Spectrophotometric determination of boron in iron and steel with curcumin after separation by 2-ethyl-1,3-hexanediol-chloroform extraction.
A simple and reliable method for determining approximately 0.0001% or more of total boron in iron and low- and high-alloy steels is described. After the sample is decomposed at <70 degrees in the presence of hydrogen peroxide and potassium hydrogen fluoride, the insoluble material is filtered off and ultimately fused with sodium carbonate. The cooled melt is dissolved in dilute hydrochloric acid and the solution is combined with the main solution. Fluoride is subsequently complexed with zirconium and boron is separated from iron and other elements by extraction as borate from 1M sulphuric acid medium into chloroform containing 2-ethyl-1,3-hexanediol. Boron, in a 1-ml portion of the extract, is ultimately determined spectrophotometrically at 550 nm in an ethanol medium, after formation of the curcumin rosocyanin complex in a glacial acetic acid-concentrated sulphuric acid medium. Acid-soluble and acid-insoluble boron can also be determined. Common ions, including large amounts of manganese, chromium, vanadium, titanium, molybdenum, tungsten, niobium and tantalum do not interfere.
Donaldson
E M
EM
Mineral Sciences Laboratories, Canada Centre for Mineral and Energy Technology, Energy, Mines and Resources Canada, Ottawa, Canada.