Calcium sulfate cement (CSC) has emerged as a potential bone filler material mainly because of the possibility of incorporating therapeutic agents. Delivery of the cement through a needle or cannula will make it more useful in clinical applications. However, it was not possible to make CSC injectable because of the inherent lack of viscosity. The present work demonstrates the design development of a viscous and fully-injectable CSC by incorporating hydrogen orthophosphate ions, which does not hamper the biocompatibility of the material. The effect of addition of hydrogen orthophosphate on the rheological properties of the CSC paste was studied using a custom made capillary rheometer. The physicochemical changes associated with cement setting process were examined using X-ray diffraction and Fourier transform infrared spectroscopy and the thermal changes were measured through isothermal differential scanning calorimetry. Micromorphological features of different compositions were observed in environmental scanning electron microscopy and the presence of phosphate ions was identified with energy dispersive X-ray spectroscopic analysis and inductively coupled plasma-optical emission spectroscopy. The results indicated that HPO4 (2-) ions have profound effects on the rheological properties and setting of the CSC paste. Significant finding is that the HPO4 (2-) ions are getting substituted in the calcium sulfate dihydrate crystals during setting. The variations of setting time and compressive strength of the cement with the additive concentration were investigated. An optimum concentration of 2.5 % w/w gave a fully-injectable cement with clinically relevant setting time (below 20 min) and compressive strength (12 MPa). It was possible to inject the optimised cement paste from a syringe through an 18-gauge needle with thumb pressure. This cement will be useful both as bone filler and as a local drug delivery medium and it allows minimally invasive bone defect management.

Calcium sulfate dihydrate, constituted as uniform crystals of low dimensions, is a potential biomaterial for clinical applications like bone graft substitution and drug delivery. In this work, isopropyl alcohol has been used as a solvent to obtain low dimensional calcium sulfate dihydrate crystals from calcium nitrate ‐ sulfuric acid system. Reactants in 0.5 molar concentration at ambient conditions generated uniform rod‐shaped crystals of length 3–5 µm. Analysis using X‐ray Diffractometry and Fourier Transform Infrared Spectrometry showed the material to be well crystallized, phase‐pure calcium sulfate dihydrate.The nucleation kinetics has been studied by observing the induction time of phase formation in solutions of millimolar concentrations through turbidimetry at 300 K. The data have been analysed using classical nucleation theory to deduce parameters like interfacial tension (or surface free energy), nucleation rate and critical radius. The surface free energy obtained (5.6 mJ/m2) is comparatively lower than that reported for aqueous precipitation, which could be attributed to the presence of isopropyl alcohol. On escalating the supersaturation ratio, the nucleation rate drastically increased and the critical radius decreased exponentially. Particles formed at supersaturation 1.39 showed a monomodal distribution centered at 8.2 nm in Dynamic Light Scattering analysis. Comparable particle sizes were obtained in Transmission Electron Microscopy.

A new bioactive calcium sulfate-based formulation (named 'BioCaS') has been developed for bone filler applications. This is a self-setting injectable cement where the preset form comprises bassanite obtained from the uniform submicron-sized precursor crystals of gypsum, modified with hydrogen orthophosphate ions. The results of the safety and efficacy evaluation of BioCaS cement, done as per the International Standards and guidelines, are presented in this paper. The study plan consisted of in vitro screening tests of cytotoxicity and haemolysis and in vivo biocompatibility evaluation, including an acute systemic toxicity test (in mice), an intracutaneous reactivity test (in rabbits), a pyrogen test (in rabbits) and a maximization sensitization test (in guinea pigs). The efficacy of the material in healing bone defects was investigated by implanting it in artificially created defects in rabbit femora, with clinically established hydroxyapatite porous ceramic as the control, followed by histological analysis at 12, 26 and 52 weeks. Set BioCaS cement consisted of hydrogen orthophosphate incorporating low-dimensional gypsum crystal lattices, the bioactivity of which has been identified by immersion in simulated body fluid. BioCaS was proved to be non-cytotoxic and non-haemolytic in the screening tests. In the live/dead assay, human osteoblast-like human osteosarcoma cells adhered well and spread on the surface of the material, attaining typical morphology and affirming the bone cell compatibility of the material. In the biocompatibility evaluation there were no acute systemic effects and the material proved non-pyrogenic. There was no intracutaneous erythemic or oedematous reactivity and no hypersensitivity observed in the Magnusson-Kligman method. The material satisfied the biocompatibility requirements. Bone implantation study revealed BioCaS to be osteoconductive and its efficacy of healing the experimental bone defects in rabbit femora is on a par with that of hydroxyapatite ceramic. The material resorbed at a pace matching that of new bone formation. This property of osteotransductivity will help the defect to heal and gain strength faster.

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A fusion welding technique to join a semi-solid processed A356 cast plate is explored using Gas Tungsten Arc Welding (GTAW). Semi-solid metal (SSM) billets of non-dendritic microstructure produced by rheocasting in a mould placed inside a linear electromagnetic stirrer were used for this study. GTAW experiments were conducted to simulate different thermal gradients near the fusion zone. The geometries of the weld pool as well as the temperature gradient in the fusion boundary were measured to understand the microstructure evolution. Simulation of the welding process was performed to aid in the analysis. Quantitative metallography provided the shape factor as a measure of globularity of the primary a-Al phase. Based on the studies, a model has been proposed to explain the observation of globular microstructure in the fusion zone of the welds. Conclusions show a positive correlation of thermal gradient with globular microstructure formation in this class of alloys.

Polyurethane potting compounds based on hexamethylene diisocyanate-trimethylol propane (HDI-TMP) adduct (Component "A") and polypropylene glycol, polyethylene glycol and castor oil (Component "B") were prepared as potential compounds for the fabrication of haemodialyzer. The setting characteristics of the potting compounds having isocyanate index 2.0 are better than those compounds having 1.35. The aging stability of PEG and PPG based potting compounds are poorer than those of castor oil based potting compounds. Appreciable hydrolytic, oxidative and chemical stability could be observed with castor oil based potting compounds of HDI-TMP adduct.

Polyurethane potting compounds based on multifunctional isocyanurate of aliphatic diisocyanate, hexamethylene diisocyanate (HDI-IC) as Component A and polypropylene glycol, polyethylene glycol and castor oil (Component B) were prepared as potential potting compounds for the fabrication of a haemodialyser. The setting characteristics of the potting compounds having isocyanate index 2.54 are better than those of the compounds having 1.77. The ageing stability of castor oil and PPG-based potting compounds having isocyanate index 2.54 is better than that of PEG oil-based potting compounds. Appreciable hydrolytic, oxidative and chemical stability could be observed with HDI-IC/PPG/2.54 potting compounds for development of haemodialyser, oxygenator, etc.