125 results found
Chen W, Cheng TNH, Khaw LF, et al., 2021, Protein purification with nanoparticle-enhanced crystallisation, Separation and Purification Technology, Vol: 255, Pages: 1-7, ISSN: 1383-5866
In this study, silica nanoparticle was synthesised and used to promote lysozyme crystallisation effectively against high concentrations of protein impurity (bovine serum albumin (BSA); concentration = 25.0–50.0 mg/mL vs 5.0–25.0 mg/mL for lysozyme) at 1 mL scale, demonstrating that crystallisation is a viable and scalable protein purification technology with the aid of heterogeneous nucleants. The silica nanoparticle expedited the crystallisation of lysozyme through the enhancement of nucleation, significantly improving the process productivity. Furthermore, this study demonstrates the proper use of nanoparticle in terms of process time, as the improvement of product recovery by silica nanoparticle has a monomodal peak shape over time.
Ouyang J, Zhou L, Liu Z, et al., 2020, Biomass-derived activated carbons for the removal of pharmaceutical mircopollutants from wastewater: A review, SEPARATION AND PURIFICATION TECHNOLOGY, Vol: 253, ISSN: 1383-5866
Chen W, Karde V, Cheng TNH, et al., 2020, Surface hydrophobicity: effect of alkyl chain length and network homogeneity, Frontiers of Chemical Science and Engineering, ISSN: 2095-0179
Understanding the nature of hydrophobicity has fundamental importance in environmental applications. Using spherical silica nanoparticles (diameter = 369 ± 7 nm) as the model material, the current study investigates the relationship between the alkyl chain network and hydrophobicity. Two alkyl silanes with different chain length (triethoxymethylsilane (C1) vs trimethoxy(octyl)silane (C8)) were utilised separately for the functionalisation of the nanoparticles. Water contact angle and inverse gas chromatography results show that the alkyl chain length is essential for controlling hydrophobicity, as the octyl-functionalised nanoparticles were highly hydrophobic (water contact angle = 150.6 ± 6.6°), whereas the methyl-functionalised nanoparticles were hydrophilic (i.e. water contact angle = 0°, similar to the pristine nanoparticles). The homogeneity of the octyl-chain network also has significant effect on hydrophobicity, as the water contact angle was reduced significantly from 148.4 ± 3.5° to 30.5 ± 1.0° with a methyl-/octyl-silane mixture (ratio = 160 : 40 µL · g-1 nanoparticles).
Li X, Chen W, Yang H, et al., 2020, Protein crystal occurrence domains in selective protein crystallisation for bio-separation, CrystEngComm, Vol: 22, Pages: 4566-4572, ISSN: 1466-8033
Bio-separation is a key bottleneck in the manufacture of biopharmaceuticals. In this work, we report experimental evidence of direct selective protein crystallisation from a binary protein mixture solution. Lysozyme–thaumatin mixtures with a wide protein composition range (0–100 mg mL−1, respectively) were tested under the same crystallisation cocktail conditions using the hanging-drop vapour-diffusion (HDVD) crystallisation method. This work demonstrates the selectivity of crystallisation from a model binary protein mixture and four crystal occurrence domains were determined as the operation windows of selective crystallisation of the target protein: 1) an unsaturated region with no crystal formation, 2 & 3) target regions with only a single type of protein crystals (lysozyme crystals only or thaumatin crystals only) and 4) a mixture region which have a mixture of both types of protein. This study demonstrates that protein crystallisation is not only applicable to high-purity protein solutions and emphasizes the vital impacts of the presence of protein impurities in the process of target protein crystallisation. The study concludes that protein crystallisation is a feasible approach to separate a target protein from a complex mixture environment which can be achieved by manipulating the crystallisation operation conditions such as mixture composition, precipitant concentration, and operation time.
Delmas LC, White AJP, Pugh D, et al., 2020, Stable metal-organic frameworks with low water affinity built from methyl-siloxane linkers, CHEMICAL COMMUNICATIONS, Vol: 56, Pages: 7905-7908, ISSN: 1359-7345
Karde V, Guo M, Heng JYY, 2020, Influence of interparticle structuring on the surface energetics of a binary powder system, International Journal of Pharmaceutics, Vol: 581, ISSN: 0378-5173
The structuring of component particles in binary compositions affects the solid-solid interfacial properties. This work reports the effect of interparticle interactions in binary powder compositions of D-Mannitol and glass beads through the heterogeneity data obtained from Finite Dilution Inverse Gas Chromatography (FD-IGC). Three different scenarios viz. structured, random and segregated systems of the binary powder composition were considered for the analysis in the IGC column. Binary mixtures with large size disparity between the components produced structured mixtures exhibiting a guest-host type of interactions and energetic homogeneity irrespective of the energetics of the finer component. Random and segregated systems revealed a heterogeneous trend in the data indicating preferential probing of the active sites of the composition, particularly at the lower probe coverages. The results demonstrate that in the multicomponent binary systems the surface energetics is influenced by the solid-solid interfaces and structuring of the component particles within the mix i.e., the surface energy analysis could reveal a mixing behavior in powders. Furthermore, an adsorption energy distribution model based on Boltzmann statistics and simulation fitting approach was employed to deconvolute the distribution of the changing energy landscape of the binary mixtures.
Ngeow YW, Williams DR, Chapman A, et al., 2020, Surface Energy Mapping of Modified Silica Using IGC Technique at Finite Dilution, ACS OMEGA, Vol: 5, Pages: 10266-10275, ISSN: 2470-1343
Roque ACA, Pina AS, Azevedo AM, et al., 2020, Anything but Conventional Chromatography Approaches in Bioseparation, BIOTECHNOLOGY JOURNAL, Vol: 15, ISSN: 1860-6768
Rosbottom I, Cheng TNH, Heng JYY, 2020, Computational analysis of the solid-state and solvation properties of carbamazepine in relation to its polymorphism, Chemical Engineering and Technology, Vol: 43, Pages: 1152-1159, ISSN: 0930-7516
The solvent‐dependent polymorphism of the active pharmaceutical ingredient (API) carbamazepine is interpreted from calculations of the solid‐state and API‐solvent intermolecular interactions. These simulations suggested that apolar solute‐solute interactions could be disrupted by apolar solvents. In contrast, the polar solute‐solute interactions were found to be easily disrupted by polar and protic solvents. This is consistent with experimental observations that the crystallization of the metastable form II is more dominant in apolar solvents. The Mercury program remains the gold standard in terms of usability; however, further expansion into more complex simulation techniques could make this package of even greater use in pharmaceutical manufacturing workflows.
Chen W, Park SJ, Kong F, et al., 2020, High protein-loading silica template for heterogeneous protein crystallization, Crystal Growth and Design, Vol: 20, Pages: 866-873, ISSN: 1528-7483
As a purification technology, crystallization is advantageous over chromatography and precipitation in terms of purity, cost, and scalability. In general, proteins have slow crystallization kinetics due to their complex configurations, but this problem can be overcome with heterogeneous nucleants. High protein-loading mesoporous silica is a promising nucleant due to its favorable interaction with protein. The current study employs such a template in the batch crystallization of lysozyme and thaumatin at 1 mL scale. Using lysozyme as the main model protein, the results show that the template had high protein loading (220–300 mg lysozyme/g silica) and induced significantly faster crystallization as compared to the unseeded samples over a wide range of initial protein concentration (10.0–47.5 mg/mL) at 25 °C with 0.5 M potassium sodium tartrate tetrahydrate (precipitant) concentration. It was found that the template had to be saturated with the target protein before the experiments to achieve faster kinetics, or else it could delay the crystallization process. These findings were reaffirmed by the crystallization experiments of thaumatin. The current study demonstrates the effectiveness of high protein-loading silica as a nucleant in protein crystallization and the importance of its pretreatment with the target protein.
Yang H, Huang L, Zhang F, et al., 2019, Gravity on crystallization of lysozyme: slower or faster?, Crystal Growth and Design, Vol: 19, Pages: 7402-7410, ISSN: 1528-7483
With the increase in applications of protein-based medicines approved and developed, downstream manufacturing of biopharmaceuticals has challenges of finding cost-effective and reliable routes. Biocrystallization and centrifugation have both been used to isolate and purify macromolecules, such as therapeutic protein and other functional proteins. However, the centrifugation cannot perfectly separate biomolecules, and the biocrystallization mainly focuses on structure determination on a scale of microliters or below. In this work, protein crystallization of lysozyme, with a concentration of 35–45 mg/mL, and sodium chloride, with a concentration of 45–55 mg/mL in the solution, on a scale of milliliters was performed under centrifugation. Different gravity levels of 1–20000g and centrifugation durations have been investigated during the nucleation and crystal growth process. There were no obvious influences of low gravity (<100g) and short duration (<5 min) of centrifugation on the crystallization process: i.e., on the changes in concentrations. With continuous centrifugation (>30 min), high gravity (>1000g) hindered the nucleation, i.e., it reduced the drop in concentration at the nucleation stage; however, it accelerated the crystal growth process, i.e. enhanced a drop in concentration at the crystal growth stage.
Parambil JV, Poornachary SK, Heng JYY, et al., 2019, Template-induced nucleation for controlling crystal polymorphism: from molecular mechanisms to applications in pharmaceutical processing, CrystEngComm, Vol: 21, Pages: 4122-4135, ISSN: 1466-8033
Over the last two decades, the use of template surfaces to induce heterogeneous crystal nucleation has been explored primarily to address two different goals: first, as an alternative to the conventional seeding technique used for polymorph control and, second, as a technique to promote the nucleation rate in novel crystallisation processes and formulations. The former need conceivably arises due to the risk of crystallising a new polymorph despite pre-seeding the solution with the desired crystal form. In this context, we review ongoing efforts in the research area of template-induced crystallisation, covering both experimental and simulation studies directed towards deeper understanding of the underpinning mechanisms. In addition, we report on the use of template-induced crystal nucleation as a process intensification technology for formulating drug substances and as a technique for enabling nucleation and polymorphic control during continuous manufacturing of active pharmaceutical ingredients.
Lapidot T, Matar OK, Heng JYY, 2019, Calcium sulphate crystallisation in the presence of mesoporous silica particles: experiments and population balance modelling, Chemical Engineering Science, Vol: 202, Pages: 238-249, ISSN: 0009-2509
A population balance model is used to investigate the effect of mesoporous silica particles on calcium sulphate crystallisation in a stirred batch crystalliser. The model accounts for nucleation, growth, agglomeration, breakage, and particle-assisted nucleation, and the model equations are solved numerically using the method of classes over a logarithmic, non-uniform mesh. The crystallisation process is characterized experimentally using electrical conductivity to track the ion concentration and laser diffraction to measure the steady-state crystal size distribution obtained at the end of the experiments. The experiments are carried out over a range of temperatures, initial supersaturations, particle pore diameters, and particle loadings. The model is first fitted to experimental data obtained in the absence of particles to determine kinetic parameters of the nucleation, growth, agglomeration, and breakage for pure calcium sulphate crystallisation. Varying pore diameter did not influence the catalytic effect of the particles, however, particle loading was found to significantly decrease the nucleation induction time. The model was extended to account for the presence of particles by fitting two additional mechanisms. The first proposed a particle-assisted nucleation where nuclei are produced via heterogeneous crystallisation, then detach by particle-particle collision that is second-order with respect to particle loading. The second proposed that the crystal breakage frequency increases linearly with particle loading. Good agreement with the experimental data is demonstrated over the range of conditions examined.
Ouyang J, Zhou L, Liu Z, et al., 2019, Solubility determination and modelling of benzamide in organic solvents at temperatures from 283.15 K and 323.15 K, and ternary phase diagrams of benzamide-benzoic acid cocrystals in ethanol at 298.15 K, JOURNAL OF MOLECULAR LIQUIDS, Vol: 286, ISSN: 0167-7322
Zou J, Wu J, Wang Y, et al., 2019, Synergistic effect of graphene oxide and different valence of cations on promoting catalase crystallization, Crystal Growth & Design, Vol: 19, Pages: 2838-2844, ISSN: 1528-7483
This study tests the effect of using the combination of graphene oxide (GO) with different valence cations as a heterogeneous nucleant on promoting catalase crystallization. By using GO and three types of salts with different valences, NaCl, MgCl2, and YCl3, the addition of GO with all three salts resulted in an increase in the percentage of crystal drops and a decrease in induction time. The experimental results further verified that there is a synergistic effect of GO and cations as the percentage of crystal drops was higher when GO with cations was added compared to control experiments where only GO or cations presented. It was also observed that the improvement in crystallization became more significant when cations with higher valence were utilized. It is believed that the enhancement in crystallization was due to the synergistic effect arising from the cation-π and electrostatic interactions between GO sheets and cations. These interactions subsequently contributed to the positively charged salt, which adsorbed and connected both negatively charged catalase molecules and the GO surfaces, increasing the local protein concentration and leading to crystallization. In addition, we compared LaCl3 and CeCl3 with YCl3 to verify the effect of the same valence salt on catalase crystallization and found that the higher the charge density, the more pronounced the promotion effect. This study provides a new protein crystallization methodology by exploiting GO with cations as heterogeneous nucleant to promote catalase crystallization and brings about a new model for investigating protein crystallization mechanisms.
Yang H, Belviso BD, Li X, et al., 2019, Optimization of vapor diffusion conditions for anti-CD20 crystallization and scale-up to meso batch, Crystals, Vol: 9, ISSN: 2073-4352
The crystal form is one of the preferred formulations for biotherapeutics, especially thanks to its ability to ensure high stability of the active ingredient. In addition, crystallization allows the recovery of a very pure drug, thus facilitating the manufacturing process. However, in many cases, crystallization is not trivial, and other formulations, such as the concentrate solution, represent the only choice. This is the case of anti-cluster of differentiation 20 (anti-CD20), which is one of the most sold antibodies for therapeutic uses. Here, we propose a set of optimized crystallization conditions for producing anti-CD20 needle-shaped crystals within 24 h in a very reproducible manner with high yield. High crystallization yield was obtained with high reproducibility using both hanging drop vapor diffusion and meso batch, which is a major step forward toward further scaling up the crystallization of anti-CD20. The influence of anti-CD20 storage conditions and the effect of different ions on the crystallization processes were also assessed. The crystal quality and the high yield allowed the first crystallographic investigation on anti-CD20, which positively confirmed the presence of the antibody in the crystals.
Ngeow YW, Chapman AV, Heng JYY, et al., 2019, Characterization of silica modified with silanes by using thermogravimetric analysis combined with infrared detection, Rubber Chemistry and Technology, Vol: 92, Pages: 237-262, ISSN: 0035-9475
Tire treads with reduced rolling resistance and increased wet grip can be achieved by coupling hydrophilic silica to hydrocarbon rubber by using an alkoxysilane. The silica surface was modified by reaction with a wide range of coupling and non-coupling silanes. The chemistry and extent of these silanizations were elucidated using thermogravimetric analysis (TGA) combined with infrared detection. The silane grafting efficiencies were typically 52–72%, but efficiencies were lower in the bulkier [3-(di-(tridecyloxypenta(ethyleneoxy))ethoxysilyl]propyl mercaptan. However, the silica surface coverage increases with increasing size of the silane. Grafting efficiencies were lower with higher silane loadings. In the TGA, ethoxy and methoxy groups are displaced from the grafted silanes mainly at moderate temperatures (up to about 495 °C) to form siloxane bridges. Over a similar temperature range, the weaker S–S bonds present in bis(3-triethoxysilylpropyl) tetrasulfide (TESPT)- or bis[3-(triethoxysilyl)propyl] disulfide (TESPD)-modified silica are cleaved, leading to weight losses from TESPT or TESPD bound at one end to the silica and from TESPT bound at both ends. The remaining weight losses from bound silanes occurred mainly at higher temperatures. In the commercial silanized silica Coupsil 8113, TGA indicates that about two of three ethoxy groups in each triethoxysilane were lost during the silanization process.
Zhang B, Wang Y, Thi S, et al., 2019, Enhancement of lysozyme crystallization using DNA as a polymeric additive, Crystals, Vol: 9, ISSN: 2073-4352
This study reports the first experimental evidence of using DNA as a polymeric additive to enhance protein crystallization. Using three kinds of DNA with different molecular weights—calf DNA, salmon DNA, and herring DNA—this study showed an improvement in the success rate of lysozyme crystallization, as compared to control experiments, especially at low lysozyme concentration. The improvement of crystallization is particularly significant in the presence of calf DNA with the highest molecular weight. Calf DNA also speeds up the induction time of lysozyme crystallization and increases the number of crystals per drop. We hypothesized the effect of DNA on protein crystallization may be due to the combination of excluded volume effect, change of water’s surface tension, and the water competition effect. This work confirms predications of the potential use of DNA as a polymeric additive to enhance protein crystallization, potentially applied to systems with limited protein available or difficult to crystallize.
Ngeow YW, Heng JYY, Williams DR, et al., 2019, TEM observation of silane coupling agent in silica-filled rubber tyre compound, Journal of Rubber Research, Vol: 22, Pages: 1-12, ISSN: 1511-1768
The microdispersion of silica in filled elastomer vulcanisates was evaluated by transmission electron microscopy (TEM)—network visualisation analysis. In this study, the silica is modified with a wide range of coupling and non-coupling silanes. The silica-filled elastomer samples were microtomed using a glass knife. The resulting TEM micrographs were interpreted and characterised based on aggregates with a cross-sectional area larger than 100 nm2. The study showed that silica surface modification has reduced the silica aggregate size by approximately 30–40% compared to an untreated silica-filled elastomer vulcanisate. The TEM micrographs showed evidence of coupling between silica and the elastomer phase and demonstrated a good estimation of silica microdispersion in the elastomer phase. This study has shown that the presence of different surface functionalities has an effect on the silica microdispersion.
Yang H, Chen W, Peczulis P, et al., 2019, The development and workflow of a continuous protein crystallisation process: A case of lysozyme, Crystal Growth & Design, Vol: 19, Pages: 983-991, ISSN: 1528-7483
In the present work, a workflow on the development of a continuous protein crystallisation is introduced, with lysozyme as a model protein, from micro L screening experiments, to small scale batch crystallisation experiments in a shaking crystallisation platform, and to batch and continuous crystallisation experiments in an oscillatory flow platform. The lysozyme crystallisation investigated were for a concentration range from 30 to 100 mg/mL, shaking conditions from 100 to 200 rpm in the batch shaking crystallisation platform, and oscillatory conditions with amplitude (x) from 5 to 30 mm and frequency (f) from 0.1 to 1.0 Hz in the batch oscillatory flow crystallisation platform. We propose the use of the Reynold’s number (Re) for scaling up of the process from the shaking batch to the continuous oscillatory flow platform. Additionally, it is shown that the nucleation rate increased with increase in concentration of initial lysozyme solution, or increase in shear rate, inducing smaller size of lysozyme crystals. These indicate that continuous crystallisation platforms may offer advantages to the downstream bioprocessing of proteins.
Zhang R, Liao W, Sun Y, et al., 2019, Investigating the Role of Glass and Quartz Substrates on the Formation of Interfacial Droplets, JOURNAL OF PHYSICAL CHEMISTRY C, Vol: 123, Pages: 1151-1159, ISSN: 1932-7447
Burnett DJ, Karde V, Heng J, 2019, Surface energy of albumins and the effect of relative humidity, ISSN: 1526-7547
© 2019 Omnipress - All rights reserved. Statement of Purpose: Mositure can greatly affect the structure, stability, folding and activity of protein molecules. The interactions of the sorbed moisture with the proteins can make them susceptible to undergo physico-chemical changes under humid conditions. These protein-water interactions get influenced by the number of polar and non-polar groups and their arrangement along the protein molecule. Water also plays an important role in hydrogen bonded networks and various hydrophilic and hydrophobic interactions. Although an important contributor for protein functionality, these water–protein interactions are still far from being fully understood. Surface energy could be employed as a potential descriptor for investigating these interactions.
Zhang B, Mei AR, Isbell MA, et al., 2018, DNA origami as seeds for promoting protein crystallization, ACS Applied Materials & Interfaces, Vol: 10, Pages: 44240-44246, ISSN: 1944-8244
This study reports the first experimental evidence of DNA origami as a seed resulting in the increase in probability of protein crystallization. Using DNA origami constructed from long single-stranded M13 DNA scaffolds folded with short single-stranded DNA staples, it was found that the addition of the DNA origami in concentrations of 2-6 nM to mixtures of a well-characterized protein (Catalase) solution (1.0-7.0 mg/mL) resulted in a higher proportion of mixtures with successful crystallization, up to 11x greater. The improvement to crystallization is evident particularly for mixtures with low concentrations of Catalase (< 5 mg/mL). DNA origami in different conformations: a flat rectangular sheet and a tubular hollow cylinder, were examined. Both conformations improved crystallization as compared to control experiments without M13 DNA or non-folded M13 DNA, but exhibited little difference in the extent of protein crystallization improvement. This work confirms predictions of the potential use of DNA origami to promote protein crystallization, with potential application to systems with limited protein available or difficult to crystallize.
Morgeneyer M, Ramirez A, Poletto M, et al., 2018, Particle technology as a uniform discipline? Towards a holistic approach to particles, their creation, characterisation, handling and processing!, Chemical Engineering Research and Design, ISSN: 0263-8762
Yao Z, Wu D, Heng JYY, et al., 2018, Surface characterization of bio-fillers from typical mollusk shell using computational algorithms, International Journal of Adhesion and Adhesives, Vol: 84, Pages: 48-53, ISSN: 0143-7496
The generation of surface free energy parameters calculated from contact angle data is a burdensome and time-consuming process. To facilitate these calculations, computational algorithms using three different programming languages—MATLAB, C and Python—were developed and validated by surface properties determination of PO and CPO. The results indicated that the surface free energy parameters calculated using the three algorithms were consistent. The unknowns were obtained directly from within the C and Python programs, however, indirectly from within MATLAB function. In addition, the assembly statements of the C function were longer than those of the other two. The obtained results were also compared with those from an IGC analysis. It showed that the values determined using the contact angle methods were consistent, although lower than those obtained by IGC analysis. Compared to , the component contributed less to . The lower and values for CPO which added up to a lower value, could reduce filler particle/particle interactions, allowing a better dispersion in a polymer matrix.
Yang H, Peczulis P, Inguva P, et al., 2018, Continuous protein crystallisation platform and process: Case of lysozyme, Chemical Engineering Research and Design, Vol: 136, Pages: 529-535, ISSN: 1744-3598
In this work, we designed and built a continuous crystallisation oscillatory flow platform. The lysozyme crystallisation behaviours were investigated at concentrations from 30 to 100 mg/mL, under oscillatory conditions with amplitude (x0) from 10 to 25 mm and frequency (f) from 0.05 to 0.25 Hz in a batch oscillatory flow crystallisation platform. The nucleation rate increased with increase in concentration of initial lysozyme solution, and was also found to increase with increase in shear rate. By learning the thermodynamics and kinetics of lysozyme crystallisation in batch oscillatory flow, the batch crystallisation process was successfully transferred to a continuous oscillatory flow crystallisation process. The equilibrium state of continuous crystallisation reached at residence time 200 min, and the final product crystals shape and size were consistent during the continuous process. This work demonstrates the feasibility of oscillatory flow based platforms for the development of continuous protein crystallisation as for downstream bioseparation.
Hadjittofis E, Isbell M, Karde V, et al., 2018, Influences of crystal anisotropy in pharmaceutical process development, Pharmaceutical Research, Vol: 35, ISSN: 0724-8741
Crystalline materials are of crucial importance to the pharmaceutical industry, as a large number of APIs are formulated in crystalline form, occasionally in the presence of crystalline excipients. Owing to their multifaceted character, crystals were found to have strongly anisotropic properties. In fact anisotropic properties were found to be quite important for a number of processes including milling, granulation and tabletting. However, an understanding of crystal anisotropy and an ability to control and predict crystal anisotropy are mostly subjects of interest for researchers, as they can have a profound influence on the development of more efficient process development approaches. A number of studies dealing with the aforementioned phenomena are grounded on over-simplistic assumptions, neglecting key attributes of crystalline materials, most importantly the anisotropic nature of a number of their properties. Moreover, concepts such as the influence of interfacial phenomena in the behaviour of crystalline materials during their growth and in vivo, are still poorly understood. The review aims to address concepts from a molecular perspective, focusing on crystal growth and dissolution. It begins with a brief outline of fundamental concepts of intermolecular and interfacial phenomena. The second part discusses their relevance to the field of pharmaceutical crystal growth and dissolution. Particular emphasis is given to works dealing with mechanistic understandings of the influence of solvents and additives on crystal habit. Furthermore, comments and perspectives, highlighting future directions for the implementation of fundamental concepts of interfacial phenomena for the rational understanding of crystal growth and dissolution processes, have been provided.
Yao Z, Wu D, Heng JYY, et al., 2017, Comparative study of surface properties determination of colored pearl-oyster-shell-derived filler using inverse gas chromatography method and contact angle measurements, International Journal of Adhesion and Adhesives, Vol: 78, Pages: 55-59, ISSN: 0143-7496
Mollusk shells, such as clam, mussel, oyster and pearl oyster shells, are potential candidates for commercial calcium carbonate-based fillers. In this work, the surface properties of colored pearl-oyster-shell-derived filler (CMF) were investigated with comparison to those of pearl oyster shell powder (MSP), using an inverse gas chromatography (IGC) method and contact angle measurements. A developed computational model for the interpretation of surface free energy heterogeneity distributions was applied to both samples. The contact angle measurements revealed an amphiphilic nature. The dispersion component of surface free energy for both samples calculated using the Owens–Wendt–Kaelble (OWK), van Oss–Chaudhury–Good (vOCG) and Wu methods were consistent with those determined using the IGC method. The deconvolution of surface energetic sites confirmed their energetic heterogeneity. The CMF displayed lower work of cohesion, which could be beneficial to the fabrication of polymer composites, as typically reduced filler particle-particle interactions would result.
Yang H, Song C, lim Y, et al., 2017, Selective Crystallisation of Carbamazepine Polymorphs on Differing Surface Properties, CrystEngComm, Vol: 19, Pages: 6573-6578, ISSN: 1466-8033
Surface-induced nucleation of carbamazepine (CBZ) in ethanol was investigated with different surface materials: glass, polytetrafluoroethylene (PTFE) and tin. The introduction of foreign surfaces with different areas and surface chemistries into the solution has an impact on the crystal morphology and polymorphic form (Form II or III). With an increase in supersaturation, a higher possibility of crystallisation of CBZ metastable Form II was observed, as expected. Increasing the number of inserts resulted in a direct increase in the surface area available for heterogeneous nucleation. The increase in surface area resulted in the greater possibility of obtaining the metastable Form II of CBZ. The stable Form III preferred to nucleate on tin rather than on glass and PTFE. The results indicate that the two different polymorphs of CBZ can be selectively crystallised out from solution with the aid of a foreign surface. The kinetic mechanism of heterogeneous nucleation of the different polymorphs induced by foreign surfaces was discussed. The potential applications will be used to control and design the crystallisation process.
Yao Z, Heng JYY, Lanceros-Mendez S, et al., 2017, Surface free energy and mechanical performance of LDPE/CBF composites containing toxic-metal free filler, International Journal of Adhesion and Adhesives, Vol: 77, Pages: 58-62, ISSN: 0143-7496
Heavy-metal contamination in children's toys is a widespread problem, and the international community has issued a series of safety standards to restrict and control the use of toxic metals in toys. In this work, a colored filler (CBF) was prepared using pearl oyster shell (POS) as the green raw material and azo dye as the colorant. Its surface properties were subsequently studied in comparison to those of POS powder using the inverse gas chromatography method. The dispersion surface free energy profiles for both CBF and POS showed that this component contributed the major part (>70%) to the total surface free energy. The CBF possessed lower polar surface free energy and was relatively more hydrophobic. It also showed a lower thermodynamic work of cohesion, allowing its better dispersion in a low density polyethylene (LDPE) matrix. Mechanical performance studies showed that adding CBF could significantly increase the tensile strength, elastic modulus, flexural strength and flexural modulus of LDPE composites. The absence of toxic metals coupled with excellent mechanical performance makes the CBF an ideal candidate as a filler for children's toys fabrication.
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