In-Depth Method Investigation for Determination of Boron in Silicate Samples Using an Improved Boron-Mannitol Complex Digestion Method by Inductively Coupled Plasma Mass Spectrometry.

Abstract

In this paper, a boron-mannitol complex wet acid digestion method proposed for the accurate determination of boron in silicate samples by inductively coupled plasma mass spectrometry (ICP-MS) was investigated in detail for the first time. With the addition of 50 μL of mannitol (2% wt.) into the mixture of 0.6 mL of concentrated HF and 30 μL of concentrated HNO3, the 50 mg of silicate sample was effectively decomposed after being heated overnight with optional pre-ultrasonic treatment. Following fluoride formation prevention by 8% HNO3 (wt.) and fluoride decomposition using 6% HCl (wt.), the samples were fluxed in 2.0 mL of 40% HNO3 (wt.) for 4 h and aged overnight. By diluting 1000-fold using 2% HNO3 (wt.) solution, the samples were directly quantified by an ICP-MS, showing boron recoveries of the standard materials including diabase W-2, basalt JB-2a, and rhyolite JR-2 in the range of 95.5-105.5% (n = 5). For this wet acid method, it was found that the contents of boron had no obvious difference under digestion temperatures of 65, 100, and 140 °C. It was also found that the ICP-MS quantification accuracy deteriorated at the mass of 11B when boron content was about 7250 ng yielding positive bias with average recoveries of 115.5-119.8% (n = 5), while the determination results remained unaffected at the mass of 10B. Furthermore, the digestion efficiency of boron by laboratory high-pressure closed digestion method was assessed. The boron recoveries with samples treated by the high-pressure closed digestion method were found to vary within 49.5-98.0% (n = 5) and even lowered down to 31.1% when skipping pressure relief procedure. The long-term quantification stability study showed that the boron content generally declined in one month for the high-pressure closed digestion method and exhibited no significant changes for the proposed method. By applying such an improved boron-mannitol complex digestion method, the boron concentration in the studied silicate standard materials were accurately determined, providing critical data for further boron isotope analyses and associated geochemical studies. This in-depth method investigation for silicate boron determination demonstrates the feasibility of this boron-mannitol complex strategy under a wide digestion temperature of 65-140 °C, and also sheds light on the extensive applications of boron as a geological tracer.