A method for the determination of ultratrace amounts of boron in high-purity tantalum materials [tantalum metal, tantalum(V) oxide, tantalum pentachloride and tantalum pentaethoxide] is described. On-line anion-exchange matrix separation combined with inductively coupled plasma mass spectrometry (ICP-MS) was employed for the determination of boron at the ng g−1 level. Tantalum materials were dissolved using HF and/or HNO3 prior to analysis. The loss of boron in the sample preparation procedure was examined as the recovery of boron by adding a definite amount of boron to each tantalum material sample before decomposition, and it was almost negligible. In an anion-exchange method using 0.1 M HF carrier solution, tantalum and boron in the sample solution were first adsorbed on a strongly basic anion-exchange resin. Next, boron was eluted from the resin with 5 M HCl, whereas tantalum was retained strongly adsorbed. The eluted boron was introduced
directly into the ICP-MS system for quantitative analysis at m/z 10 and 11. Because of the long elution time of boron, the transient signal was integrated in the time range 70–300 s on the chromatogram. Although the elution of boron in the time range was ca. 40% of total boron in the sample solution injected, the determination limits (10σ) obtained by the present method were 30, 25, 15 and 13 ng g−1 for tantalum metal, tantalum(V) oxide, tantalum pentachloride and tantalum pentaethoxide, respectively. The method was applied to the determination of boron in commercially available high-purity tantalum materials and it was found that the concentrations of boron were in the ng g−1–μg g−1 range.
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