铝土矿中微量镓的分析方法进展

综述了近几年国内铝土矿中镓分析方法的研究进展,叙述了用于微量镓分析测定的光度法、伏安法、原子吸收光谱法、电感耦合等离子体-原子发射光谱法、电感耦合等离子体-质谱法、X射线荧光光谱法等分析方法,对方法的优缺点进行了评述,并对今后微量镓分析测定方法进行了展望.     

Radiolabeled Nanogels for Nuclear Molecular Imaging

An efficient and simple synthesis approach to form stable ⁶⁸Ga‐labeled nanogels is reported and their fundamental properties investigated. Nanogels are obtained by self‐assembly of amphiphilic statistical prepolymers derivatised with chelating groups for radiometals. The resulting nanogels exhibit a well‐defined spherical shape with a diameter of 290 ± 50 nm. The radionuclide ⁶⁸Ga is chelated in high radiochemical yields in an aqueous medium at room temperature. The phagocytosis assay demonstrates a highly increased internalization of nanogels by activated macrophages. Access to these ⁶⁸Ga‐nanogels will allow the investigation of general behavior and clearance pathways of nanogels in vivo by nuclear molecular imaging.

     

The Electronic and Infrared Absorption Spectra of Toluene-d

Abstract

The infrared and ultraviolet absorption spectra of toluene-d have been investigated for the first time in the regions 400 - 4000 cm^?1 and 2350 ?2750 A° respectively. The intense band at 2666.3 A°(37494 cm^?1) in the u.v. vapour absorption spectrum has been identified as the o,o band and others have been interpreted in terms of the three (519,632 and 785 cm^?1) ground state and the six (454,526,743,935,963 and 1180 cm^?1 excited state fundamentals. The correlation of the various frequencies of the ground and excited states of toluene and toluene-d has been done. The observed isotopic shift for toluene-d is 14 cm^?1.     

Multicomponental Fluorimetric Determination of Aluminium, Gallium and Indium

For the fast characteristics of mixtures of Aluminium, Gallium and Indium the fluorimetric evaluation in the form of complexes with 8-Hydroxyquinoline-5-sulphonic acid is described at selected pH. The highly collinear correlated fluorescent spectra and their first derivation were evaluated under various experimental conditions with the Multiple Linear Regression (MLR), Partial Least Squares (PLS) methods and Kalman filtering. When comparing the results, the PLS gives the least relative prediction errors under optimal conditions, 5.6–15.9% for the concentration range of Al 0.025–0.2 μg cm⁻³, Ga 0.1–0.8 μg cm⁻³ and In 0.1–0.8 μg cm⁻³ in the mixture.     

New Ga/N‐based Active Lewis Pairs,Trifunctional Ga–Ga Compounds,Reactions with Cyanamide and Dual Insertion of Isocyanate

Hydrogallation of Me₃Si–C≡C–NR'₂ with R₂Ga–H (R = tBu, CH₂tBu, iBu) yielded Ga/N‐based active Lewis pairs, R₂Ga–C(SiMe₃)=C(H)–NR'₂ ( 7 ). The Ga and N atoms adopt cis‐positions at the C=C bonds and show weak Ga–N interactions. tBu₂GaH and Me₃Si–C≡C–N(C₂H₄)₂NMe afforded under exposure of daylight the trifunctional digallium(II) compound [MeN(C₂H₄)₂N](H)C=C(SiMe₃)Ga(tBu)–Ga(tBu)C(SiMe₃)=C(H)[N(C₂H₄)₂NMe] ( 8 ), which results from elimination of isobutene and H₂ and Ga–Ga bond formation. 8 was selectively obtained from the ynamine and [tBu(H)Ga–Ga(H)tBu]₂[HGatBu₂]₂. 7a (R = tBu; NR'₂ = 2,6‐Me₂NC₅H₈) and H₈C₄N–C≡N afforded the adduct tBu₂Ga‐C(SiMe₃)=C(H)(2,6‐Me₂NC₅H₈) · N≡C–NC₄H₈ ( 11 ) with the nitrile bound to gallium. The analogous ALP with harder Al atoms yielded an adduct of the nitrile dimer or oligomers of the nitrile at room temperature. The reaction of 7a with Ph–N=C=O led to the insertion of two NCO groups into the Ga–C_vinyl bond to yield a GaOCNCN heterocycle with Ga bound to O and N atoms ( 12 ).     

Visible and NIR luminescence of nanocrystalline β-Ga2O3:Er prepared by solution combustion synthesis

In this paper we report on facile solution combustion synthesis of erbium doped β-Ga₂O₃ with urea as fuel. The product was characterized using powder X-ray diffraction and transmission electron microscopy (TEM). X-ray diffraction and TEM showed that the material is nanostructured. Luminescence properties of β-Ga₂O₃:Er are studied with excitation in near infrared (Nd:YAG laser at 1064 nm) and visible (argon laser at 514.5 nm). A strong NIR emission of Er³⁺ in the window of minimal optical loss in silica based optical fibers, due to the ⁴I_13/2→⁴I_15/2 transition at 1.55 μm has been observed. Codoping with Yb³⁺ significantly increases the intensity of that important emission.     

Reversible Size Control of Liquid‐Metal Nanoparticles under Ultrasonication

This paper describes the reversible control of the size of liquid‐metal nanoparticles under ultrasonication. Gallium was utilized as a liquid metal, which has a melting point of 29.8 °C. Investigating the effects of ultrasonication (power, time, and temperature) on the formation of gallium nanoparticles revealed that the process is similar to the formation of oil in water (O/W) or water in oil (W/O) emulsions, as the temperature significantly affects the size of the gallium nanoparticles (GaNPs). Under ultrasonication, the balance between the break‐up and coalescence of the GaNPs can be adjusted by changing the temperature or adding acid through modulating the natural surface oxide layer (which can be removed with acid) and the stabilizing effect of the surfactant dodecanethiol. Coalescence was predominant at higher temperatures, whereas particle break‐up was found to be predominant at lower temperatures. Furthermore, the change in size was accompanied by a shift in the plasmonic absorption of the GaNPs in the UV region.     

Effect of switching ultrasonic amplitude in preparing a hybrid of fullerene (C60) and gallium oxide (Ga2O3)

In this study, we proposed ‘switching ultrasonic amplitude’ as a new strategy of applying ultrasonic energy to prepare a hybrid of buckminsterfullerene (C₆₀) and gallium oxide (Ga₂O₃), C₆₀/Ga₂O₃. In the proposed method, we switched the ultrasonic amplitude from 25% to 50% (by 5% amplitude per 10 min, within 1 h of ultrasonic irradiation) for the sonochemical treatment of a heterogeneous aqueous mixture of C₆₀ and Ga₂O₃ by a probe-type ultrasonic horn operating at 20 kHz. We found that compared to the conventional techniques associated with high amplitude oriented ultrasonic preparation of functional materials, switching ultrasonic amplitude can better perform in preparing C₆₀/Ga₂O₃ with respect to avoiding titanium (Ti) as an impurity generating from the tip erosion of a probe-type ultrasonic horn during high amplitude ultrasonic irradiation in an aqueous medium. Based on SEM/EDX analysis, the quantity of Ti (wt.%) in C₆₀/Ga₂O₃ prepared by the proposed technique of switching ultrasonic amplitude was found to be 1.7% less than that prepared at 50% amplitude of ultrasonic irradiation. The particles of C₆₀/Ga₂O₃ prepared by different modes of amplitude formed large (2–12 μm) aggregates in their solid phase.Whereas, in the aqueous medium, they were found to disperse in their nano sizes. The minimum particle size of the as-synthesized C₆₀/Ga₂O₃ in an aqueous medium prepared by the proposed method of switching ultrasonic amplitude reached to approximately 467 nm. Comparatively, the minimum particle sizes were approximately 658 nm and 144 nm, using 25% and 50% amplitude, respectively. Additionally, Ga₂O₃ went under hydration during ultrasonic irradiation. Moreover, due to the electron cloud interference from C₆₀ in the hybrid structure of C₆₀/Ga₂O₃, the vibrational modes of Ga₂O₃ were Raman inactive in C₆₀/Ga₂O₃.     

“Four-component” assembly of polyaromatic 4H-cyclopenta[b]thiophene structures based on GaCl3-promoted reaction of styrylmalonates with 5-phenylthiophene-2-carbaldehyde

New “four-component” self-assembly of polyaromatic thiophene structures based on styrylmalonates and 5-phenylthiophene-2-carbaldehyde has been developed. This process is promoted by GaCl₃ and involves two [2?+?3]-annulation steps on the CHO-groups and para-substitution into one Ph-ring. The main feature of discovered process is a high diastereoselectivity with a significant increase in molecular complexity. The resulting polyaromatic structures containing two thiophene moieties in each structure have intense color and strong absorption in a near UV spectral region with absorption maxima in the range of 257–360?nm.