This study presents a novel tool to predict temperature-exposure of incinerated pig teeth as a proxy for understanding impacts of fire on human teeth. Previous studies on the estimation of temperature-exposure of skeletal elements have been limited to that of heat-exposed bone. This predictive tool was developed using a multinomial regression model of colourimetric and hydroxyapatite crystal size variables using data obtained from unheated pig teeth and teeth incinerated at 300 °C, 600 °C, 800 °C and 1000 °C. An additional variable based on the observed appearance of the tooth was included in the tool. This enables the tooth to be classified as definitely burnt (600 °C-1000 °C) or uncertain (27 °C/300 °C). As a result, the model predicting the temperature-exposure of the incinerated teeth had an accuracy of 95%. This tool is a holistic, robust and reliable approach to estimate temperature of heat-exposed pig teeth, with high accuracy, and may act as a valuable proxy to estimate heat exposure for human teeth in forensic casework.
Zerumbone, a natural dietary lipophilic compound with low water solubility (1.296 mg/L at 25°C) was used in this investigation. The zerumbone was loaded into nanostructured lipid carriers using a hot, high-pressure homogenization technique. The physicochemical properties of the zerumbone-loaded nanostructured lipid carriers (ZER-NLC) were determined. The ZER-NLC particles had an average size of 52.68 ± 0.1 nm and a polydispersity index of 0.29 ± 0.004 μm. Transmission electron microscopy showed that the particles were spherical in shape. The zeta potential of the ZER-NLC was -25.03 ± 1.24 mV, entrapment efficiency was 99.03%, and drug loading was 7.92%. In vitro drug release of zerumbone from ZER-NLC was 46.7%, and for a pure zerumbone dispersion was 90.5% over 48 hours, following a zero equation. Using the MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) assay in human T-cell acute lymphoblastic leukemia (Jurkat) cells, the half maximal inhibitory concentration (IC50) of ZER-NLC was 5.64 ± 0.38 μg/mL, and for free zerumbone was 5.39 ± 0.43 μg/mL after 72 hours of treatment. This study strongly suggests that ZER-NLC have potential as a sustained-release drug carrier system for the treatment of leukemia.
C1ORF123 is a human hypothetical protein found in open reading frame 123 of chromosome 1. The protein belongs to the DUF866 protein family comprising eukaryote-conserved proteins with unknown function. Recent proteomic and bioinformatic analyses identified the presence of C1ORF123 in brain, frontal cortex and synapses, as well as its involvement in endocrine function and polycystic ovary syndrome (PCOS), indicating the importance of its biological role. In order to provide a better understanding of the biological function of the human C1ORF123 protein, the characterization and analysis of recombinant C1ORF123 (rC1ORF123), including overexpression and purification, verification by mass spectrometry and a Western blot using anti-C1ORF123 antibodies, crystallization and X-ray diffraction analysis of the protein crystals, are reported here. The rC1ORF123 protein was crystallized by the hanging-drop vapor-diffusion method with a reservoir solution comprised of 20% PEG 3350, 0.2 M magnesium chloride hexahydrate, 0.1 M sodium citrate pH 6.5. The crystals diffracted to 1.9 Å resolution and belonged to an orthorhombic space group with unit-cell parameters a = 59.32, b = 65.35, c = 95.05 Å. The calculated Matthews coefficient (VM) value of 2.27 Å(3) Da(-1) suggests that there are two molecules per asymmetric unit, with an estimated solvent content of 45.7%.
Glass-ceramics are a group of materials that takes advantage of the various glass-forming methods before they are subsequently heat-treated in a controlled manner to effect nucleation and crystallization to produce crystalline materials. The production of glassceramic materials is to overcome the low mechanical strength in pure glassy materials. In this work, a study on the crystallisation of a soda-lime-silica glass was undertaken to ascertain how the processing parameters affect the crystallization of such glasses, viz. either via a single or two-step heat-treatment procedure, as well as the effect of soaking duration at the heat-treatment temperature. A soda-lime-silica glass system was chosen because the raw materials for producing such glasses are readily available and can be considered to be the cheapest. The glass produced was examined by thermal analysis to determine the nucleation and crystallization temperatures before they were heat-treated using a single-step and a two-stage heat-treatment procedures. The resultant glassceramics produced were characterized using x-ray diffraction as well as by scanning electron microscopy. The results thus obtained showed that a two-stage heat-treatment procedure is more successful in producing a well-crystallized glass-ceramic product.
Nitrogen-infused wet oxidation at different temperatures (400-1000 °C) was employed to transform tantalum-hafnia to hafnium-doped tantalum oxide films. High-temperature wet oxidation at 1000 °C marked an onset of crystallization occurring in the film, accompanied with the formation of an interfacial oxide due to a reaction between the inward-diffusing hydroxide ions, which were dissociated from the water molecules during wet oxidation. The existence of nitrogen has assisted in controlling the interfacial oxide formation. However, high-temperature oxidation caused a tendency for the nitrogen to desorb and form N-H complex after reacting with the hydroxide ions. Besides, the presence of N-H complex implied a decrease in the passivation at the oxide-Si interface by hydrogen. As a consequence, defect formation would happen at the interface and influence the metal-oxide-semiconductor characteristics of the samples. In comparison, tantalum-hafnia subjected to nitrogen-infused wet oxidation at 600 °C has obtained the highest dielectric constant, the largest band gap, and the lowest slow trap density.
White rice husk ash (RHA), an agriculture waste containing crystalline tridymite and alpha-cristobalite, was used as a silica source for zeolite Beta synthesis. The crystallization of zeolite Beta from RHA at 150 degrees C in the presence of tetraethylammonium hydroxide was monitored by XRD, FTIR and (29)Si MAS NMR techniques. It was found that zeolite Beta started to form after 12h and the complete crystallization of zeolite Beta phase was achieved after 2d. XRD, (29)Si MAS NMR and solid yield studies indicate that the transformation mechanism of silica present in RHA to zeolite Beta involves dissolution of the ash, formation of an amorphous aluminosilicate after 6h of crystallization, followed by dissolution in the mother liquor and final transformation to pure zeolite Beta crystals.
As part of a search for novel inhibitors of HIV-1 reverse transcriptase, the acetone extract of the giant African snail, Achatina fulica, was shown to be active. Fractionation of the extract yielded inophyllums A, B, C, and E and calophyllolide (1a, 2a, 3a, 3b, and 6), previously isolated from Calophyllum inophyllum Linn., a known source of nutrition for A. fulica. From a methanol/methylene chloride extract of C. inophyllum, the same natural products in considerably greater yield were isolated in addition to a novel enantiomer of soulattrolide (4), inophyllum P (2b), and two other novel compounds, inophyllums G-1 (7) and G-2 (8). The absolute stereochemistry of inophyllum A (1a) was determined to be 10(R), 11(S), 12(S) from a single-crystal X-ray analysis of its 4-bromobenzoate derivative, and the relative stereochemistries of the other inophyllums isolated from C. inophyllum were established by a comparison of their 1H NMR NOE values and coupling constants to those of inophyllum A (1a). Inophyllums B and P (2a and 2b) inhibited HIV reverse transcriptase with IC50 values of 38 and 130 nM, respectively, and both were active against HIV-1 in cell culture (IC50 of 1.4 and 1.6 microM). Closely related inophyllums A, C, D, and E, including calophyllic acids, were significantly less active or totally inactive, indicating certain structural requirements in the chromanol ring. Altogether, 11 compounds of the inophyllum class were isolated from C. inophyllum and are described together with the SAR of these novel anti-HIV compounds.
A novel (2E)-1-(5-chlorothiophen-2-yl)-3-{4-[(E)-2-phenylethenyl]phenyl}prop-2-en-1-one [C21H15ClOS] compound has been synthesized and its structure has been characterized by FT-IR, Raman and single-crystal X-ray diffraction techniques. The conformational isomers, optimized geometric parameters, normal mode frequencies and corresponding vibrational assignments of the compound have been examined by means of HF, MP2, BP86, BLYP, BMK, B3LYP, B3PW91, B3P86 and M06-2X functionals. Reliable vibrational assignments and molecular orbitals have been investigated by the potential energy distribution and natural bonding orbital analyses, respectively. The compound crystallizes in the triclinic space group P-1 with the cis-trans-trans form. There is a good agreement between the experimentally determined structural parameters and vibrational frequencies of the compound and those predicted theoretically using the density functional theory with the BLYP and BP86 functionals.
Dermatophagoides farinae is one of the major house dust mite (HDM) species that cause allergic diseases. N-terminally His-tagged recombinant Der f 21 (rDer f 21), a group 21 allergen, with the signal peptide truncated was successfully overexpressed in an Escherichia coli expression system. The purified rDer f 21 protein was initially crystallized using the sitting-drop vapour-diffusion method. Well diffracting protein crystals were obtained after optimization of the crystallization conditions using the hanging-drop vapour-diffusion method with a reservoir solution consisting of 0.19 M Tris-HCl pH 8.0, 32% PEG 400 at 293 K. X-ray diffraction data were collected to 1.49 Å resolution using an in-house X-ray source. The crystal belonged to the C-centered monoclinic space group C2, with unit-cell parameters a = 123.46, b = 27.71, c = 90.25 Å, β = 125.84°. The calculated Matthews coefficient (VM) of 2.06 Å(3) Da(-1) suggests that there are two molecules per asymmetric unit, with a solvent content of 40.3%. Despite sharing high sequence identity with Blo t 5 (45%) and Blo t 21 (41%), both of which were determined to be monomeric in solution, size-exclusion chromatography, static light scattering and self-rotation function analysis indicate that rDer f 21 is likely to be a dimeric protein.
Bleached kenaf core pulps (BKC) were hydrolyzed in H2SO4 (0.5M) at different time (0min to 90min) at room temperature. After the hydrolysis process, the viscosity average molecular weight (Mŋ) for BKC sample has reduced from 14.5×10(4) to 2.55×10(4). The hydrolyzed BKC was then dissolved in NaOH:urea:water and in LiOH:urea:water mixed solvent at the ratio of 7:12:81 and 4.6:15:80.4, respectively. The increased in hydrolysis time has decreased Mŋ of cellulose leading to easy dissolution process. Higher porosity and transparency with lower crystallinity index (CrI) of regenerated membrane produced can be achieved as the Mŋ reduced. The properties of membrane were observed through FESEM, UV-vis spectrophotometer and XRD. This study has proven that acid hydrolysis has reduced the Mŋ of cellulose, thus, enhanced the properties of regenerated membrane produced with assisted by alkaline/urea system.
In this study, the effect of lecithin (LEC) on the crystallization and gelation of fruit wax (FW) with sunflower oil was researched. A synergistic effect on the gel strength was observed at FW : LEC ratios of 75 : 25 and 50 : 50, compared to the corresponding single component formulations (100 : 0 and 0 : 100). Even below the critical gelling concentration (Cg) of FW, the addition of lecithin enabled gel formation. Lecithin affected the thermal behavior of the structure by delaying both crystallization and gel formation. The phospholipid acted as a crystal habit modifier changing the microstructure of the oleogel, as was observed by polarized light microscopy. Cryo-scanning electron microscopy revealed a similar platelet-like arrangement for both FW as a single oleogelator and FW in combination with LEC. However, a denser structure could be observed in the FW : LEC oleogelator mixture. Both the oil-binding capacity and the thixotropic recovery were enhanced upon lecithin addition. These improvements were attributed to the hydrogen bonding between FW and LEC, as suggested by Raman spectroscopy. We hypothesized that lecithin alters the molecular assembly properties of the FW due to the interactions between the polar moieties of the oleogelators, which consequently impacts the hydrophobic tail (re)arrangement in gelator-gelator and solvent-gelator interactions. The lipid crystal engineering approach followed here offered prospects of obtaining harder self-standing structures at a lower oleogelator concentration. These synergistic interactions provide an opportunity to reduce the wax concentration and, as such, the waxy mouthfeel without compromising the oleogel properties.
Cutinase catalyzes the hydrolysis of water-soluble esters and long-chain triglycerides and belongs to the family of serine hydrolases. The enzyme is thought to represent an evolutionary link between the esterase and lipase families and has potential applications in a wide range of industrial hydrolytic processes, for which an understanding of the molecular basis of its substrate specificity is critical. Glomerella cingulata cutinase has been cloned and the protein has been overexpressed in Escherichia coli, purified and subsequently crystallized in a wide range of different crystal forms in the presence and absence of inhibitors. The best crystals are those of the apo cutinase, which diffract to beyond 1.6 A resolution and belong to space group P4(1)2(1)2 or P4(3)2(1)2. Crystals of cutinase with the inhibitors PETFP or E600 belong to space groups P2(1)2(1)2(1) and P2(1), respectively, and diffract to approximately 2.5 A resolution. All of the crystals are suitable for structural studies, which are currently ongoing.
Sulfur has been highly sought by many industries everywhere around the world for various applications. This exceptionally useful element has been largely manufactured especially in powder form each year reflecting its increase in demand in line with technological advancement and uses for various product applications. The manufacturing processes include mining as well as chemical reactions in Claus Process. Rubber industries normally use abundance of sulfur in their latex compound to introduce vulcanization. The geneal concern of sulfur for rubber vulcanization is dispersibility in the rubber matrix due to improper optimization of its preparation process prior to latex compounding. Another crucial issue is crystallization of soluble sulfur from its insoluble origin, either during or post-rubber vulcanization that constitutes to formation of sulfur bloom that grows on the surface of the rubber articles. It is known that both issues are related to the process conditions and compounding recipe that could not be fully solved. Various studies have been conducted to minimize such occurences – from process optimization to sulfur chemistry itself – and of continuous improvement and innovation to solve various threats in sulfur applications. This paper reviews on detailed description on elemental sulfur, of respective industrial applications, and most importantly highlights on sulfur trends and issues normally encountered.
The main purpose of this study was to analyzed and examined the cocoa butter samples from Sabah. This work presence the crystal phases present in cocoa butter sample thus proved the existence of polymorphs obtained from differential scanning calorimeter (DSC) analysis and confirmed by X-ray diffraction (XRD). The cocoa butter samples were extracted using a conventional method by Soxhlet Extraction method. Crystals were formed under controlled static and tempered conditions. Cocoa butter polymorphism demonstrates that it is the actual crystallization temperature, not the cooling rate that determines the polymorph that crystallizes.
Biological fermentation of Rhizopus oryzae was introduced to extract cellulose nanofibre from durian skin fibre (DSF).
The diameter of the extracted durian skin nanofibre (DSNF) was in the range of 49-81 nm. The changes of chemical
composition of DSNF were clearly seen after evaluated via TAPPI standard test methods. Verification via Fourier transform
infrared (FTIR) confirmed the deduction of hemicelluloses and lignin in DSNF in the range of 1200 to 1000 cm-1. X-ray
diffraction (XRD) demonstrated increment in the crystallinity from 58.3 to 72.2% after biological fermentation. DSNF was
then incorporated into polylactic acid (PLA) via extrusion and injection moulding processes. The effect of 1-5 wt. % DSNF
content on PLA biocomposites was investigated for its mechanical and thermal properties. The presence of only 1 wt. %
improved the tensile and impact strength by 14.1 MPa and 33.1 kJ/m2
, respectively. The thermal properties of PLA-1DSNF
biocomposite also recorded higher thermal stability, glass transition temperature (Tg
), crystallization temperature (Tc
)
and melting temperature (Tm). Additionally, from the DMA, it was determined that PLA-1DSNF possessed lower storage
modulus and loss modulus, as well as low energy dissipation.
Diacylglycerol at 1 or 6% was added into refined bleached and deodorized palm oil (RBDPO) and crystallized from the melt in a thermally controlled water bath at 22°C for 90 min. Slurries were withdrawn after 5, 15, 30, 60 and 90 min of crystallization for solid fat content (SFC) and crystal morphology studies. Crystallization was also performed in a similar manner using a Labmax reactor connected to a FBRM detector to obtain the information on crystal count and size distribution during crystallization. SFC of the slurries increased with increase in crystallization time up to a certain level followed by a plateau. SFC of RBDPO added with DAG was also higher with the increase in percentage of DAG added and no induction time was observed to initiate crystallization in RBDPO added with DAG. The addition of DAG caused rapid crystallization of RBDPO as observed by enhance nucleation and larger crystal size with increase in the percentages of DAG added.
Refined bleached and deodorized palm oil (RBDPO) was crystallized from the melt in a thermally controlled water bath at 14 and 22°C for 90 min. Slurries were withdrawn after 5, 15, 30, 60 and 90 min of crystallization for crystal morphology studies. Crystallization was also performed in a similar manner using a Labmax reactor connected to a FBRM detector to obtain the information on crystal count and size distribution during crystallization. Based on the shape of the crystals viewed under the microscope, all crystals appeared as needle shaped spherulitic β´- form at both crystallization temperatures studied. Crystals were slightly larger with increase in crystallization time and at higher crystallization temperature (22°C). Crystals size range between 4.34 to 22.29µm. FBRM recorded high count of crystals with increased in crystallization time and at lower temperature (14°C).
Interesterification reaction involves rearrangement of the fatty acid radicals on the glycerol backbone, either randomly (chemical interesterification) or regioselectivity (enzymatic interesterification). Refined, bleached and deodourised palm oil (RBDPO) and palm kernel oil (RBDPKO) were blended in ratios from 25:75 to 75:25 (wt/wt). All blends were subjected to enzymatic (EI) and chemical interesterification (CI) using Lipozyme TL IM (4% w/w) and sodium methoxide (0.2% m/m) as the catalysts, respectively. The effect of EI and CI on the triacylglycerol (TAG) composition, thermal behaviour, polymorphism, crystal morphology and crystallisation kinetics were studied. The aim of this research is to characterise the nature of crystals in food product for certain desired structure. The crystallisation behaviour discussed in this study involves microstructure (PLM), polymorphism (XRD), thermal properties and crystallisation kinetics by DSC. The alteration in TAG composition was greater after CI as compared to EI with the reduction of LaLaLa (from 11.00% to 5.15%) and POO (from 14.28% to 4.87%). The DSC complete melting and crystallisation temperature of blend with 75% PO increased after CI, from 39.58 °C to 41.67 °C and from -30.84 °C to -28.33 °C, respectively. EI contributed to finer crystals than CI. However, the β' and β polymorph mixture and crystallisation kinetics (n = 2) of PO-PKO blends did not change after CI and EI. The knowledge on controlling crystallisation of RBDPO and RBDPKO blends is vital for proper processing condition like margarine production.
Hydroxyapatite (HAp) is an attractive bioceramics due to its similar composition to bone mineral and its ability to promote bone-implant interaction. However, its low strength has limited its application as load bearing implants. This paper presented a work focusing on the improvement of HAp mechanical property by synthesizing iron (Fe)-reinforced bovine HAp nanocomposite powders via mechanosynthesis method. The synthesis process was performed using high energy milling at varied milling time (3, 6, 9, and 12h). The samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), and scanning electron microscopy (SEM). Its mechanical properties were investigated by micro-Vicker's hardness and compression tests. Results showed that milling time directly influenced the characteristics of the nanocomposite powders. Amorphous BHAp was formed after 9 and 12h milling in the presence of HPO4(2-) ions. Continuous milling has improved the crystallinity of Fe without changing the HAp lattice structure. The nanocomposite powders were found in spherical shape, agglomerated and dense after longer milling time. The hardness and Young's modulus of the nanocomposites were also increased at 69% and 66%, respectively, as the milling time was prolonged from 3 to 12h. Therefore, the improvement of the mechanical properties of nanocomposite was attributed to high Fe crystallinity and homogenous, dense structure produced by mechanosynthesis.
The formation of struvite crystals or magnesium ammonium phosphate (MgNH4PO4) in palm oil mill effluent (POME) occurs as early as in the secondary stage of POME treatment system. Its growth continues in the subsequent tertiary treatment which reduces piping diameter, thus affecting POME treatment efficiency. Hypothesis. The beneficial use of the crystal is the motivation. This occurrence is rarely reported in scientific articles despite being a common problem faced by palm oil millers. The aim of this study is to characterize struvite crystals found in an anaerobic digester of a POME treatment facility in terms of their physical and chemical aspects. The compositions, morphology and properties of these crystals were determined via energy dispersive spectroscopy (EDS), elemental analysis, scanning electron microscopy (SEM) and x-ray diffraction (XRD). Solubility tests were carried out to establish solubility curve for struvite from POME. Finally, crystal growth experiment was done applying reaction crystallization method to demonstrate struvite precipitation from POME. Results showed that high phosphorous (P) (24.85 wt%) and magnesium (Mg) (21.33 wt%) content was found in the struvite sample. Elemental analysis detected carbon (C), hydrogen (H), nitrogen (N) and sulfur (S) below 4 wt%. The crystals analysed by XRD in this study were confirmed as struvite with 94.8% struvite mineral detected from its total volume. Having an orthorhombic crystal system, struvite crystals from POME recorded an average density of 1.701 g cm-3. Solubility curve of struvite from POME was established with maximum solubility of 275.6 mg L-1 at pH 3 and temperature 40 °C. Minimum solubility of 123.6 mg L-1 was recorded at pH 7 and temperature 25 °C. Crystal growth experiment utilizing POME as the source medium managed to achieve 67% reduction in phosphorous content. This study concluded that there is a potential of harnessing valuable nutrients from POME in the form of struvite. Struvite precipitation technology can be adapted in the management of POME in order to achieve maximum utilization of the nutrients that are still abundant in POME. At the same time maximization of nutrient extractions from POME will also reduce pollutants loading in the final discharge.