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High-Resolution Graphite Furnace Atomic Absorption Spectrometry Determination of Bismuth in Lithium Niobate Optical
Dániel Csontos1, László Kovács1, Krisztián Lengyel1
1Department of Applied and Nonlinear Optics, Institute for Solid State Physics and Optics, HUN-REN Wigner Research Centre for Physics, P.O. Box 49, H-1525 Budapest, Hungary.
Abstract:
High-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS) methods with solid and solution sampling were developed for the determination of the Bi dopant in high-purity lithium niobate (LiNbO3) crystals. Samples were cut from the cylindrical crystal bulks, cleaned, and pulverized. A HF-HNO3 mixture was applied for microwave digestion of LiNbO3 (≈0.07 g per sample). Atomization transients, pyrolysis, and atomization curves were studied with various media and chemical modifiers, e.g., triammonium citrate (TAC), Pd-Mg-(NO3)2. For solid samples, the optimal pyrolysis and atomization temperatures of Bi were found at 1000 and 1800 °C, respectively, whereas, for solution samples, much lower values of 500 and 1300 °C were obtained. TAC slightly, but Pd-Mg considerably increased the optimal pyrolysis and atomization temperatures, i.e., up to 1300 and 2100 °C, respectively. The dissolved LiNbO3 matrix acted as an internal modifier, exhibiting optimal pyrolysis and atomization temperatures for Bi. For solid sample analysis, 0.05-0.4 mg (average: 0.1 mg) of LiNbO3 powder was dosed into graphite boats, while conventional standard addition and three-point estimation were used for calibration. The limit of detection (LOD) was 0.4 and 0.3 μg/g for solid and solution analysis, respectively, using Bi I 227.6580 nm and Bi I 223.0608 nm lines, respectively. Utilizing the latter for solid sampling, an LOD of 0.03 μg/g can be attained. The analytical results for all methods were in good agreement (mean bias: <12%). The precision of the solid and solution sample methods was at 6-16% (average: 12%) and 1-13% (average: 4.4%), respectively. The Bi content of the crystals ranged from 56 to 311 μg/g. The characteristic mass for solid and solution sampling was 220 and 17 pg, respectively. The accuracy of the method was checked against the GBW07407 (laterite soil) certified reference material.
