Rapid determination of carbohydrates in heroin drug seizures using capillary electrophoresis with short-end injection

A simple and rapid method for the analysis of carbohydrates in heroin samples by capillary electrophoresis utilizing a borate complexation method is described. Separations were performed using an uncoated fused silica capillary, 50 cm × 50 mm I.D. × 360 mm O.D. with an effective separation length of 9 cm. The system was run at 60°C with an applied voltage of -8 kilovolts. Injection of each sample was for 1 sec at -50 mbar. UV detection was employed with the wavelength set at 195 nm. The background electrolyte consisted of 65 mM borate, pH 12.0. Samples and standards were prepared in the run buffer containing 2 mg/mL of mannose as an internal standard. Under these conditions a test mixture containing glucose, sucrose, lactose, mannitol and mannose as an internal standard was resolved within 5 min. The method was used to determine the concentration of carbohydrates in heroin seizure samples and synthetic heroin samples. The results were in good agreement with the reported values.

The rapid analysis of heroin drug seizures using micellar electrokinetic chromatography with short-end injection

A simple and rapid method for the analysis of heroin seizures by micellar electrokinetic chromatography with short-end injection is described. Separations were performed using an uncoated fused silica capillary, 50 cm×50 mm I.D.×360 mm O.D. with an effective separation length of 8 cm. The system was run at 25°C with an applied negative voltage of –25 kilovolts. Injection of each sample was for 2 s at –50 mbar. UV detection was employed with the wavelength set at 210 nm. The background electrolyte consisted of 85:15 (water:acetonitrile, v/v) containing final concentrations of 25 mM SDS and 15 mM sodium borate, pH 9.5. Samples and standards were prepared in 0.1% v/v acetic acid and diluted in the run buffer containing 1 mg/ml of N,N-dimethyl-5-methoxytryptamine as an internal standard. Under these conditions a text mixture containing caffeine, paracetamol, morphine, codeine, heroin, and acetylcodeine was resolved within 1.5 min. The method was used to determine the concentration of heroin in heroin seizure samples, and the results were in good agreement with those obtained by a validated gas chromatographic method.

Microscopic nature and elemental composition of brown coal fly ash particles from a large coal fired power station

In this study, Australian brown coal fly ash particles have been collected from power station and analysed by scanning electron microscopy to obtain morphological information and elemental composition of individual particles. The most common particles found to be the irregular shape particle aggregates. Other shapes include ball shape with smooth surface and with some attachments; and crystal shape fine particles. The X-ray spectra of each fly ash particle revealed five groups of elemental composition, they are Si-rich particles; Ca-rich particles; Fe-rich particles; particles with Mg-Ca Matrix and particles with Si-Ca matrix. A particle sire distribution analysis has been conducted using particle size analyser and found to have a mean particle size of 21fim. The sample then was separated into fine and coarse fractions using aerodynamic classifier, and the elemental composition of both fractions were determined by ICP-AES. Borate fusion and acid dissolution method was used for sample preparation. It is found that some environmental sensitive elements such as Zn, Pb, Ni, K and Cu are enriched in fine fly ash particles. Ca has much higher contents in fine particles as well. Si and Mg have higher concentrations in coarse particles.

Luminescence and microstructure of Sr2Mg(BO3)2 doped with Eu

Sr₂Mg(B0₃)₂ doped with Eu was synthesized respectively in air and weak reducing atmosphere (combustion of carbon particle), whose photoluminescence characteristics and structure were also studied at room-temperature. In air, the fluorescent body's color was white for different synthesized temperatures. At room temperature, the sample was excited and showed red typical emission spectrum of Eu³⁺ whose emission apex were sharp near 612 nm and emission spect~m was made up of the charge transformation band (CTB) of Eu^{3 +} and excitation spectrum of 4f→4f high energy level transition, then reached the area of VUV. However, under reducing atmosphere (combustion of carbon particles), the color of the sample yielded was yellow, whose color became deeper with increasing temperature and showed phase transition. Using UV excitation, the luminescence of yellow sample was very weak. In a complicated broad spectrum at visible light area, the red emission spectrum of Eu²⁺ was not observed. Crystal structure and luminescence of the sample were completely different from the results of Diaz and Keszler. Two samples were prepared under oxidation and reducing atmosphere at high temperature, which were different on crystal structure and microstructure. By studying Sr₂Mg(B0₃)₂:Eu³⁺ a series of directional faults or educts were found, because Eu^{3 +} ions substituted for Sr^{2 +} ions. However, microstructure of Sr₂Mg(B0₃ )₂: Eu^{2 +} is more complicated, whose excitation spectrum might be excited by Eu^{2 +}. By XRD patten of the samples, phase transitibn could be found. Twins and clusters that were formed from point defect such as interstitial atom and big angle crystal boundary could be found by TEM.

Halogen-free chelated orthoborate ionic liquids and organic ionic plastic crystals

Five halogen-free orthoborate salts comprised of three different cations (cholinium, pyrrolidinium and imidazolium) and two orthoborate anions, bis(mandelato)borate and bis(salicylato)borate, were synthesised and characterised by DSC, X-ray diffraction and NMR. DSC measurements revealed that glass transition points of these orthoborate salts are in the temperature range from −18 to −2 °C. In addition, it was found that [EMPy][BScB] and [EMIm][BScB] salts have solid–solid phase transitions below their melting points, i.e. they exhibit typical features of plastic crystals. Salts of the bis(salicylato)borate anion [BScB]− have higher melting points compared with corresponding salts of the bis(mandelato)borate anion [BMB]−. Single crystal X-ray diffraction crystallography (for [Chol][BScB] crystals) and solid-state multinuclear (13C, 11B and 15N) NMR spectroscopy were employed for the structural characterisation of [Chol][BScB], [EMPy][BScB] and [EMIm][BScB], which are solids at room temperature: a strong interaction between [BScB]− anions and [Chol]+ cations was identified as (i) hydrogen bonding between OH of [Chol]+ and carbonyl groups of [BScB]− and (ii) as the inductive C–Hπ interaction. In the other salt, [EMIm][BScB], anions exhibit ππ stacking in combination with C–Hπ interactions with [EMIm]+ cations. These interactions were not identified in [EMPy][BScB] probably because of the lack of aromaticity in cations of the latter system. Our data on the formation of a lanthanum complex with bis(salicylato)borate in the liquid mixture of La3+(aq) with [Chol][BScB] suggest that this class of novel ILs can be potentially used in the extraction processes of metal ions of rare earth elements.

Evaluation of coatings for mg alloys for biomedical applications

The aim of this work was to assess a number of coatings developed for Mg for biomedical applications. The Mg substrates were high-purity (HP) Mg and ME10, an alloy recently developed for improved extrudability. The research utilized the new fishing-line specimen configuration to allow direct comparison to our recent in vivo and in vitro measurements. The in vitro measurements were immersion tests of fishing-line specimens immersed in Nor's solution at 37 °C. Tests of substantial duration are needed because the corrosion rates of uncoated samples are low. Nor's solution is the designation given to Hank's solution through which CO2 is bubbled at a partial pressure of 0.009 atm. In this solution, pH is maintained constant by the interaction of CO2 and the bicarbonate ions in the solution. This is the same buffer as that which maintains the pH of blood. Coatings examined were: (i) an anodization using a bio-friendly alkaline electrolyte consisting of phosphate, borate, and metasilicate, (ii) octyltrimethoxysilane (OSi), (iii) 1,2-bis[triethoxysilyl]ethane (BTSE), (iv) anodization+OSi, and (v) anodization + BTSE. The performance of coated samples was comparable to or better than that of the uncoated samples, and there was a substantially better performance for the ME10 samples after anodization+OSi. Reasons for the various performances are discussed.