Sampling modulation technique in radio-frequency helium glow discharge emission source by use of pulsed laser ablation

An emission excitation source comprising a high-frequency diode-pumped Q-switched Nd:YAG laser and a radio-frequency powered glow discharge lamp is proposed. In this system sample atoms ablated by the laser irradiation are introduced into the lamp chamber and subsequently excited by the helium glow discharge plasma. The pulsed operation of the laser can produce a cyclic variation in the emission intensities of the sample atoms whereas the plasma gas species emit the radiation continuously. The salient feature of the proposed technique is the selective detection of the laser modulation signal from the rest of the continuous background emissions, which can be achieved with the phase sensitive detection of the lock-in amplifier. The arrangement may be used to estimate the emission intensity of the laser ablated atom, free from the interference of other species present in the plasma. The experiments were conducted with a 13.56 MHz radio-frequency (rf) generator operated at 80 W power to produce plasma and the laser at a wavelength of 1064 nm (pulse duration:34 ns, repetition rate:7 kHz and average pulse energy of about 0.36 mJ) was employed for sample ablation. The measurements resulted in almost complete removal of nitrogen molecular bands (N₂⁺ 391.44 nm). Considerable reduction (about 75%) in the emission intensity of a carbon atomic line (C I 193.03 nm) was also observed.     

Zeolites. Efficient and Eco-friendly Catalysts for the Synthesis of Benzimidazoles

Summary. A superior method of synthesis of 2-substituted benzimidazoles by means of the heterogeneous catalysis of synthetic and natural zeolites in the reaction of 1,2-diaminobenzene with acid chlorides is described.     

Direct determination of trace metals in solid samples by atomic absorption spectrometry with electrothermal atomizers: Part 4. Interference effects in the determination of lead and bismuth in steels

The origin of observed interference effects is investigated by comparing signals obtained for lead and bismuth before and after the addition of different matrix components. It is concluded that the applicability of the solid-sampling technique should be related to the solubility of the impurity in the matrix components and to the volatilities of the impurity and matrix. The extent to which trace elements are removed from steels is similarly established by using steels and graphite pieces to which the element was added. The samples are introduced under isothermal conditions and peak areas are evaluated. It is found that 80% of lead or bismuth is recovered from stainless steel at 2100°C. Thus standardization against aqueous solutions gives inaccurate results for solid samples.     

An Efficient and Selective Solid State Oxidation of Thiols to Disulfides with Quinolinium Fluorochromate on Silica Gel

Various kinds of aliphatic (cyclic and acyclic), aromatic, and heterocyclic thiols are converted into the corresponding disulfides by quinolinium fluorochromate (QFC) on silica-gel in excellent yields. Selective oxidation of thiols in the presence of sulfides is also achieved under solid phase conditions.     

A Novel Spectrophotometric Method for the Determination of Zolmitriptan in Pharmaceutical Formulations

A simple, rapid, cost effective and extraction‐free spectrophotometric method has been developed for the determination of zolmitriptan in pharmaceutical raw and dosage forms. The method is based on the charge‐transfer reaction of zolmitriptan in acetonitrile medium with 0.2% 2,3‐dichloro‐5,6‐dicyano‐1,4‐benzoquinone to form a colored product peaking at 555 nm. Beer's law is obeyed in the concentration range 10‐250 μg mL^?1 with molar absorptivity of 1.7 × 10³ L mole^?1 cm^?1. The effects of variables such as reagent concentration, time of reaction, color stability and interferences have been investigated to optimize the procedure. The results have been validated analytically and statistically. The proposed method has been successfully applied for the determination of zolmitriptan in pharmaceutical formulations. Results indicate that the method is accurate, precise and reproducible (relative standard deviation < 2%).     

Reactions of a stable silylene with halocarbons

An unusual product formation is observed for the insertion reaction of the thermally stable silylene Si[(NCH(2)Bu(t))(2)C(6)H(4)-1,2][abbrev. as Si(NN)] into the carbon-halogen bond of alkyl or aryl halides RHal (Hal=Cl, Br). In general, depending on the halogen, the reaction either results in a disilane of type (NN)Si(Hal)-(R)Si(NN) for Hal=Cl or a mixture of disilane and the monosilane (NN)Si(R)(Hal) for Hal=Br. The results are put into context to previously suggested mechanisms. The disilane (NN)Si(Hal)-(R)Si(NN)(Hal=Cl or Br) is thermally labile and mild thermolysis yields the corresponding monosilane (NN)Si(R)(Hal) and silylene 1. Additionally, strong evidence is presented for a radical pathway for the reaction of 1 and RHal.