Determination of mercury in soils and sediments by graphite furnace atomic absorption spectrometry with slurry sampling

A graphite furnace atomic absorption spectrometric procedure for the determination of mercury is presented, in which the samples are suspended in a solution containing hydrofluoric and nitric acids. Silver nitrate (4% m/v) and potassium permanganate (3%) are incorporated, in the order specified, and aliquots are directly introduced into the graphite furnace. A fast heating programme with no conventional pyrolysis step is used. The detection limit for mercury in a 125 mg ml⁻¹ suspension is 0.1 μg g⁻¹. Calibration is performed by using aqueous standards. The reliability of the procedure is proved by analysing certified reference materials.     

Validation of an analytical method to determine trace metal impurities in fluoride compounds by flame atomic absorption spectroscopy

 The development of an analytical method for the determination of some heavy metals (Fe, Cu, Co, Zn and Ni) in fluoride compounds [Cu(BF₄)₂, Sn(BF₄)₂, Pb(BF₄)₂ and HBF₄] by flame atomic absorption spectroscopy is described. This method is to be used as a routine analytical method in an industrial quality control laboratory. To this end the "performance characteristics" of an instrumental analytical method such as matrix effects, sensitivity, linearity, detection and quantitation limits, precision and accuracy were evaluated for every system under study. The results of these investigations showed that non-spectral interferences (due to the presence of large concentrations of major metals such as Cu, Sn and Pb) were observed. Nevertheless it was possible to define a matrix concentration interval where matrix effects were not statistically significant, and therefore a direct calibration approach could be used as the calibration tool whenever the major metal concentration was not higher than 40×10^–3 kg l^–1. A guide to the developement of an analytical method for trace metal determination is provided. General tools for quality control have been used in order to show how an analytical method can be tested daily and evaluated in a convenient manner. Received: 29 January 1997 Accepted: 11 March 1997     

Analytical applications of membrane extraction in chromatography and electrophoresis

An overview of the analytical applications of membrane-based systems for sample enrichment in chromatography and capillary electrophoresis is presented. A brief introduction to the different types of membranes and the main forces related to the transport through them is also given.     

Comparative study of epithelial and fibroblastic cell lines as an alternative cytotoxicity test to the Draize method

Several methods are being used with considerable advantage as alternatives to the Draize test, although some technical difficulties still persist. This work compared the sensitivity of HeLa and NCTC L 929 cells to evaluate the cytotoxicity of shampoos used by adults and children (undiluted and diluted to 25, 5, 1, and 0.1%), and eye drops and their containers and surfactants (diluted to 30, 10, 1, and 0.1%). Nondiluted adult shampoos and their 25 and 5% dilutions were cytotoxic for both cell lines. When diluted to 1%, only one of the shampoos was noncytotoxic, whereas among those diluted to 0.1%, only one was cytotoxic. Children's shampoos were cytotoxic when not diluted or diluted to 25%. From those diluted to 5%, only one was noncytotoxic for both cell lines. The cytotoxic tests showed that the eye drops and their containers were noncytotoxic. Surfactants were cytotoxic when diluted to 30 and 10% and noncytotoxic when diluted to 1 and 0.1%. An excellent correlation (r = 0.95) was demonstrated between the sensitivity of the HeLa and NCTC L929 cells in the evaluation of cytotoxicity reactions.     

Determination of dinoseb by adsorptive stripping voltammetry using a mercury film electrode

An adsorptive stripping voltammetric method for the determination of the pesticide dinoseb (2-sec.-butyl-4,6-dinitrophenol) at the mercury film electrode is described. The deposition of the mercury film on a glassy carbon disk electrode was optimized. The temperature, at which the mercury film was deposited, was demonstrated to have a strong influence on the stripping peaks, the first one being much more intense than the second. A systematic study of the variables affecting the stripping response was carried out by differential pulse voltammetry. The results obtained have been compared with those at the HMDE; a significant improvement in the sensitivity of the method developed with the MFE was observed. Using a 300 s accumulation time, the limits of determination and detection were 3.6 × 10^–10 and 1.1 × 10^–10 mol L^–1, respectively. The effect of the presence of several herbicides on the dinoseb response was also tested. The method has been applied to the determination of the pesticide in spiked apple juice at two concentration levels: 12.0 and 1.2 g L^–1 of juice.     

ISOLATION,CHARACTERIZATION AND RECONSTITUTION OF PHYCOBILIPROTEIN ROD-CORE LINKER POLYPEPTIDE COMPLEXES FROM THE PHYCOBILISOME OF Mastigocladus laminosus*

A rod-core complex, (αβ)₆^PC. L_RC^29.5,(αβ)₃^APC.L_C^8.9, composed of hexameric phycocyanin (PC) and trimeric allophycocyanin (APC) subcomplexes associated to the CpcG2 gene product, has been isolated from the phycobilisome of Mastigocladus laminosus. Exactly the same complex was obtained by reconstitution using the subcomplexes(αβ)₃^PC. L_RC 29.5 and (aβ)₃^APC.L_C^8.9 as educts. Spectroscopic analysis of the isolated PC-L_R and PC-L_RC complexes from M. laminosus shows that the L_RC cause the largest red-shift in the absorbance and fluorescence emission maxima of PC. These results indicate that L_RC mediate PC-APC interactions in vitro. Only the CpcG2 polypeptide was able to promote this specific interaction, as neither CpcG3-PC nor, as a negative control, CpcC-PC complexes showed any reconstitution products with the core subcomplex (αβ)₃^APC.L_c^8.9. This is an indication that each of the four L_RC in the phycobilisomes of M. laminosus and Anabaena sp. PCC 7120 attaches two peripheral rods specifically to one of four different core binding sites.