Novel ion-imprinted polymer coated on nanoporous silica as a highly selective sorbent for the extraction of ultratrace quantities of gold ions from mine stone samples

We have developed a gold ion-imprinted polymer (GIP) by incorporating a dipyridyl ligand into an ethylene glycol dimethacrylate matrix which then was coated onto porous silica particles. The material was used for the selective extraction of ultratrace quantities of gold ion from mine stones, this followed by its quantitation by FAAS. The effects of concentration and volume of eluent, pH of the solution, flow rates of sample and eluent, and effect of potentially interfering ions, especially palladium and platinum, was investigated. The limit of detection is <0.2 ng?mL^?1, the precision (RSD%) is 1.03 %, and recoveries are >99 %. In order to show the high selectivity and efficiency of the new sorbent, the results were compared to those obtained with more simple sorbents possessing the same functional groups. The accuracy of the method was demonstrated by the accurate determination of gold ions in a certified reference material. To the best of our knowledge, there is no report so far on an imprint for gold ions that has such a selectivity over Pd(II) and Pt(II) ions.

Optimization of simultaneous derivatization and extraction of aliphatic amines in water samples with dispersive liquid-liquid microextraction followed by HPLC

Dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) with simultaneous derivatization followed by high-performance liquid chromatography-diode array detection (HPLC-DAD) was applied for preconcentration and determination of primary and secondary aliphatic amines in environmental water samples. A ternary mixture consisting of a disperser, an extractant and a derivatization reagent was used for the simultaneous derivatization and extraction of aliphatic amines in different water samples. The effects of various experimental parameters on derivatization and extraction efficiency were studied simultaneously using experimental design. A Plackett-Burman design was performed for screening of variables in order to determine the significant variables affecting the extraction efficiency. Then, the significant factors were optimized by using a Box-Behnken design (BBD) and the response surface equations were derived. Under optimal conditions, the preconcentration factors were between 210 and 290. The limit of detections (LODs) ranged from 0.005 to 0.02 μg/L and dynamic linear ranges (DLRs) of 0.05-500 and 0.1-500 μg/L were obtained for most of analytes. The performance of the method was evaluated for extraction and determination of primary and secondary aliphatic amines in environmental water samples in micrograms per liter and satisfactory results were obtained (RSDs <12.5%).     

Determination of haloperidol in biological samples with the aid of ultrasound‐assisted emulsification microextraction followed by HPLC‐DAD

A rapid and simple quantitative method for preconcentration and determination of haloperidol in biological samples was developed using ultrasound‐assisted emulsification microextraction, based on the solidification of floating organic droplet combined with HPLC‐DAD. The effects of several factors were investigated. A total of 30 μL of 1‐undecanol as an extraction solvent was injected slowly into a glass‐centrifuge tube containing 4 mL alkaline sample solution that was located inside the ultrasonic water bath. The formed emulsion was centrifuged and the fine droplets of solvent were floated at the top of the test tube, then it was cooled in an ice bath and the solidified solvent was transferred into a conical vial, after melt, the analysis of the extract was carried out by HPLC. Under the optimal conditions, the extraction efficiencies were more than 90% and the preconcentration factors were obtained between 119–122. The LOQs were obtained between 4–8 μg/L and the calibration curves were linear within the range of 4–1000 μg/L. Finally this method was applied to the determination of haloperidol in plasma and urine samples in the range of μg/L and satisfactory results were achieved (RSDs <7%).     

Temperature-tuned difference-frequency mixing in periodically poled KTiOPO4

4 (PPKTP). We generated 12 μW of radiation tunable around 1.6 μm by difference-frequency mixing of the outputs of a frequency-doubled Nd:YLF laser at 523 nm (240 mW) and a tunable Ti:sapphire laser near 760 nm (340 mW). A temperature tuning rate of 0.73 nm/°C for the generated wavelength and a FWHM temperature acceptance bandwidth of 6.9 °C cm was observed. The effective d₃₃ coefficient was estimated to be ∼5 pm/V. Received: 02 September 1998     

Non-critically phase-matched,Ti:Sapphire-pumped picosecond optical parametric oscillator using LiB3O5

We report a new source of high-repetition rate and widely tunable picosecond pulses for the near infrared. A singly resonant, cw, picosecond optical parametric oscillator based on temperature-tuned LiB₃O₅ and synchronously pumped by 1.8 ps pulses from a self-mode-locked Ti:Sapphire laser is demonstrated. The oscillator can provide average output powers of up to 90 mW under non-critical type-I phase matching at a pulse repetition rate of 81 MHz. Without dispersion compensation, transform-limited signal pulses with 720 fs durations have been generated at 1.2 times threshold. With the available mirror set, signal tuning over 1.374–1.530 µm and idler tuning over 1.676–1.828 µm is demonstrated for a range of pump wavelengths and phase-matching temperatures. With additional mirrors, continuous tuning throughout 1–2.7 µm should be readily attainable with a single LiB₃O₅ crystal.     

Doubly resonant continuous-wave optical parametric oscillator pumped by a single-mode diode laser

The performance characteristics of a doubly (signal and idler) resonant continuous-wave optical parametric oscillator based on periodically poled lithium niobate and pumped by a 100-mW single-mode laser diode at 810 nm are reported. Pump power thresholds as low as 16 mW and wavelength tuning over the range 1.15-1.25 microm at the signal and 2.31-2.66 microm at the idler were achieved through variation of crystal temperature, pump wavelength, and grating period. Up to 5 mW of signal output was obtained with the single-mode diode pump, and signal powers of up to 39 mW were obtained when pumping with a 400-mW injection-locked broad-area diode laser.     

Poly(N-bromoacrylamide): an efficient and useful catalyst for the protection of carbonyl compounds as dithiolanes, dithianes and oxathiolanes under solvent-free and microwave conditions

Poly(N-bromoacrylamide) (PNBA) was prepared and used as a heterogeneous electrophilic catalyst under solvent-free and microwave conditions for the mild and efficient protection of carbonyl compounds as their dithiolane, dithiane and oxathiolane derivatives with 1,2-ethanedithiol, 1,3-propanedithiol and 2-mercaptoethanol, respectively in good to excellent yields. This method is simple, efficient and straightforward for synthesis of 1,3-oxathiolanes, 1,3-dithiolanes and 1,3-dithianes from carbonyl compounds. The catalyst is recoverable and reusable.     

Novel NiFe/Si/Au magnetic nanocatalyst: Biogenic synthesis,efficient and reusable catalyst with enhanced visible light photocatalytic degradation and antibacterial activity

The aim of this paper is to biosynthesize NiFe₂O₄/SiO₂/Au (NiFe/Si/Au) magnetic nanocatalyst using the sonochemical method. This is the first study to synthesize this compound using this method. To obtain optimum morphology and size of products, the synthesis was performed in the presence of polyvinylpyrrolidone, maltose, glucose, and fructose as capping agents and Crataegus pentagyna leaf extract and NaBH₄ as reducing agents. Vibrating-sample magnetometer, field-emission scanning electron microscopy, Fourier-transform infrared, transmission electron microscopy, X-ray diffraction, energy-dispersive X-ray spectroscopy, and differential reflectance spectroscopy techniques were performed to confirm the preparation of magnetic products. The as-synthesized magnetic samples were used to enhance the photocatalytic degradation and antibacterial activity. The NiFe/Si/Au nanocatalysts exhibited an excellent photocatalytic activity by degradation of rhodamine b, methylene blue, and erythrosine as organic contaminants under ultraviolet and visible light irradiation. The degradation curves illustrate that the degradation of anionic dyes is more than that of cationic dyes. In addition, antibacterial activity of as-prepared nanocatalyst against seven bacterial species was investigated. Because of their antibacterial effects, as-synthesized products show a high antibacterial activity against various bacteria. Consequently, the NiFe/Si/Au nanocatalysts with high antibacterial activity and excellent potential photocatalyst activity can be used in environmental and medical sciences for wastewater treatment.     

Multivariate optimization of surfactant‐assisted directly suspended droplet microextraction combined with GC for the preconcentration and determination of tramadol in biological samples

In this work, a novel procedure based on surfactant‐assisted directly suspended droplet microextraction for the determination of tramadol prior to GC with flame ionization detection is proposed. In this technique, a free microdroplet of solvent is transferred to the surface of an immiscible aqueous sample containing Triton X‐100 and tramadol while being agitated by a stirring bar placed on the bottom of the sample vial. After the predetermined time, the microdroplet of solvent is withdrawn by a syringe and analyzed. The effective parameters such as the type of organic solvent, extraction time, microdroplet volume, salt content of the donor phase, stirring speed, the source phase pH, concentration of Triton X‐100, and extraction temperature were optimized. For this purpose, a multivariate strategy was applied based on an experimental design in order to screen and optimize the significant factors. This method requires minimal sample preparation, analysis time, solvent consumption, and represents significant advantages over customary analytical methods. The linearity ranged from 10 to 2000 μg/L with RSDs (n = 5) of 7.3–10. Preconcentration factors and the LODs were 391–466 and 2.5–6.5 μg/L, respectively. Finally, this method was applied to the analysis of biological samples and satisfactory results were obtained.     

Comparison of the performance of pyridine-functionalized nanoporous silica particles for the extraction of gold(III) from natural samples

We have developed a technique for the solid-phase extraction of gold using various kinds of pyridine-functionalized nanoporous silica prior to its determination in various samples using FAAS. The effects of solution pH, sample and eluent flow rate, sample volume and of potentially interfering ions are compared. The limits of detections vary from 28 to 53?pg?mL^?1. The accuracy and precision are between 99.8% and 98.3?% and 0.7 to 1.6?% (RSD), respectively. The method was successfully applied to several standard reference materials.