Determination of sexual hormones in liquid cosmetics by polymer monolith microextraction coupled with high performance liquid chromatography

A method was presented for the determination of testosterone, methyltestosterone and progesterone in liquid cosmetics by coupling polymer monolith microextraction (PMME) to high performance liquid chromatography with UV detection. A poly (methacrylic acid-ethylene glycol dimethacrylate) monolithic capillary column was selected as the extraction medium, which showed high extraction capacity towards these compounds. To achieve optimum extraction performance, several parameters relating to PMME were investigated, including extraction flow rate and pH value, inorganic salt and organic phase concentration of the sample matrix. By simple dilution with phosphate solution and filtering, the sample solution then could be directly injected into the device for extraction. The limits of detection of testosterone, methyltestosterone and progesterone were calculated to be 2, 3, 2, 8 and 4.6 mu g/L. Good linearity was achieved in the range of 10 to 1000 mu g/L with a linear coefficient. r value above 0. 996. Excellent method reproducibility was found by intra- and inter-day precisions, yielding the relative standard deviations of < 7. 7 % and < 7. 5 %, respectively. Recovery for them in the real samples was between 83% and 119%.

Optimization of cubic GaN growth by metalorganic chemical vapor deposition based on residual strain relaxation

The reduction of residual strain in cubic GaN growth by inserting a thermoannealing process is investigated. It is found that the epilayer with smaller tensile strain is subject to a wider optimal "growth window." Based on this process, we obtain the high-quality GaN film of pure cubic phase with the thickness of 4 mum by metalorganic chemical vapor deposition. The photoluminescence spectrum at room temperature shows the thick GaN layer has a near-band emission peak with a full width at half maximum of 42 meV which confirms its high crystal quality, further supported by the x-ray (002) diffraction measurement. A simplified model is demonstrated to interpret this strain effect on the growth process. (C) 2003 American Institute of Physics.

MOCVD growth of cubic GaN: Materials and devices

Many impressive progresses have been made recently on the growth of cubic-phase GaN by MBE and MOCVD. In this paper, some of our recent progress will be reviewed, including the growth of high quality cubic InGaN films, InGaN/GaN heterostructure blue and green LEDs. Cubic-phase GaN films were grown on GaAs (100) substrates by MOCVD. Growth conditions were optimized to obtain pure cubic phase GaN films up to a thickness of 4 mum. An anomalous compressive strain was found in the as-grown GaN films in spite of a smaller lattice constant for GaN compared with that of GaAs substrates. The photoluminescence FWHM of high quality InGaN epilayers was less than 100 meV The InGaN/GaN heterostructure blue LED has intense electroluminescence with a FWHM of 20 nm.

Liquid-liquid extraction of Pa-233(V) with Aliquat 336

The extraction of protactinium with Aliquat 336 (methyl-tri-caprylyl ammonium chloride) in toluene, cyclohexane and chloroform from HCl, HNO3, H2SO4, HClO4, HF and mixed HCl-HF media was investigated by radioactive tracer technique. Distribution ratios of protactinium between the aqueous solution and the organic phase were determined as a function of shaking time, concentrations of acid in aqueous solution phase, extractant concentration and type of diluents in the organic phase. Aliquat 336 can almost quantitatively extract protactinium from strong HCl solution. At the same time, small amounts of HF in HCl solutions have a strong effect on Pa distribution.

Liquid-liquid extraction of protactinium(V) using tri-iso-octylamine

Solvent extraction of protactinium with tri-iso-octyl-amine (TIOA) in xylene, benzene, carbon tetrachloride and chloroform from HCl, HF, HNO3, HClO4 and H2SO4 media was studied using Pa-233 as a radiotracer. The extraction efficiencies of protactinium were determined as a function of shaking time, concentrations of mineral acids in aqueous phase, extractant concentrations and diluents in organic phase. The extraction mechanism was discussed. The results show that the extracted species in the organic phase is [(R3N-H)(n)Pa(OH)(x)Cl-y(5-x-y)].

Synthesis and luminescent properties of Lu3Ga5O12 : RE3+ (RE = Eu, Tb, and Pr) nanocrystalline phosphors via sol-gel process

Lu3Ga5O12:Eu3+, Lu3Ga5O12:Tb3+, and Lu3Ga5O12:Pr3+ phosphors were prepared through a Pechini-type sol-gel process. X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), photoluminescence, and cathodoluminescence spectra were utilized to characterize the synthesized phosphors. The XRD results reveal that the sample begins to crystallize at 800 degrees C and fully crystallined pure Lu3Ga5O12 phase can be obtained at 1000 degrees C. The FESEM image indicates that the phosphor sample is composed of aggregated rice grainlike particles with sizes around 80-120 nm.

Reversed micelle formation in a model liquid-liquid extraction system

The formation of reversed micelles and the roles of extractant and extracted complexes were investigated in the Cyanex923/n-heptane/H2SO4 system. Interfacial tension (gamma), electrical conductivity (kappa), and water content measurements showed that Cyanex923 had a tendency to self-assemble, forming reversed micelles. The changes in electrical conductivity with concentration of H2SO4 in the organic phase (CH2SO4,(0)) exhibited an S-type curve: a correlation was found between the change in electrical conductivity and the water content as a function of CH2SO4,(0),.

Uniform YVO4:Ln(3+) (Ln = Eu, Dy, and Sm) nanocrystals: Solvothermal synthesis and luminescence properties

Well-dispersed YVO4:Ln(3+) (Ln = Eu, Dy, and Sm) nanocrystals with uniform morphology and size have been synthesized via a facile solvothermal route. XRD results demonstrate that all of the three samples can be well indexed to the pure tetragonal phase Of YVO4, indicating that the Eu3+, Dy3+, and Sm3+ have been effectively doped into the host lattices of YVO4. TEM images show that the YVO4 nanocrystals exhibit ellipsoid shape and a mean size of about 20 nm, which is in good agreement with the estimation of XRD results.

Facile synthesis and luminescence properties of octahedral YVO4:Eu3+ microcrystals

Uniform octahedral YVO4:Eu3+ microcrystals have been successfully prepared through a designed two-step hydrothermal conversion method. One-dimensional precursor Y4O(OH)(9)NO3 was first prepared through a simple hydrothermal process without using any surfactant, catalyst or template. Subsequently, well-defined octahedral YVO4 was synthesized at the expense of the precursor during a hydrothermal conversion process. XRD results demonstrate that the diffraction peaks of the final product can be well indexed to the pure tetragonal phase of YVO4.

Synthesis and Luminescent Properties of LaAlO3:RE3+ (RE = Tm, Tb) Nanocrystalline Phosphors via a Sol-Gel Process

LaAlO3:Tm3+ and LaAlO3:Tb3+ phosphors were prepared through a Pechini-type sol-gel process. X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), photoluminescence, and cathodoluminescence (CL) spectra were utilized to characterize the synthesized phosphors. The XRD results reveal that the fully crystalline pure LaAlO3 Phase can be obtained at 800 degrees C. The FE-SEM image indicates that the phosphor samples are composed of aggregated spherical particles with sizes ranging from 40 to 80 nm. Under the excitation of ultraviolet light (230 nm) and low-voltage electron beams (1-3 kV), the LaAlO3:Tm3+ and LaAlO3:Tb3+ phosphors show the characteristic emissions of Tb3+ (D-1(2)-> H-3(6,4),F-3(4) transitions) and Tm3+ (D-5(3,4)-> F-7(6,5,4,3) transitions) respectively. The CL of the LaAlO3:Tm3+ phosphors have high color purity and comparable intensity to the Y2SiO5:Ce3+ commercial product, and the CL colors of Tb3+-doped LaAlO3 phosphors can be tuned from blue to green by changing the doping concentration of Tb3+ to some extent.

Tunable Photoluminescence and Cathodoluminescence Properties of Eu3+-Doped LaInO3 Nanocrystalline Phosphors

LaInO3:Eu3+ phosphors were prepared by a Pechini sol-gel process. X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), diffuse reflectance, photoluminescence, cathodoluminescence spectra, as well as lifetimes were utilized to characterize the synthesized phosphors. XRD results reveal that the sample begins to crystallize at 600 degrees C and pure LaInO3 phase can be obtained at 800 degrees C. The crystallinity increases upon raising the annealing temperature. The FE-SEM images indicate that LaInO3:Eu3+ phosphors are composed of fine and spherical grains around 40-80 nm in size. Under the excitation of UV light and low-voltage electron-beams, LaInO3:Eu3+ phosphors show the characteristic emissions of the Eu3+ (D-5(J)-F-7(J) J,J(')=0,1,2,3 transitions). The luminescence colors can be tuned from yellowish warm white to red by changing the doping concentration of Eu3+ to some extent. The corresponding luminescence mechanisms have been proposed.

Synthesis and luminescent properties of LaInO3: RE3+ (RE = Sm, Pr and Tb) nanocrystalline phosphors for field emission displays

LaInO3: Sm3+, LaInO3: Pr3+ and LaInO3: Tb3+ phosphors were prepared through a Pechini-type sol-gel process. X-ray diffraction, field emission scanning electron microscopy, photoluminescence, and cathodoluminescence (CL) spectra were utilized to characterize the synthesized phosphors. XRD results reveal that the pure LaInO3 phase can also be obtained at 700 degrees C. FE-SEM images indicate that the LaInO3: Sm3+, LaInO3: Pr3+ and LaInO3: Tb3+ phosphors are composed of aggregated spherical particles with sizes around 80-120 nm. Under the excitation of ultraviolet light and low voltage electron beams (1-5 kV), the LaInO3: Sm3+, LaInO3: Pr3+ and LaInO3: Tb3+ phosphors show the characteristic emissions of Sm3+ ((4)G(5/2)-H-6(5/2,7/2,9/2) transitions, yellow), Pr3+ (P-3(0)-H-3(4), P-3(1)-H-3(5), D-1(2)-H-3(4) and P-3(0)-F-3(2) transitions, blue-green) and Tb3+ (D-5(4)-F-7(6.5,4.3) transitions, green) respectively. The corresponding luminescence mechanisms are discussed. These phosphors have potential applications in field emission displays.

Carbon dioxide pressure induced heterogeneous and homogeneous Heck and Sonogashira coupling reactions using fluorinated palladium complex catalysts

The Heck reaction of iodobenzene and methyl acrylate was investigated with CO2-philic Pd complex catalysts having fluorous ponytails and the organic base triethylamine (Et3N) in the presence of CO2 under solventless conditions at 80 degrees C. The catalysts are not soluble in the organic phase in the absence Of CO2 and the reaction occurs in a solid-liquid biphasic system. When the organic liquid mixture is pressurized by CO2, CO2 is dissolved into the organic phase and this promotes the dissolution of the I'd complex catalysts. As a result, the Heck reaction occurs homogeneously in the organic phase, which enhances the rate of reaction. This positive effect Of CO2 pressurization competes with the negative effect that the reacting species are diluted by an increasing amount of CO2 molecules dissolved. Thus, the maximum conversion appears at a CO2 pressure of around 4 MPa under the present reaction conditions. The catalysts are separated in the solid granules by depressurization and are recyclable without loss of activity after washing with n-hexane and/or water.

Synthesis of REF3 (RE = Nd, Tb) nanoparticles via a solvent extraction route

NdF3 and TbF3 nanoparticles were successfully synthesized via a solvent extraction route using Cynex923 (R3P=O). X-ray diffraction (XRD) study showed that pure hexagonal phase NdF3 and pure orthorhombic phase TbF3 could be obtained under the current synthetic conditions. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) observations indicated that as-obtained NdF3 nanoplates have a diameter of 50-80 nm and thickness of 10-20 nm and TbF3 products have sphere morphologies with diameter from 70 to 170 nm. The driving force for the growth of NdF3 nanoplates could be attributed to the hexagonal crystal structure. The luminescence properties of NdF3 and TbF3 nanoparticles were investigated, which indicated that NdF3 nanoparticles showed typical emission at 888,1064, and 1328 nm and TbF3 nanoparticles showed characteristic emission of Tb3+ (f-f).

Nanocrystalline LaAlO3:Sm3+ as a Promising Yellow Phosphor for Field Emission Displays

Nanocyrstalline LaAlO3:Sm3+ phosphors were prepared through a Pechini-type sol-gel process. X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), photoluminescence, and cathodoluminescence (CL) spectra were utilized to characterize the synthesized phosphors. XRD results reveal that the sample begins to crystallize at 600 degrees C, and pure LaAlO3 phase can be obtained at 700 degrees C. FE-SEM images indicate that the Sm3+-doped LaAlO3 phosphors are composed of aggregated spherical particles with sizes ranging from 40 to 80 nm. Under the excitation of UV light (245 nm) and low-voltage electron beams (1-3 kV), the Sm3+-doped LaAlO3 phosphors show the characteristic emissions of the Sm3+ ((4)G(5/2)-H-6(5/2), H-6(7/2), H-6(9/2) transitions) with a yellow color. The CL intensity (brightness) of the Sm3+-doped LaAlO3 phosphor is higher than that of the commercial product [Zn(Cd)S:Ag+] (yellow) to some extent.