Determination of trace elements in marine plankton by inductively coupled plasma mass spectrometry (ICP-MS)

A method has been developed for the determination of 23 elements in marine plankton in which inductively coupled plasma (ICP) source mass spectrometry (MS) was used to quantify the elements in the solution after digestion in a mixture of hydrofluoric and nitric acids in sealed PTFE vessels in a microwave field. The procedure was validated by the analysis of a standard reference soil (SRM 2709 San Joaquin Soil) and a standard reference fresh water plankton (CRM 414). The method was applied to the analysis of several marine plankton samples grown under controlled conditions including several whose growth media had been enriched with selenium. Matrix induced signal suppressions and instrumental drift were corrected by internal standardization. The suitabilities of germanium, indium, rhodium, scandium and yttrium as internal standard elements were evaluated. Neither scandium nor yttrium could be used due to the presence of these elements in the samples, germanium was used for the determination of As, Co, Cu, Fe, Ni, Se, Si and Zn, indium was used for Al, Ba, Ca, Eu, Sr, and Tl, and rhodium was used for Cd, Cr, Hg, Mg, Pb, Sb, Sn, and V. For Al, Ca, Cr, Cu, Fe, Mg, Mn, Ni, Si, Sr, V, and Zn internal standardization did not completely compensate for the suppressive effect of the heavier elements and the solutions were diluted. However, for As, Ba, Cd, Co, Eu, Hg, Pb, Sb, Se, Sn and T1, it was possible to obtain accurate results despite the 35-40% suppression in the signals. Isobaric overlap was only a problem in the cases of 42Ca and 78Se; 44Ca and 77Se, respectively, were used. Memory effects were only observed with Hg for which a nitric acid-sodium chloride solution was the most effective wash-out solution. The marine plankton samples were able to tolerate a higher concentration of Hg as the selenium concentration increased.     

Determination of silicon by an indirect atomic-absorption method using carbon-rod electrothermal atomization

An indirect procedure has been developed for the determination of trace amounts of silicon by atomic-absorption with carbon-rod electrothermal atomization. After dissolution, the silicon is extracted as silicomolybdic acid into a mixture of diethyl ether and pentan-1-ol (5 + 1). The co-extraction of excess of molybdate reagent is prevented by the addition of citrate, which also destroys phosphomolybdic and arsenomolybdic acids. The organic layer is washed with hydrochloric acid, mul quantities are transferred to the electrothermal atomizer and the molybdenum is measured. The method has been applied to analysis of several steels.     

Selective detection and identification of Se containing compounds--review and recent developments

The complexity of selenium (Se) chemistry in the environment and in living organisms presents broad analytical challenges. The selective qualitative and quantitative determination of particular species of this element is vital in order to understand selenium's metabolism and significance in biology, toxicology, clinical chemistry and nutrition. This calls for state-of-the-art analytical techniques such as hyphenated methods that are reviewed with particular emphasis on interfaced separation with element-selective detection and identification of the detected selenium compounds. Atomic spectral element specific detection for monitoring chromatographic eluent enabled quantitative determination of selenium species in selenized yeast and qualitative measurement for breath samples. Gas chromatography with atomic emission detection (AED) of ethylated species and fluoroacid ion pair HPLC applied to the analysis of currently produced or archived selenized yeast and Brassica juncea have revealed the presence of a previously unrecognised Se-S amino acid, S-(methylseleno)cysteine.     

Flow injection reagent introduction by supported liquid and nafion membranes: determination of phosphate

The use of membrane tubing for the introduction of reagents for the determination of phosphate in waters by flow injection analysis was studied. The use of membranes eliminates the need for confluence points in the design of flow injection manifolds. This increases the sensitivity of the manifold by providing a sufficient reagent excess for the reaction without diluting the sample. Methods for the introduction of acid, molybdate and hydrazine were devised for the determination of phosphate by the Molybdenum Blue method. Several membranes were examined and Nafion and Accurel (microporous polypropylene) were found to be most useful. Molybdate introduction was achieved using a supported liquid membrane (SLM). Calibration was linear and a detection limit of 12 ppb phosphate (4 ppb phosphorus) was obtained.