IR band position with the heating temperature to lower wavenumbers. At nanoscale, melting of the organic phase and clustering of hydroxyapatite (HAP) bone crystals can be observed. For comparison, unheated archaeological bones have been analyzed in order to test if the heat-induced modification can be distinguished from diagenetic alterations, generally dissolution-recrystallisation processes, in soils.

Electron microscopy of crystalline structure in thermotropic random copolymers

1991 ◽  
Vol 49 ◽  
pp. 1054-1055
Author(s):  
Afzana Anwer ◽  
S. Eilidh Bedford ◽  
Richard J. Spontak ◽  
Alan H. Windle
Keyword(s):  
Electron Microscopy ◽  
Crystalline Structure ◽  
Liquid Crystalline ◽  
Elevated Temperatures ◽  
Random Copolymers ◽  
Molecular Characteristics ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Identical Monomer ◽  
Periodic Layer

Random copolyesters composed of wholly aromatic monomers such as p-oxybenzoate (B) and 2,6-oxynaphthoate (N) are known to exhibit liquid crystalline characteristics at elevated temperatures and over a broad composition range. Previous studies employing techniques such as X-ray diffractometry (XRD) and differential scanning calorimetry (DSC) have conclusively proven that these thermotropic copolymers can possess a significant crystalline fraction, depending on molecular characteristics and processing history, despite the fact that the copolymer chains possess random intramolecular sequencing. Consequently, the nature of the crystalline structure that develops when these materials are processed in their mesophases and subsequently annealed has recently received considerable attention. A model that has been consistent with all experimental observations involves the Non-Periodic Layer (NPL) crystallite, which occurs when identical monomer sequences enter into register between adjacent chains. The objective of this work is to employ electron microscopy to identify and characterize these crystallites.

scholarly journals pH-controlled synthesis of sustainable lauric acid/SiO2 phase change material for scalable thermal energy storage

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Shafiq Ishak ◽  
Soumen Mandal ◽  
Han-Seung Lee ◽  
Jitendra Kumar Singh
Keyword(s):  
Electron Microscopy ◽  
Phase Change ◽  
Lauric Acid ◽  
Photoelectron Spectroscopy ◽  
Phase Change Materials ◽  
Precursor Solution ◽  
Thermal Reliability ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Heating And Cooling

AbstractLauric acid (LA) has been recommended as economic, eco-friendly, and commercially viable materials to be used as phase change materials (PCMs). Nevertheless, there is lack of optimized parameters to produce microencapsulated PCMs with good performance. In this study, different amounts of LA have been chosen as core materials while tetraethyl orthosilicate (TEOS) as the precursor solution to form silicon dioxide (SiO2) shell. The pH of precursor solution was kept at 2.5 for all composition of microencapsulated LA. The synthesized microencapsulated LA/SiO2 has been characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), X-Ray photoelectron spectroscopy (XPS), Scanning electron microscopy (SEM), and Transmission electron microscopy (TEM). The SEM and TEM confirm the microencapsulation of LA with SiO2. Thermogravimetric analysis (TGA) revealed better thermal stability of microencapsulated LA/SiO2 compared to pure LA. PCM with 50% LA i.e. LAPC-6 exhibited the highest encapsulation efficiency (96.50%) and encapsulation ratio (96.15%) through Differential scanning calorimetry (DSC) as well as good thermal reliability even after 30th cycle of heating and cooling process.

A new model for packing of type-I collagen molecules in the native fibril

1981 ◽  
Vol 1 (10) ◽  
pp. 801-810 ◽  
Author(s):  
Karl A. Piez ◽  
Benes L. Trus
Keyword(s):  
Type I Collagen ◽  
Hexagonal Lattice ◽  
Three Dimensional ◽  
Equatorial Region ◽  
Type I ◽  
X Ray Diffraction ◽  
X Ray ◽  
Left Handed ◽  
Crystal Model ◽  
Collagen Molecules

A specific fibril model is presented consisting of bundles of five-stranded microfibrils, which are usually disordered (except axially) but under lateral compression become ordered. The features are as follows (where D = 234 residues or 67 nm): (1) D-staggered collagen molecules 4.5 D long in the helical microfibril have a left-handed supercoil with a pitch of 400–700 residues, but microfibrils need not have helical symmetry. (2) Straight-tilted 0.5-D overlap regions on a near-hexagonal lattice contribute the discrete x-ray diffraction reflections arising from lateral order, while the gap regions remain disordered. (3) The overlap regions are equivalent, but are crystallographically distinguished by systematic displacements from the near-hexagonal lattice. (4) The unit cell is the same as in a recently proposed three-dimensional crystal model, and calculated intensities in the equatorial region of the x-ray diffraction pattern agree with observed values.

Research on compatibility and surface of high impact bio-based polyamide

2021 ◽  
pp. 095400832110055
Author(s):  
Yang Wang ◽  
Yuhui Zhang ◽  
Yuhan Xu ◽  
Xiucai Liu ◽  
Weihong Guo
Keyword(s):  
Electron Microscopy ◽  
Mechanical Properties ◽  
Scanning Electron Microscopy ◽  
Differential Scanning Calorimetry ◽  
Crystallization Behavior ◽  
High Impact ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Scanning Electron

The super-tough bio-based nylon was prepared by melt extrusion. In order to improve the compatibility between bio-based nylon and elastomer, the elastomer POE was grafted with maleic anhydride. Scanning Electron Microscopy (SEM) and Thermogravimetric Analysis (TGA) were used to study the compatibility and micro-distribution between super-tough bio-based nylon and toughened elastomers. The results of mechanical strength experiments show that the 20% content of POE-g-MAH has the best toughening effect. After toughening, the toughness of the super-tough nylon was significantly improved. The notched impact strength was 88 kJ/m2 increasing by 1700%, which was in line with the industrial super-tough nylon. X-ray Diffraction (XRD) and Differential Scanning Calorimetry (DSC) were used to study the crystallization behavior of bio-based PA56, and the effect of bio-based PA56 with high crystallinity on mechanical properties was analyzed from the microstructure.

scholarly journals Development of an Oxcarbazepine Solid Dispersion Using Skimmed Milk to Improve the Solubility and Dissolution Profile

2019 ◽  
Vol 11 (05) ◽  
Author(s):  
M. Shah ◽  
D. Patel
Keyword(s):  
Electron Microscopy ◽  
Solid Dispersion ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Infra Red ◽  
Crystalline Nature ◽  
Skimmed Milk ◽  
Scanning Electron

Oxcarbazepine has low solubility and low oral bioavailability, so it’s a challenge to formulate suitable dosage form. In this present investigation, to improve the dissolution rate and solubility, skimmed milk is used as a carrier. Physical mixers were prepared using various drugs to carrier ratio and spray drying technology was used to develop solid dispersion with the carrier. Various techniques were used to characterize the solid dispersion immediately after they were made which includes differential scanning calorimetry, scanning electron microscopy, fourier transform infra- red spectroscopy, X-ray diffraction and in-vitro dissolution profiles. The differential scanning calorimetry thermograms of raw drug indicated of its anhydrous crystalline nature. In thermograms of solid dispersion, the characteristic peak was absent suggesting the change from crystalline nature to amorphous form. X-ray diffraction confirmed those results. X-ray diffraction results of raw drug showed highly intense peak characteristic of its crystalline nature where solid dispersion showed less intense, more diffused peak indicating the change in crystalline form. Fourier transforms infra-red spectroscopy studies showed there was no interaction between drug and carrier. Scanning electron microscopy support the amorphous nature of mixer. The whole formulation showed distinct enhancement in the drug release behavior and solubility. The optimum oxcarbazepine to skimmed milk ratio 1:3 enhances the in-vitro drug release by 3.5 fold and also show distinct increase in solubility. It was concluded that for improvement of solubility of poorly water soluble oxcarbazepine, skimmed milk powder as a carrier can be utilize very well.

scholarly journals A Trifecta of New Insights into Ovine Footrot for Infection Drivers, Immune Response and Host Pathogen Interactions.

2021 ◽  
Author(s):  
Adam M. Blanchard ◽  
Ceri E. Staley ◽  
Laurence Shaw ◽  
Sean R Wattegedera ◽  
Christina-Marie Baumbach ◽  
...  
Keyword(s):  
Immune Response ◽  
Type I Collagen ◽  
Global Analysis ◽  
Bacterial Species ◽  
Skin Barrier ◽  
Control Measures ◽  
Skin Barrier Function ◽  
Type I ◽  
Bacterial Populations

Footrot is a polymicrobial infectious disease in sheep causing severe lameness, leading to one of the industry’s biggest welfare problems. The complex aetiology of footrot makes in-situ or in-vitro investigations difficult. Computational methods offer a solution to understanding the bacteria involved, how they may interact with the host and ultimately providing a way to identify targets for future hypotheses driven investigative work. Here we present the first combined global analysis of the bacterial community transcripts together with the host immune response in healthy and diseased ovine feet during a natural polymicrobial infection state using metatranscriptomics. The intra tissue and surface bacterial populations and the most abundant bacterial transcriptome were analysed, demonstrating footrot affected skin has a reduced diversity and increased abundances of, not only the causative bacteria Dichelobacter nodosus , but other species such as Mycoplasma fermentans and Porphyromonas asaccharolytica . Host transcriptomics reveals a suppression of biological processes relating to skin barrier function, vascular functions, and immunosurveillance in unhealthy interdigital skin, supported by histological findings that type I collagen (associated with scar tissue formation) is significantly increased in footrot affected interdigital skin comparted to outwardly healthy skin. Finally, we provide some interesting indications of host and pathogen interactions associated with virulence genes and the host spliceosome which could lead to the identification of future therapeutic targets. Impact Statement Lameness in sheep is a global welfare and economic concern and footrot is the leading cause of lameness, affecting up to 70% of flocks in the U.K. Current methods for control of this disease are labour intensive and account for approximately 65% of antibiotic use in sheep farming, whilst preventative vaccines suffer from poor efficacy due to antigen competition. Our limited understanding of cofounders, such as strain variation and polymicrobial nature of infection mean new efficacious, affordable and scalable control measures are not receiving much attention. Here we examine the surface and intracellular bacterial populations and propose potential interactions with the host. Identification of these key bacterial species involved in the initiation and progression of disease and the host immune mechanisms could help form the basis of new therapies.

Effects of Lattice Defects on Cathode Properties of LiMn2O4 Synthesized at Low Temperatures for Lithium Ion Secondary Battery

2008 ◽  
Vol 388 ◽  
pp. 41-44 ◽  
Author(s):  
Hiroyuki Kaiya ◽  
Shinya Suzuki ◽  
Masaru Miyayama
Keyword(s):  
Absorption Spectroscopy ◽  
Low Temperatures ◽  
Heating Temperature ◽  
Sol Gel ◽  
Lithium Ion ◽  
Lattice Defects ◽  
X Ray ◽  
Secondary Battery ◽  
Cation Mixing ◽  
X Ray Absorption

Effects of lattice defects on cathode properties of LiMn2O4 synthesized at low temperatures were investigated. LiMn2O4 powders were synthesized by a sol-gel method. The specific capacities of LiMn2O4 decreased from 134 to 81 mAh g-1 with decreasing heating temperature from 750 to 200°C. X-ray absorption spectroscopy showed that a large amount of lattice defects such as cation vacancies existed and cation mixing occurred in LiMn2O4 calcined at low temperatures. It was found that the low specific capacities of LiMn2O4 calcined at low temperatures were attributed to these lattice defects.

scholarly journals Age Hardening of Extruded AA 6005A Aluminium Alloy Powders

Materials ◽  
2019 ◽  
Vol 12 (14) ◽  
pp. 2316
Author(s):  
Feijoo ◽  
Cabeza ◽  
Merino ◽  
Pena ◽  
Rey
Keyword(s):  
Electron Microscopy ◽  
Heating Temperature ◽  
Hot Extrusion ◽  
Atomic Ratio ◽  
Age Hardening ◽  
Al Alloy ◽  
Ingot Metallurgy ◽  
Scanning Calorimetry ◽  
Transmission Electron ◽  
Peak Aging

Pre-alloyed micron-sized 6005A Al alloy (AA 6005A) powders, with a Mg/Si atomic ratio of 0.75, obtained by high pressure inert gas atomization were consolidated by uniaxial cold pressing at 200 MPa into cylindrical Al containers and hot extruded at 450, 480 and 500 °C with an extrusion rate of 7:1, followed by artificial T6 precipitation hardening. Ageing conditions were varied between 170 °C and 190 °C and times of 6, 7 and 8 hours. The microstructure of the extruded profiles was analysed using X-Ray diffractometry (XRD), light optical microscopy (LOM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Differential scanning calorimetry (DSC) was used to study the possible phase transformations. After our results, the peak-aging hardness condition was achieved at 180 °C for 6 h. Mechanical properties of the powder metallurgy (P/M) aluminium alloys consolidated by hot extrusion were superior to those of the extruded profiles of wrought alloy using conventional ingot metallurgy (I/M) billets. AA 6005A wrought P/M alloy via T6 heat treatment shown yield stress of 317 MPa and elongation of 21% at the extrusion pre-heating temperature of 500 °C.

Effect of Heat Treatments on Wettability of Nacre

2020 ◽  
Vol 985 ◽  
pp. 86-90
Author(s):  
Andi Muhammad Anshar ◽  
Sengo Kobayashi ◽  
Satoshi Okano
Keyword(s):  
Electron Microscopy ◽  
Thermal Analysis ◽  
Scanning Electron Microscopy ◽  
Heating Temperature ◽  
Pearl Oyster ◽  
Heat Treatments ◽  
Organic Substances ◽  
Water Contact ◽  
X Ray ◽  
Scanning Electron

The surface wettability of biomaterials influences on osteoblast behavior and bone formation. In this research, the variation of wettability of nacre by heat treatments was examined. Plates of the nacre were fabricated from shells of the Akoya pearl oyster. The specimens were heated at 100, 200, 300, 400, 500, and 600 °C. Characterizations of the specimens during and after heat treatments were carried out using scanning electron microscopy, X-ray diffractometry, and thermogravimetry-differential thermal analysis. The water contact angle (WCA) of the specimen was measured to evaluate wettability. The color of nacre changed from iridescent color to brownish weak-iridescence by the heating at and over 300 °C. The nacre heated at and over 300 °C became brittle because organic substances in nacre, which acts as the glue between the aragonite platelets were evaporated by the heating. The WCA of the specimen was decreased with increasing heating temperature, which should be related to the decrease in the number of organic substances in nacre by the heating.

scholarly journals Comprehensive Assessment of Nile Tilapia Skin (Oreochromis niloticus) Collagen Hydrogels for Wound Dressings

Marine Drugs ◽  
2020 ◽  
Vol 18 (4) ◽  
pp. 178 ◽  
Author(s):  
Baosheng Ge ◽  
Haonan Wang ◽  
Jie Li ◽  
Hengheng Liu ◽  
Yonghao Yin ◽  
...  
Keyword(s):  
Wound Dressing ◽  
Type I Collagen ◽  
Polyacrylamide Gel Electrophoresis ◽  
Sodium Dodecyl ◽  
Wound Dressings ◽  
Type I ◽  
Rheological Characterization ◽  
Scanning Calorimetry ◽  
Soluble Collagen ◽  
Collagen Hydrogels

Collagen plays an important role in the formation of extracellular matrix (ECM) and development/migration of cells and tissues. Here we report the preparation of collagen and collagen hydrogel from the skin of tilapia and an evaluation of their potential as a wound dressing for the treatment of refractory wounds. The acid-soluble collagen (ASC) and pepsin-soluble collagen (PSC) were extracted and characterized using sodium dodecyl sulphate-polyacrylamide gel electrophoresis (SDS-PAGE), differential scanning calorimetry (DSC), circular dichroism (CD) and Fourier transform infrared spectroscopy (FTIR) analysis. Both ASC and PSC belong to type I collagen and have a complete triple helix structure, but PSC shows lower molecular weight and thermal stability, and has the inherent low antigenicity. Therefore, PSC was selected to prepare biomedical hydrogels using its self-aggregating properties. Rheological characterization showed that the mechanical strength of the hydrogels increased as the PSC content increased. Scanning electron microscope (SEM) analysis indicated that hydrogels could form a regular network structure at a suitable PSC content. Cytotoxicity experiments confirmed that hydrogels with different PSC content showed no significant toxicity to fibroblasts. Skin repair experiments and pathological analysis showed that the collagen hydrogels wound dressing could significantly accelerate the healing of deep second-degree burn wounds and the generation of new skin appendages, which can be used for treatment of various refractory wounds.

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