Isotope dilution analysis using flow injection inductively
coupled plasma mass spectrometry was applied to determine low boron contents in iron and steel samples.
Sample dissolution was carried out in a microwave
oven
with an HCl, HNO3, and H2SO4
acid mixture and high-pressure digestion vessels. A solvent extraction procedure using acetylacetone−chloroform was applied for the
separation of the iron matrix as the sulfate (pH = 1.4
±
0.1). Test solutions corresponding to 50 mg
mL-1 of
sample, with the total boron content and iron contents
below 1 μg mL-1, were obtained. Flow
injection was used
as a sampling system to minimize problems arising from
the total salt concentration of the test solutions.
This
method made it possible to analyze boron in iron and steel
at submicrogram per gram levels. The detection limit
(3σ), in micrograms of boron per gram of sample, was
0.02, and the precision for concentrations above 10 times
the detection limit was better than 1%. Accuracy was
tested with eight standard reference materials with boron
certified values in the 0.5−10 μg g-1
range.
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