Study of metal-loaded activated charcoals for the separation and determination of selenium species by energy dispersive X-ray fluorescence analysis

Conversion of adsorption properties of activated charcoal (C^∗) by metal modification towards selenite, selenate and seleno-dl-methionine (Se-Met) was studied. Several metals were included in modification studies and also a procedure was developed for the separation and independent determination of microgram quantities of these selenium species in aqueous solution. Selenium species were collected one by one from the same sample solution onto collector material by adsorbing them directly or after complex formation onto different metal-loaded activated charcoals (MgC^∗ and FeC^∗). The mass of selenium in these collectors was measured directly by energy dispersive X-ray fluorescence spectrometry (EDXRF). Detection limits for all three selenium species were better than 6 μg corresponding to concentration of 60 μg/l with 0.100 l of initial sample volume.     

Physico-Chemistry of the Limestone Sulphation Process

Aspects of the mechanism of the overall reaction between CaCO₃/CaO and SO₂/SO₃ under oxidizing conditions are discussed. The limestone and lime sulphation processes were carried out in a thermobalance under conditions relevant to atmospheric fluidized bed combustion. Sulphated samples, prepared in the form of cross-section particles, were examined in a scanning electron microscope by energy-dispersive X-ray and back-scattered electron imaging. Photomicrographs are presented. The reaction proceeded from the outer surface of the particles and along the pores. Surface textural changes during the reaction were considered. The layer of products was identified as controlling both the rate and extent of limestone/lime sulphation. In the products, two sulphur-bearing solids (CaSO₄ and CaS) were identified. The presence of CaS, which may cause difficulties in practice, is attributed to CaSO₃ disproportionation. This revised version was published online in August 2006 with corrections to the Cover Date.     

Determination of manganese in brain samples by slurry sampling graphite furnace atomic absorption spectrometry

A simple procedure for the determination of manganese in different sections of human brain samples by graphite furnace atomic absorption spectrometry has been developed. Brain sections included cerebellum, hypothalamus, frontal cortex, vermix and encephalic trunk. Two sample preparation procedures were evaluated, namely, slurry sampling and microwave-assisted acid digestion. Brain slurries (2% w/v) could be prepared in distilled, de-ionized water, with good stability for up to 30 min. Brain samples were also digested in a domestic microwave oven using 5 ml of concentrated HNO₃. A mixed palladium+magnesium nitrate chemical modifier was used for thermal stabilization of the analyte in the electrothermal atomizer up to pyrolysis temperatures of 1300 °C, irrespective of the matrix. Quantitation of manganese was conducted in both cases by means of aqueous standards calibration. The detection limits were 0.3 and 0.4 ng ml⁻¹ for the slurry and the digested samples, respectively. The accuracy of the procedure was checked by comparing the results obtained in the analysis of slurries and digested brain samples, and by analysis of the NIST Bovine Liver standard reference material (SRM 1577a). The ease of slurry preparation, together with the conventional set of analytical and instrumental conditions selected for the determination of manganese make such methodology suitable for routine clinical applications.     

The Reaction of Maleic and Phthalic Anhydrides with 2-Methylimidazole

The reaction of maleic anhydride with 2-methylimidazole in acetonitrile and DMF is accompanied by the appearance of strong absorption bands in the visible part of the spectrum due to the formation of molecular complexes. In acetonitrile the reaction proceeds by two routes via the formation of an amide and the molecular complex. Phthalic anhydride reacts with 2-methylimidazole to give amide but not to form molecular complexes.     

Cavitands bearing four fluorophores

The synthesis of novel cavitands containing four fluorophores [tert-butoxycarbonyl protected 2,2′-bis(furyl)benzidine (t-BOC FurylBz) or 5,5′-bis(4-aminophenyl)-2,2′-bifuryl (t-BOC PFDA)] and ionophoric functional groups on the upper rim is reported. The cavitands bearing the four fluorophores emit blue light photoluminescence. In particular, the cavitand containing PFDA moieties exhibits a high photoluminescence quantum yield.     

流动注射在线萃取-火焰原子吸收法测定食用盐中的锌

基于锌与 1 (2 吡啶偶氮 ) 2 萘酚 (简称PAN)形成的配合物可被氯仿萃取 ,从高盐基体样品中分离富集锌 ,利用自行设计的分相器 ,实验确定了最佳的流动注射在线萃取 火焰原子吸收光度法测定锌的流路系统和化学反应条件。在选定的工作条件下 ,其RSD和检出限分别为 4 3 % (c=0 6 μg/mL ,n =1 1 )和0 0 3 μg/mL ,测定速度为 2 5样 /h。用于实际样品的测定 ,加标回收率为 97%～1 0 6 %。     

Sequential determination of platinum, ruthenium, and molybdenum in carbon-supported Pt, PtRu, and PtMo catalysts by atomic absorption spectrometry

A simple accurate and precise analytical method for the determination of platinum, ruthenium, and molybdenum in Pt, PtRu, and PtMo nanoparticles catalysts deposited on high-surface area carbon by flame atomic absorption spectrometry (FAAS) and graphite furnace atomic absorption spectrometry (GFAAS) is described. The complete digestion of samples (0.010-0.020 g), which contain noble metals (NMs) in the range between 0 and 30% in combination among them or with other non-NMs, is obtained under mild conditions using both concentrated HCl and HCl+HNO₃ (1+1 (v/v)) mixture to boiling for 30 min in an open vessel. Carbon is separated from the solution by filtering it. Under optimized conditions of the flame, the poor sensitivity of platinum is enhanced 50-fold in presence of 1% (m V⁻¹) ascorbic acid, whereas the analytical signal of ruthenium increased by the presence of co-existing platinum. Any kind of interference is observed on the analytical signal of molybdenum. Recovery test obtained by analyzing commercial powder catalysts ranged from 99 to 101%. The precision, expressed as relative standard deviation of five measurements, is better than 1%. Electrode catalysts, made by using the carbon-supported platinum-based powder catalysts, have been analyzed for the metal loadings onto the electrode by GFAAS after dissolution under the same conditions used for the powder catalysts. The precision, expressed as relative standard deviation of three measurements, is better than 2%.     

Determination of trace elements in biological materials using tetramethylammonium hydroxide for sample preparation

A method to prepare milk powder, bovine liver and bovine muscle samples for analysis by electrothermal atomic absorption spectrometry (ETAAS) is proposed. Samples are mixed with a small amount of tetramethylammonium hydroxide (TMAH) and a stable and homogeneous slurry is produced in ca. 2 h with heating at 60–70 °C. After such sample preparation and dilution with water, trace elements are determined in certified reference materials. Pyrolysis and atomisation temperatures are optimised for each element, and several modifiers are investigated. External calibration is used for every analyte. Limits of detection (LODs), precision and accuracy are reported for Cd, Pb, Ni, Cr, Cu and Ag and compared with those obtained after conventional acid digestion. The main advantages of the proposed method are the simplicity of sample preparation and the longer lifetime of the graphite tube.     

STUDY ON THE NANOSECOND TRANSIENT ABSORPTION SPECTRA OF HYPOCRELLIN A

In this paper, the nanosecond transient absorption spectra and the fluorescence spectraof Hypocrellin A(HA) are examined in solvents of varying polarity. There are three absorp-tion bands in dilute HA solutions: Ⅰa, Ⅱa are defined as the triplet-triplet absorption ofHA, the band Ⅲa is supposed to be the absorption of the solvent--sepatated ion pair (SSIP).In more concentrated solutions, only the absorption of SSIP was observed. The effects ofsolvent polarity on transient absorption spectra and fluorescence spectra of HA and the effectof oxygen on the intensities of the fluorescence of HA are discussed. Then a reasonablemechanism for the photolysis of HA is proposed.