Influence of Storage Duration on Retention of Original Fracture Toughness

Accurate knowledge of bone properties is central in the prediction of failure and the development of injury treatment protocols. Often when bone properties are measured experimentally, bone specimens have to be chemically preserved prior to or during testing. Understanding the effect of the bone preservation method on the material properties is important. Degradation of properties due to preservation methods may lead to incorrect reporting of values of the bone properties. A salient question is, therefore, whether the preservation of bovine cortical bone in ethanol for extended periods of time affects fracture toughness; and if so, whether that affect is reversible. To answer these questions, a three-point bending test set-up was constructed to perform experiments over a period of 9 weeks. A total of 109 specimens of cortical bone of the same orientation were manufactured from the mid-diaphysis of the femur. These specimens were separated into three groups based on location in the femur; namely, medial, lateral, and posterior. The specimens were preserved in ethanol. At the end of each week, a sample of specimens was selected for testing, with the last sample tested after 9 weeks of preservation. It was shown that after 9 weeks of preservation in ethanol, followed by rehydration with physiological saline, the fracture toughness of the specimen was unchanged from that of the control specimen. Omission of rehydration in saline resulted in to an increased fracture toughness of up to 17%.     

Highly Regioselective Ring Opening of Epoxides with Thiols Catalyzed by SbCl3 Under Solvent-Free Conditions

The ring-opening reaction of epoxides with thiols by SbCl ₃ supported on Kieselguhr under solvent-free conditions, afforded high yields of β-hydroxy sulfides. Nucleophilic attack of the thiols occurs regioselectively at the less hindered side of the epoxides.     

Cup-shaped E,E-stilbenophane: synthesis,crystal structure and supramolecular chemistry

A new E,E-stilbenophane was synthesised and characterised. The crystal structure of this cyclophane shows that this molecule has a cup-shaped structure, which hosts a phenyl ring of neighbouring molecule as guest in its cavity with a π–π distance of about 3.7 Å. Moreover, the NMR spectra and theoretical analysis (gauge-independent atomic orbitals (GIAO) and quantum theory of atoms in molecules (QTAIM)) suggest that the silver recognition by E,E-stilbenophane host molecules is based on cation–π interactions in which the π-electrons of the double bonds play a major role.     

Acid‐induced homogenous liquid‐phase microextraction: Application of medium‐chain carboxylic acid as extraction phase

In this research, a novel homogeneous liquid‐phase microextraction method was successfully developed based on applying octanoic acid as low‐density extraction solvent. The method was applied for extraction and determination of chlorophenols (CPs) as model compounds. Twelve milliliter of the sample solution was poured into a home‐designed glass vial. Sixty microliter of octanoic acid was solved in water sample by adjusting pH and ionic strength. By rapid addition of 75 μL of concentrated HCl (6 M), a cloudy solution was obtained. Phase separation occurred at 5000 rpm for 5 min. After that, 20 μL of the collected phase (approximately 26 μL) was injected into the HPLC‐UV instrument for analysis. The effect of some parameters such as the volume of concentrated HCl (phase separation reagent), ionic strength, extraction time, centrifugation time, and the volume of extracting phase on the extraction efficiency of the CPs were investigated and optimized. The preconcentration factors in a range of 159–218 were obtained under the optimal conditions. The linear range, detection limits (S/N = 3), and precision (n = 3) were 1– 200, 0.3–0.5 μg/L, and 4.6–5.1%, respectively. Tap water, seawater, and river water samples were successfully analyzed for the existence of CPs using the proposed method and satisfactory results were obtained.     

Synthesis, spectroscopy, electrochemistry and thermal study of vanadyl tridentate Schiff base complexes: theoretical study of the structures of compounds by ab initio calculations

The VO(IV) complexes of tridentate ONN Schiff ligands were synthesized and characterized by IR, UV–Vis and elemental analysis. The electrochemical properties of the vanadyl complexes were investigated by cyclic voltammetry. A good correlation was observed between the oxidation potentials and the electron-withdrawing character of the substituents on the Schiff base ligands, showing the following trend: MeO < H < Br < NO₂. The thermogravimetry (TG) and differential thermoanalysis (DTA) of the VO(IV) complexes were carried out in the range of 20–700 °C. The VOL¹(OH₂) and VOL²(OH₂) decomposed in three steps, whereas the VOL³(OH₂) and VOL⁴(OH₂) complexes decomposed in two steps. The thermal decomposition of these complexes is closely related to the nature of the Schiff base ligands and proceeds via first-order kinetics. The structures of compounds were determined by ab initio calculations. The optimized molecular geometry and atomic charges were calculated using MP2 method with 6-31G(d) basis. The results suggested that, in the complexes, V(IV) ion is in square-pyramid N₂O₃ coordination geometry. Also the bond lengths and angles were studied and compared.     

Speciation Analysis of Cr(III) and Cr(VI) after Solid Phase Extraction Using Modified Magnetite Nanoparticles

A new solid phase extraction (SPE) method has been developed for the speciation of Cr(III) and Cr(VI). This method is based on the adsorption of Cr(VI) on modified alumina‐coated magnetite nanoparticles (ACMNPs). Total chromium in different samples was determined as Cr(VI) after oxidation of Cr(III) to Cr(VI) using H₂O₂. The chromium concentration has been determined by flame atomic absorption spectrometric (FAAS) technique and amount of Cr(III) was calculated by substracting the concentration of Cr(VI) from total chromium concentration. The effect of parameters such as pH, amount of adsorbent, contact time, sample volume, eluent type, H₂O₂ concentration and cetyltrimethylammonium bromide (CTAB) concentration as modifier on the quantitative recovery of Cr(VI) were investigated. Under the optimal experimental conditions, the preconcentration factor, detection limit, linear range and relative standard deviation (RSD) of Cr(VI) were 140 (for 350 mL of sample solution), 0.083 ng mL^?1, 0.1‐10.0 ng mL^?1 and 4.6% (for 5.0 ng mL^?1, n = 7), respectively. This method avoided the time‐consuming column‐passing process of loading large volume samples in traditional SPE through the rapid isolation of CTAB@ACMNPs with an adscititious magnet. The proposed method was successfully applied to the determination and speciation of chromium in different water and wastewater samples and suitable recoveries were obtained.     

Synthesize,Characterization and Application of Phosphine‐free Polymer Supported Palladium Nanoparticles as Effective Catalyst in Suzuki‐Miyaura Cross‐coupling Reactions

Heterogeneous catalysts were developed by supporting palladium nanoparticles on modified cross‐linked polyacrylamide and successfully applied in Suzuki‐Miyaura cross‐coupling reactions. These catalysts are stable to air and moisture, and no sign of metal leaching was detected during the reactions as judged by elemental analysis of palladium by ICP‐OES technique and hot filtration test, which demonstrates the heterogeneous character of the catalysts. High yields of desired products were resulted by using these phosphine‐free catalysts at temperatures below 80 °C without aid of any additional ligands. The heat stability of the catalysts at the operating temperature was confirmed by thermogravimetric analysis (TGA). These catalysts are easy to use and cost effective. They can be recovered from reaction mixture by a simple filtration and reused in more successive reactions without significant loss in activity. The catalyst activity was restored by an ultrasonication program after deactivation in 10 cycles.     

Efficient One‐Pot Four‐Component Synthesis and X‐ray Crystallographic Structure of 2‐Pyridone Derivatives

A series of 3‐cyano‐2‐pyridone derivatives were synthesized by one‐pot four‐component condensation reaction involving a benzaldehyde derivative, alkyl cyanoacetate, acyclic or cyclic ketones, and ammonium acetate in reflux condition. The X‐ray structure of the products 5a and 5d confirm symmetric dimers via hydrogen bonding interactions between individual pyridine molecules showing, in addition, also π–π stacking interactions.     

Characterization of pure phase Zn(II) oxide nanoparticles via thermal decomposition of two zinc(II) complexes of the 6,6′-dimethyl-2,2′-bipyridine ligand

Two zinc(II) complexes [Zn(6,6′-dimethyl-2,2′-bipy)Cl₂] _n (1) and [Zn(6,6′-dimethyl-2,2′-bipy)I₂] _n (2) are synthesized from the reaction of the 6,6′-dimethyl-2,2′-bipy ligand with ZnCl₂ and ZnI₂. Zinc(II) oxide nanoparticles are synthesized by the thermolysis of [Zn(6,6′-dimethyl-2,2′-bipy)Cl₂] _n (1) and [Zn(6,6′-dimethyl-2,2′-bipy)I₂] _n (2) at two different temperatures. The ZnO nanoparticles are characterized by X-ray diffraction and scanning electron microscopy (SEM). SEM images show the average size of the ZnO nanoparticles produced of 50 nm and 60 nm in compounds 1 and 2 respectively.