Relationship between shoulder pain and skin temperature measured by infrared thermography in a wheelchair propulsion test

IntroductionWheelchair Users (WCUs) depend on their upper extremities for their daily living. Therefore, it is not unusual to find that shoulder pain (SP) is a problem for WCUs and reduces their participation in sport and leisure activities.ObjectivesThe aims of this study were 1 – to analyse skin temperature measured by infrared thermography (IRT) before (pre-test), one minute after (post-test) and 10 min after (post-10) the kinematic wheelchair propulsion test (T-CIDIF) of athletic wheelchair users; 2 – to evaluate the relationship between shoulder pain (SP) and Skin Temperature Asymmetry (ΔT_sk) before and after (pre-test, post-test, post-10) the T-CIDIF, and to relate the SP with the kinematic variables of the T-CIDIF.Participants & interventions/procedureA volunteer sample of 12 wheelchair athletes completed an exercise test (T-CIDIF) in their own wheelchair. It consisted in a 30-s maximum test performed on two rollers. Two linear transducers connected to the rollers registered the number of propulsions, maximum and mean velocity and power of each arm. SP was assessed with the Wheelchair Users Shoulder Pain Index (WUSPI). Skin temperature (T_sk) of the anterior and posterior upper body was measured before and after the T-CIDIF by using an infrared camera. A total of 26 ROIs were evaluated with respect to the opposite side of the body to identify significant (ΔT_sk).Results/main outcome measure(s)Significant differences were observed between the T_sk of the post-10 and pre-test in 12 ROIs, and between the post-10 and the post-test in most of the ROIs. These differences are attenuated when the ΔT_sk is compared before and after exercise. T_sk tends to initially decrease immediately after the test and then significantly increase after 10 min of completing the T-CIDIF. The ΔT_sk vs SP analysis yielded significant inverse relationships (from r = −0.58 to r = −0.71, p < 0.05) in 5 of the 26 ROI. No significant correlations between propulsion variables and SP questionnaire were found. All T-CIDIF variables were significantly correlated with the temperature asymmetries in multiple ROIs (from r = −0.86 to r = −0.58, from p < 0.05 to p < 0.001).ConclusionsThese results present indications that high performance wheelchair athletes exhibit similar capacity of heat production than able-bodied. The thermographic data inversely correlates with the SP and the kinematic variables, but the last is not related to SP. This work contributes to improve the understanding about temperature changes in wheelchair athletes during exercise, and could be used to assess the efficacy of various sports and rehabilitation programs.     

Ultrasonic degradation of N-di and trihydroxy benzoyl chitosans and its effects on antioxidant activity

Modified chitosans with 3,4-dihydroxy benzoyl groups (CS-DHBA) and 3,4,5-trihydroxy benzoyl groups (CS-THBA) were synthesized and their chemical structures were determined by Fourier transform infrared (FT-IR) and ¹H nuclear magnetic resonance (¹H NMR) spectroscopy. Then, ultrasonic degradation of CS, CS-DHBA and CS-THBA in 1% acetic acid solution was investigated. The kinetics studies of degradation were followed by gel permeation chromatography (GPC). The results indicated that the weight-average molecular weight of chitosan decreased obviously after ultrasound treatment, but molecular weights of CS-DHBA and CS-THBA decreased slowly with increasing sonication time. Degradation kinetics model based on 1/M_t−1/M₀ = kt was used to estimate the degradation rate constant. It was found that the rates of degradation of CS-DHBA and CS-THBA are lower than CS, and follow the order: CS₄ > CS₈ > CS₁₂ > CS-THBA₄ > CS-THBA₈ ≈ CS-DHBA₄ > CS-THBA₁₂ > CS-DHBA₈ > CS-DHBA₁₂. The antioxidant activity of the CS, CS-DHBA and CS-THBA before and after sonication was investigated by the radical scavenging activity method using 1,1-diphenyl-2-picrylhydrazyl (DPPH). The DPPH scavenging free radical capacity of CS-THBA and CS-DHBA increased up to 89% and 74% respectively, when the concentration reached 6 μg/ml. The ultrasonic treatment of CS-DHBA and CS-THBA after 30 min decreased the DPPH free radical scavenging activity but ultrasonic treatment of CS increased the DPPH free radical scavenging activity.     

Adhesive As-S-Se-I immersion lenses for enhancing radiation characteristics of mid-IR LEDs operating in wide temperature range

The influence of As-S-Se-I chalcogenide glass lenses on the integral and spectral power and pattern of LED radiation has been shown. Simulation of the influence of the refractive index on the integral power for two lens shapes has been performed. The wettability and adhesion force of As-S-Se-I melt has been determined for several electronic engineering materials. Mechanical stresses between chalcogenide glass and adjacent diode body materials have been calculated for −100 to 53 °C temperature range. Stability of the immersion lenses against cracking has been experimentally investigated for −150 to 53 °C temperature range.     

Linear energy transfer dependence of Al2O3:C optically stimulated luminescence detectors exposed to therapeutic proton beams

Currently, there are no radiation detectors that can be used for routine measurements of linear energy transfer (LET) in particle therapy clinics. In this work, we characterized the LET dependence of Al₂O₃:C optically stimulated luminescence (OSL) detectors (OSLDs) exposed to therapeutic proton beams in order to evaluate their potential for clinical LET measurements. We evaluated OSLDs that were irradiated with an absorbed dose to water of 0.2 Gy in therapeutic proton beams with average energies ranging between approximately 25 MeV and 200 MeV, resulting in LET in water values between 0.45 and 2.29 keV/μm. We examined two properties of the OSL emission signal in terms of LET dependence: the signal intensities of the blue and ultraviolet (UV) emission bands, and the shapes of the OSL curves. We found that the signal intensity of the UV emission band increased consistently with LET within the range investigated, whereas the intensity of the blue emission band remained constant. Our results also demonstrated that the OSL curve shapes were more LET dependent for signals containing both the blue and UV emission bands than for signals containing only one of the bands. Both metrics we examined in this study – the relative UV/blue emission signal intensities and OSL curve shapes – show potential for LET detection in proton therapy.     

Surfactant-free coating of thiols on gold nanoparticles using sonochemistry: A study of competing processes

A method for the surfactant-free coating of gold nanoparticles with thiols using sonochemistry is presented. The gold nanoparticles were prepared by a modified Zsigmondy method, affording good control over the particle-size distribution, and the thiol coating was performed by the sonication of a biphasic system consisting of a nanoparticle suspension in water and thiols in toluene. The effects of two important reaction parameters on the particle morphology, viz. sonication time and thiol concentration, were investigated in detail using transmission electron microscopy. The effect of the thiol chain length was also studied. We show that the morphology of the coated particles is determined through a competition between two opposing effects: particle fusion, due to the sonication conditions, and digestive ripening, due to the action of the thiols. Additionally, we illustrate the utility of our technique for various applications, including surface-enhanced Raman scattering from bound molecules, and further functionalization using a thiol-exchange reaction. Our technique paves the way for an efficient synthesis of thiol-coated AuNPs of different shapes and sizes, suitable for a range of diverse applications.     

Morphologically controlled preparation of CuO nanostructures under ultrasound irradiation and their evaluation as pseudocapacitor materials

Various morphologies of copper oxide (CuO) nanostructures have been synthesized by controlling the reaction parameters in a sonochemical assisted method without using any templates or surfactants. The effect of reaction parameters including molar ratio of the reactants, reaction temperature, ultrasound exposure time, and annealing temperature on the composition and morphology of the product(s) has been investigated. The prepared samples have been characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDAX), and thermogravimetric analysis (TGA). It has been found that Cu₂(OH)₃NO₃ nanoplatelets are achieved in mild conditions which can be then converted to various morphologies of CuO nanostructures by either using high concentrations of OH⁻ (formation of nanorods), prolonging sonication irradiation (nanoparticles), or thermal treatment (nanospheres). Application of the prepared CuO nanostructures was evaluated as supercapacitive material in 1 M Na₂SO₄ solution using cyclic voltammetry (CV) in different potential scan rates ranging from 5 to 100 mV s⁻¹. The specific capacitance has been calculated using CV curves. It has been found that the pseudocapacitor performance of CuO can be tuned via employing morphologically controlled samples. Accordingly, the prolonged sonicated sample (nanoparticles) showed the high specific capacitance of 158 F.g⁻¹.     

Fabrication of Cu2O nanocrystalline thin films photosensor prepared by RF sputtering technique

Cuprous oxide (Cu₂O) nanocrystalline thin films were prepared on two types of substrates known as crystalline silicon and amorphous glass, by radio frequency reactive magnetron sputtering method. Scanning electron microscopy images confirmed that Cu₂O particles covered the entire surface of both substrates with smoothing distribution. The root mean square surface roughness for the prepared Cu₂O thin films on glass and Si (111) substrates is 4.16, and 3.36 nm, respectively. Meanwhile, X-ray diffraction results demonstrated that the two phases of Cu₂O and CuO were produced on Si (111) and glass substrates. The optical bandgap of Cu₂O thin films synthesised on glass substrate is 2.42 eV. Furthermore, the prepared Cu₂O nanocrystalline thin films have showed low reflectance value in the visible spectrum. Metal-Semiconductor-Metal photodetector based Cu₂O nanocrystalline thin films deposited onto Si (111) was fabricated using aluminium and platinum, with the current-voltage and photoresponse characteristic investigated under various applied bias voltages. The fabricated Metal-Semiconductor-Metal (M-S-M) photodetector had shown 126% sensitivity in the presence of 10 mW/cm² of 490 nm light with 1.0 V bias, displaying 90 and 100 ms response and recovery times, respectively. These findings have demonstrated the suitability of M-S-M Cu₂O photodetector as an affordable photosensor in the future.     

Tuning magnetic fingerprints of FeNi nanowire arrays by varying length and diameter

Magnetic nanowires (NWs) electrodeposited into solid templates are of high interest due to their tunable properties which are required for magnetic recording media and spintronic devices. Here, highly ordered arrays of FeNi NWs with varied lengths (ranging from 2.5 to 12 μm) and diameters (between 45 and 75 nm) were fabricated into anodic aluminum oxide templates using a pulsed ac electrodeposition technique. X-ray diffraction patterns along with energy dispersive spectroscopy indicated the formation of Fe₇₀Ni₃₀ NWs with fcc and bcc alloy phases, being highly textured along the bcc [110] direction. Magnetic properties were studied by hysteresis loop measurements at room temperature and they showed reductions in coercivity and squareness values by increasing length and diameter. Further, magnetic fingerprints of the NWs were characterized using the first-order reversal curve (FORC) analysis. FORC measurements revealed that, with increasing length and diameter from 2.5 to 10 μm and 45–55 nm, respectively, besides an increase in inter-wire magnetostatic interactions, a transition from a single domain (SD) state to a pseudo SD state occurred. Moreover, a multi-domain (MD) state was found for the longest length and diameter. While the irreversible magnetization component of the SD NWs was approximately 100%, the reversible component of MD NWs increased up to 20%.     

Sonochemical synthesis of a new nano-sized cerium(III) supramolecular compound; Precursor for nanoceria

Using a sonochemical method, nanoparticles of a new Ce(III) supramolecular compound, (NAMH⁺)₂[Ce₄(pydc)₆(pydcH)₂(H₂O)₈]·8H₂O (1), (H₂pydc = 2,6-pyridinedicarboxylic acid, NAM = nicotinamide), have been synthesized. Compound 1 was characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), FT-IR spectroscopy and elemental analyses, and its structure was determined by X-ray crystallography. It has been revealed that its structure consists of tetra-nuclear building units that extend to a 3D supramolecular network via non-covalent interactions mainly hydrogen bonding. The thermal stability of complex 1 both for its crystals and nanostructures has been studied by the thermal gravimetric (TG) method and compared with each other. The role of ultrasound irradiation power and the concentration of initial reactants on the size and morphology of the nano-structured complex 1, has been investigated. Ceria nanoparticles were obtained upon the calcination of complex 1 at 800 °C under atmospheric air. Furthermore, the fluorescent properties of complex 1 at room temperature were studied.     

Synthesis and characterization of a new nano lead(II) 0-D coordination supramolecular compound: A precursor to produce pure phase nano-sized lead(II) oxide

Nano-structure of a new 0D Pb(II) coordination supramolecular compound, [Pb₄(8-Quin)₆](ClO₄)₂(1), L = 8-HQuin = 8-hydroxyquinolin ligand has been synthesized by use of a sonochemical process and characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), Fourier transform infrared spectroscopy (FTIR) and elemental analyses. The structure of compound 1 was determined by single-crystal X-ray diffraction. The single crystal X-ray data of compound 1 implies that the Pb⁺² ions are five coordinated. Each lead atom is coordinated to nitrogen and oxygen atoms of 8-hydroxyquinolin ligand. Topological analysis shows that the compound 1 is 1,2,3,4,4M12-1net. Nanoparticles of lead(II) oxide have been prepared by calcination of lead(II) coordination polymer at 500 °C that were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD) and IR spectroscopy.     

Tracing nanoparticles and photosensitizing molecules at transmission electron microscopy by diaminobenzidine photo-oxidation

During the last three decades, diaminobenzidine photo-oxidation has been applied in a variety of studies to correlate light and electron microscopy. Actually, when a fluorophore is excited by light, it can induce the oxidation of diaminobenzidine into an electron-dense osmiophilic product, which precipitates in close proximity to the fluorophore, thereby allowing its ultrastructural detection. This method has very recently been developed for two innovative applications: tracking the fate of fluorescently labeled nanoparticles in single cells, and detecting the subcellular location of photo-active molecules suitable for photodynamic therapy. These studies established that the cytochemical procedures exploiting diaminobenzidine photo-oxidation represent a reliable tool for detecting, inside the cells, with high sensitivity fluorescing molecules. These procedures are trustworthy even if the fluorescing molecules are present in very low amounts, either inside membrane-bounded organelles, or at the surface of the plasma membrane, or free in the cytosol. In particular, diaminobenzidine photo-oxidation allowed elucidating the mechanisms responsible for nanoparticles internalization in neuronal cells and for their escape from lysosomal degradation. As for the photo-active molecules, their subcellular distribution at the ultrastructural level provided direct evidence for the lethal multiorganelle photo-damage occurring after cell photo-sensitization. In addition, DAB photo-oxidized samples are suitable for the ultrastructural detection of organelle-specific molecules by post-embedding gold immunolabeling.     

Dosimetric comparison of water phantoms,ion chambers,and data acquisition modes for LINAC characterization

PurposeIn this study a dosimetric comparison utilizing continuous data acquisition and discrete data acquisition is examined using IBA Blue Phantom (IBA Dosimetry, Schwarzenbruck, Germany) and PTW (PTW, Freiberg, Germany) MP3-M water tanks. The tanks were compared according to several factors including set up time, ease of use, and data acquisition times. A tertiary objective is to study the response of several ionization chambers in the two tanks examined.MethodsMeasurements made using a Varian 23EX LINAC (Varian Medical Systems, Palo Alto, CA) include PDDs and beam profiles for various field sizes with IBA CC13, PTW Semiflex 31010, PTW Pinpoint N31016, and PTW 31013 ion chambers for photons (6, 18 MV) and electrons (6, 9, 12, 15, and 18 MeV). Radial and transverse profile scans were done at depths of maximum dose, 5 cm, 10 cm, and 20 cm using the same set of tanks and detectors for the photon beams. Radial and transverse profile scans were done at depth of maximum dose for the electron beams on the same tanks and chambers. Data processing and analysis was performed using PTW's MEPHYSTO Navigator software and IBA's OmniPro Accept version 6.6 for the respective water tank systems.ResultsPDD values agree to within 1% and dmax to within 1 mm for the PTW MP3-M tank using PTW 31010 and Blue Phantom using IBA CC13 chamber, respectively and larger discrepancy with the PTW PinPoint N31016 chamber at 6 MV. With respect to setup time the PTW MP3-M and IBA Blue phantom tank took about 20 and 40 min, respectively. Scan times were longer by 5–15 min per field size in the PTW MP3-M tank for the square field sizes from 1 cm to 40 cm as compared to the IBA Blue phantom. However, data processing times were higher by 7 min per field size with the IBA system.ConclusionsTank measurements showed little deviation with the higher energy photons as compared to the lower energy photons with regards to the PDD measurements. Chamber construction as well as tank set up may be causing the slight deviation in data. It is important to identify the exact source of the potential errors to ensure that proper tank usage is performed when making such measurements to ensure that patient safety is in compliance. Beam profiles done with different chambers and tanks showed little to no deviation from one to another. With regards to continuous versus discrete data measurements the main difference was in the data processing technique used. Discrete data obtained required less data processing as compared to the continuous data acquired.     

Effect of spectrum processing procedure on the linearity of EPR dose reconstruction in tooth enamel

Electron Paramagnetic Resonance (EPR) spectroscopy with tooth enamel is a widely used method of dosimetry. The accuracy of EPR tooth dosimetry depends on the spectrum processing procedure, the quality of which, in its turn, relies on instrumental noise and the signals from impurities. This is especially important in low-dose evaluation. The current paper suggests a method to estimate the accuracy of a specific spectrum processing procedure. The method is based on reconstruction of the radiation-induced signal (RIS) from a simulated spectrum with known RIS intensity. The Monte Carlo method was used for the simulations. The model of impurity and noise signals represents a composite residual spectrum (CRS) obtained by subtraction of the reconstructed RIS and the native background signal (BGS) from enamel spectra measured in HMGU (Neuherberg, Germany) and IMP (Yekaterinburg, Russia). The simulated spectra were deconvoluted using a standard procedure. The method provides an opportunity to compare the simulated “true” RIS with reconstructed values. Two modifications of the EPR method were considered: namely, with and without the use of the reference Mn²⁺ signals. It was observed that the spectrum processing procedure induces a nonlinear dose response of the reconstructed EPR amplitude when the height of the true RIS is comparable with the amplitudes of noise-like random splashes of CRS. The area of nonlinearity is below the limit of detection (DL). The use of reference Mn²⁺ signals can reduce the range of nonlinearity. However, the impact of the intensities of CRS random signals on nonlinearity is two times higher than the one observed when the reference signals were not used. The reproducibility of the software response is also dependent on both the amplitude of the CRS and the use of a reference signal, and it is also two times more sensitive to the amplitude of the CRS. In most EPR studies, all of the data are used, even those for which the dose value is lower than the DL. This study shows that low doses evaluated with the help of linear dose–response can be significantly overestimated. It is recommended that linear dose response calibration curves be constructed using only data above the DL. Data below the DL should be interpreted cautiously.     

Syntheses and structural characterization of two new nanostructured Bi(III) supramolecular polymers via sonochemical method

Two new bismuth(III) coordination supramolecular polymers, {[Bi₂(Hbpp)(bpp)(μ-I)₂I₆](Hbpp)·MeOH}_n (1) and [Bi(Hbpp)(Br₄)] (2), (bpp = 1,3-di(pyridin-4-yl)propane) were prepared and were structurally characterized by single crystal X-ray diffraction. Single crystalline one-dimensional materials were prepared using a heat gradient applied a solution of the reagents using the branched tube method. The structural determination by single crystal X-ray crystallography shows that compounds 1 and 2 form monoclinic polymers with symmetry space group P2₁ in the solid state. These new nanostructured Bi(III) supramolecular compounds, {[Bi₂(Hbpp)(bpp)(μ-I)₂I₆](Hbpp)·MeOH} (1) and [Bi(Hbpp)(Br₄)] (2), were also synthesized by sonochemical method. The nanostructures were characterized by Field Emission-scanning electron microscopy (FE-SEM), powder X-ray diffraction (PXRD) and IR spectroscopy.     

Sonochemical syntheses of a new fibrous-like nano-scale manganese(II) coordination supramolecular compound; precursor for the fabrication of octahedral-like Mn3O4 nano-structure

Nanoparticles of a new three-dimensional Mn(II) coordination supramolecular compound, [Mn(L)₂(H₂O)₂] (1), (L⁻ = 1H-1,2,4-triazole-3-carboxylate), have been synthesized by a sonochemical process and characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), FT-IR spectroscopy and elemental analyses. Structural determination of compound 1 reveals the Mn(II) ion is six coordinated, bonded to two nitrogen atoms, two oxygen atoms from the L⁻ ligand and two water molecules. The thermal stability of compound 1 both its bulk and nano-size has been studied by thermal gravimetric (TG) and differential thermal analyses (DTA) and compared each other. Concentration of initial reagents effects on size and morphology of nano-structured compound 1, have been studied and shows that low concentrations of initial reagents decreased particles size and also leaded to fibrous-like nanostructures morphology. Mn₃O₄ nano-structure with an octahedral-like morphology were simply synthesized by solid-state transformation of compound 1 at 650 °C.     

Sonochemical synthesis of nanoscale mixed-ligands lead(II) coordination polymers as precursors for preparation of Pb2(SO4)O and PbO nanoparticles; thermal,structural and X-ray powder diffraction studies

Nano-structures of two new Pb(II) two-dimensional coordination polymers, [Pb(μ-4-pyc)(μ-NCS)(μ-H₂O)]_n (1) and [Pb(μ-4-pyc)(μ-N₃)(μ-H₂O)]_n (2), 4-Hpyc = 4-pyridinecarboxylic acid were synthesized by a sonochemical method. The new nano-structures were characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. Compounds 1 and 2 were structurally characterized by single crystal X-ray diffraction and consist of two-dimensional polymeric units. The thermal stability of compounds 1 and 2 were studied by thermal gravimetric and differential thermal analyses and compared. Pb₂(SO₄)O and PbO nanoparticles were obtained by calcination of the nano-structures of compounds 1 and 2 at 600 °C, respectively.     

A general method for preparing lanthanide oxide nanoparticles via thermal decomposition of lanthanide(III) complexes with 1-hydroxy-2-naphthoic acid and hydrazine ligands

Six new lanthanide(III) complexes (i.e., [Ln(L)₂(NA)_1.5]·3H₂O, where Ln=La(III), Pr(III), Nd(III), Sm(III), Gd(III), and Ce(III) and L and NA indicate N₂H₄ and C₁₀H₆(1-O)(2-COO), respectively) with 1-hydroxy-2-naphthoic acid [C₁₀H₆(1-O)(2-COOH)] and hydrazine (N₂H₄) as co-ligands were characterized by elemental, FTIR, UV-visible, and XRD techniques. In the FT-IR spectra, the N-N stretching frequency in the range of 981–949 cm⁻¹ demonstrates evidence of the presence of coordinated N₂H₄, indicating the bidentate bridging nature of hydrazine in the complexes. These complexes show symmetric and asymmetric COO⁻ stretching from 1444 to 1441 cm⁻¹ and 1582 to 1557 cm⁻¹, respectively, indicating bidentate coordination. TG-DTA studies revealed that the compounds underwent endothermic dehydration from 98 to 110 °C. This was followed by the exothermic decomposition of oxalate intermediates to yield the respective metal oxides as the end products. From SEM images, the average size of the metal oxide particles prepared by thermal decomposition of the complexes was determined to be 39–42 nm. The powder X-ray and SEM coupled with energy dispersive X-ray (EDX) studies revealed the presence of the respective nano-sized metal oxides. The kinetic parameters of the decomposition of the complexes were calculated using the Coats-Redfern equation.     

Sonochemical syntheses of binuclear lead(II)-azido supramolecule with ligand 3,4,7,8-tetramethyl-1,10-phenanthroline as precursor for preparation of lead(II) oxide nanoparticles

The new neutral binuclear lead(II) azido coordination compound, [Pb₂(tmph)₂(μ-N₃)₂(CH₃COO)₂] (1) [tmph = 3,4,7,8-tetramethyl-1,10-phenanthroline], has been synthesized by a sonochemical method. Single crystal X-ray structure shows that the overall structure of 1 is binuclear unit. Complex 1 has a bridging azido pathway, end-to-end bridging azides between a pair of lead(II) centers. This is further extended into a one-dimensional (1D) and three-dimensional (3D) supramolecular structure by Pb⋯C and π–π weak directional intermolecular interactions. The coordination number of lead(II) ions is seven, PbN₄O₃, with two N-donor atoms from tmph ligands and three O-donors from acetate anions and two N-donors from two azide anions. It has a “stereo-chemically active” electron lone pair, and the coordination sphere is hemidirected. The PbO nanoparticles were obtained by thermolysis of 1 at 180 °C with oleic acid as a surfactant. The morphology and size of the prepared PbO samples were further observed using scanning electron microscopy (SEM).     

Effect of two sonochemical procedures on achieving to different morphologies of lead(II) coordination polymer nano-structures

Micro and nano-structures of a lead(II) coordination polymer, [Pb₂(2-Me-8-Hq)₂(MeOH)₂]_n (1), [2-Me-8-HqH = 2-methyl-8-hydroxyquinoline]_, were synthesized by two sonochemical methods. These new micro and nano-structures were characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. Compound 1 was structurally characterized by single-crystal X-ray diffraction and consists of primary dimeric unit of [Pb₂(2-Me-8-Hq)₂(MeOH)₂]. Self assembly between the dimmeric units of [Pb₂(2-Me-8-Hq)₂(MeOH)₂] from Pb-O bonds results in formation of a one-dimensional lead(II) coordination polymer. The Pb^II-ion in compound 1 has PbO₆N₁ coordination sphere with a stereo-chemically ‘active’ electron lone pair on the metals. By a reversible solid-state structural transformation, we successfully prepared [Pb₂(2-Me-8-Hq)₂]_n (2) by thermal desolvation of 1. Thermal stability of compound 1 was studied by thermo gravimetric and differential thermal analyses. In addition nano-structure of PbO was prepared from calcination process of compound 1 at 873 K.