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The estimation of magnesium in small biological samples by flame spectrophotometry.

Studies of human magnesium metabolism in this laboratory called for a simple and reliable method of estimating the magnesium content of large numbers of small biological specimens (Montgomery, 1960). It has been found that a technique involving the Unicam S.P. 900 flame spectrophotometer fulfils this need. Estimations have been made on serum, red cells, urine, and acid digests of muscle and faeces. A standard instrument was used, burning acetylene and air, with a new standard atomiser containing a metal jet. Readings were made at the atomic line of 285.2 mmu.

Body Fluids↗

Determination of boron in silicon-doped gallium arsenide by electrothermal atomic absorption spectrometry and ultraviolet-visible spectrophotometry.

Two methods have been developed for the determination of boron impurities in silicon-doped gallium arsenide (GaAs) for electronics. The first method employs the electrothermal atomic absorption spectrometry (ETAAS), the second, the UV-Vis molecular absorption spectrophotomety. In both cases the GaAs sample is decomposed with aqua regia (1+1). To prevent Ga(III) interference on the ETAAS determination of boron, a double extraction of the chlorogallic acid (HGaCl4) in diethyl ether is performed. To improve the overall ETAAS performance, the graphite tubes were pre-treated with iridium(III) and tungsten(IV). A mixed chemical modifier containing Ni(II), Sr(II) and citric acid was also used. The characteristic mass (m0) is 301 +/- 47 pg and the detection limit (3sB) is 2.4 microg g(-1). The classic UV-Vis spectrophotometric procedure using curcumin was also extended to the determination of boron in GaAs. By masking Ga(III) with EDTA and a preliminary extraction of boron with 2-ethyl-hexane 1,3-diol, performed on a semi-micro scale, a detection limit of 0.6 microg g(-1) was achieved. Both methods were applied to the analysis of two Si-doped GaAs samples which were suspected of being boron-contaminated. Results are compared with those obtained by direct analysis of the decomposed sample solution using the inductively coupled plasma atomic emission spectrometry (ICP-AES).

Arsenicals↗

[Determination of trace palladium based on kinetic-spectrophotometry with malachite green-sodium hypophosphite system].

A new kinetic-spectrophotometric method for the determination of trace amount of palladium has been proposed. It is based on the palladium catalysed discoloring reaction of malachite green reduced by sodium hypophosphite in phosphoric acid buffer solution (pH = 2.0). The linear range of determination of palladium is 0-10 microgram.L-1, the detection limit is 9.78 x 10(-11) g.mL-1. The method has been used for the determination of palladium in some catalyst with satisfactory results. The mechanism of the reaction has also been discussed.

Indicators and Reagents↗