Determination of trace metallic impurities in high-purity quartz by ion chromatography

A method has been developed for the determination of relevant trace impurities (alkali, alkaline and transition metals) in high purity quartz by ion-chromatography. In situ reagent (HF) purification and simultaneous sample dissolution was achieved in a multichannel vapour phase digestion assembly. Twenty-one samples can be digested at a time in this vapour phase system. Significant decrease in the process blank levels for all the analytes was observed. Drastic reduction (250 times) of NH4+ blank was achieved in the described vapour phase digestion, which enables the determination of trace concentration of sodium in high purity quartz. After volatilisation of the matrix and unreacted HF, the clear water leached solutions were injected into an ion-chromatograph equipped with conductivity detector for the determination of alkali and alkaline earth metals. In the case of transition metals, the trace residues were leached with 10 mM HCl and after separation on a mixed bed analytical column (IonPac CS5) were detected by spectrophotometry after post column derivatisation using 4-(2-pyridylazo)resorcinol (PAR). The accuracy of the result was checked by their comparison with those obtained by independent methods like inductively coupled plasma (ICP) MS and ICP atomic emission spectrometry. The achievable detection limits are between 0.4 ng/g (Li) and 22 ng/g (Mn). The application of the method to the determination of the above trace metals in two high-purity-grade quartz samples is demonstrated.     

Pyrolysis studies of aromatic polyesters

The products of pyrolysis, at 400°C in vacuo (1 Pa), of poly(ethyleneterephthalate) (PET) and poly(butyleneterephthalate) (PBT) were studied. The products were identified by gas chromatography/mass spectrometry technique. The highly volatile products of PET contained acetaldehyde, benzene, toluene, styrene and ethylbenzene and in the case of PBT, butadiene, tetrahydrofuran, vinylcyclohexene and ethylbenzene were the major products. A qualitative analysis of the products of low volatility revealed that the main components were benzoic acid, terephthalic acid, monovinyl esters of terephthalic acid and higher oligomers in the case of PET, whereas benzoic acid, monobutenyl esters of terephthalic acid and higher oligomers were the main products from PBT. The results obtained were in good agreement with those obtained from pyrolysis experiments, carried out directly in the mass spectrometer. Mechanisms to explain the occurrence of the different products are proposed.     

A Hybrid RF and Vision Aware Fusion Scheme for Multi-Sensor Wireless Capsule Endoscopic Localization

A huge torrent of data traffic is generated from various heterogeneous applications and services at the Internet backbone. In general, at the backbone, all such applications and services are allocated spectral resources under a shared spectrum environment within elastic optical networks (EONs). In such a fully shared environment, connection requests (CRs) belonging to different traffic profiles compete for spectral resources. Hence, it is very challenging for network operators to resolve resource conflict that occur at the time of provisioning resources to such CRs. The heterogeneous traffic profile (HTP) considered in this work includes permanent lightpath demands (PLDs) and scheduled lightpath demands (SLDs). We propose various distance adaptive routing and spectrum assignment (DA-RSA) heuristics to resolve resource conflict among these two traffic profiles in EONs under a full sharing environment. Conventionally, preemption was the only technique to resolve such resource conflict among HTPs. Since preemption involves the overhead of selecting CRs to be preempted and then deallocating the resources given to those CRs, excessive preemption adversely affects the performance of the network. Therefore, in this work, we utilized bandwidth splitting as a solution to resolve resource conflict among HTPs under such a shared environment in EONs. Moreover, an integrated solution consisting of splitting and preemption is also proposed. We refer to this new integration as flow-based preemption. Our simulation results demonstrate that bandwidth splitting-based heuristics yield significant improvement in terms of the amount of bandwidth accepted in the network, link and node utilization ratio, number of transponders utilized and the amount of bandwidth dropped due to preemption. Moreover, the flow-based preemption approach is proved to be superior in performance amongst all proposed strategies.

     

Encrypted Network Traffic Classification and Resource Allocation with Deep Learning in Software Defined Network

Wireless Personal Communications - The climate has changed absolutely in every area in just a few years as digitized, making high-speed internet service a significant need in the future. Future...     

Organometallic L-Alanine Cadmium Iodide Crystals for Optical Device Fabrication

Single crystals of L-alanine cadmium iodide (LACI) were grown by the slow evaporation technique at room temperature. A single-crystal X-ray diffraction (SXRD) model was used to evaluate the crystal structure of the as-grown LACI crystal. The energy dispersive X-ray (EDX) analysis and ultraviolet-visible-near infrared (UV-vis-NIR) transmittance studies were carried out, and the results reveal the presence of elements in the title compound. From the transmittance data, the optical bandgap as a function of photon energy was estimated, and the different optical constants were calculated. A fluorescence study was performed for the LACI crystal. Thermogravimetric and differential thermal analyses have also been studied to investigate the thermal property of the LACI crystal. The efficiency of the second harmonic generation (SHG) of the title crystal was investigated. The magnetic and electrical properties were estimated by the vibrating sample magnetometer (VSM) analysis and impedance study, respectively.     

Procedure for determination of trace ions in boric acid by matrix volatilization-ion chromatography

A method for determination of anions and cations in boric acid is proposed by matrix volatilization. The boric acid matrix was eliminated as trimethyl borate ester in a vapour phase matrix elimination (VPME) system using a mixture of glycerol-methanol. In this VPME system, in situ reagent purification, sample decomposition and digest evaporation were achieved in a single step. Trace anions were separated on anion-exchange column (IonPac AS17) by an isocratic elution with 15 mM sodium hydroxide and the cations on a cation-exchange column (IonPac CS12) by 20 mM hydrochloric acid as eluents. Method detection limits (3sigma) for most ions ranged from 0.3 to 8 ng/g (ppb). Recovery experiments combined with comparison of data obtained by other methods were employed to verify the accuracy of the proposed method. Application of the method to determine trace levels of anions like acetate, oxalate, sulfate, phosphate and cations such as lithium, sodium, potassium, magnesium and calcium in two highly pure grades of boric acid using ion chromatography is demonstrated.     

Parallel algorithm for the computation of characteristic polynomials of chemical graphs

A parallel algorithm is developed for the first time based on Frame's method to compute the characteristic polynomials of chemical graphs. This algorithm can handle all types of graphs: ordinary, weighted, directed, and signed. Our algorithm takes only linear time in the CRCW PRAM model with O(n³) processors whereas the sequential algorithm takes O(n⁴) time. Especially when the number of vertices of the graph is large this method will be more efficient than the recently developed vectorized Frame and Givens–Householder methods.     

Some aspects of tailoring flame retardancy in HET-acid-based flame retardants

HET acid was condensed with either ethylene glycol or 1,4-butanediol to yield the respective oligoesters. These oligoesters were characterized by molecular weight, measured by vapor-pressure osmometry. The degradation mechanism of oligoesters of HET acid with either ethylene glycol or 1,4-butanediol was elucidated. The thermal properties of these polyesters were studied using differential thermal analysis and thermal volatilization analysis. The mechanism of degradation was proposed on the basis of pyrolysis–gas chromatography studies, the degradation products being subsequently identified by mass spectrometry. It turned out that in the course of decomposition, hexachlorocyclopentadiene was formed, which is believed to be the active substance for flame retardance in these systems. The aspect of tailoring flame retardancy by changing the chemical environment, i.e., by using different diols, is discussed.     

Effects of soluble surfactants on the deformation and breakup of stretching liquid bridges

Surfactants are routinely used to control the breakup of drops and jets in many applications such as inkjet printing, crop spraying, and DNA or protein microarraying. The breakup of surfactant-free drops and jets has been extensively studied. By contrast, little is known about the closely related problem of interface rupture when surfactants are present. Solutions of a nonionic surfactant, pentaethylene glycol monododecyl ether, or C12E5, in water and in 90 wt % glycerol/water are used to show the effects of surfactant and viscosity on the deformation and breakup dynamics of stretching liquid bridges. Equilibrium surface tensions for both solutions can be fitted with the Langmuir-Szyskowski equation. All experiments have been done at 24 degrees C. The critical micelle concentrations for C12E5 are 0.04 and 0.4 mM in water and the glycerol/water solution, respectively. With high-speed imaging, the dynamic shapes of bridges held captive between two rods of 3.15 mm diameter are captured and analyzed with a time resolution of 0.1-1 ms. The bridge lengths are 3.15 mm initially and about 5-7 mm at pinch-off. Breakup occurs after stretching for about 0.2-0.3 s, depending on the solution viscosity and the surfactant concentration. When the liquid bridges break up, the volume of the sessile drop left on the bottom rod is about 3 times larger than that of the pendant drop left on the top rod. This asymmetry is due to gravity and is influenced by the equilibrium surface tensions. Surfactant-containing low-viscosity water bridges are shown to break up faster than surfactant-free ones because of the effect of gravity. With or without surfactant, water bridges form satellite drops. Surfactant-containing high-viscosity glycerol/water bridges break up more slowly than surfactant-free ones because of strong viscous effects. Moreover, the shapes of the sessile drops close to breakup exhibit a "pear-like" tip; whether a satellite forms depends on the surface age of the bridge before stretching commences. These unexpected effects arising from the addition of surfactants are due to the capillary pressure reduction and Marangoni flows linked to dynamic surface tension.     

Experimental Evidence for the Incorporation of Two Metals at Equivalent Lattice Positions in Mixed-Metal Metal–Organic Frameworks

Metal–organic frameworks containing multiple metals distributed over crystallographically equivalent framework positions (mixed-metal MOFs) represent an interesting class of materials, since the close vicinity of isolated metal centers often gives rise to synergistic effects. However, appropriate characterization techniques for detailed investigations of these mixed-metal metal–organic framework materials, particularly addressing the distribution of metals within the lattice, are rarely available. The synthesis of mixed-metal FeCuBTC materials in direct syntheses proved to be difficult and only a thorough characterization using various techniques, like powder X-ray diffraction, X-ray absorption spectroscopy and electron paramagnetic resonance spectroscopy, unambiguously evidenced the formation of a mixed-metal FeCuBTC material with HKUST-1 structure, which contained bimetallic Fe−Cu paddlewheels as well as monometallic Cu−Cu and Fe−Fe units under optimized synthesis conditions. The in-depth characterization showed that other synthetic procedures led to impurities, which contained the majority of the applied iron and were impossible or difficult to identify using solely standard characterization techniques. Therefore, this study shows the necessity to characterize mixed-metal MOFs extensively to unambiguously prove the incorporation of both metals at the desired positions. The controlled positioning of metal centers in mixed-metal metal–organic framework materials and the thorough characterization thereof is particularly important to derive structure–property or structure–activity correlations.