Determination of sulfur in biological samples using high-resolution molecular absorption spectrometry in a graphite furnace with direct solid sampling

摘要

The determination of sulfur in biological materials using high-resolution continuum source molecular absorption spectrometry and electrothermal vaporization of the carbon monosulfide (CS) molecule has been investigated in detail using direct solid sampling. Best results have been obtained coating the platform with tungsten as a permanent modifier, adding 40 μg Pd in solution as a chemical modifier, and the only sulfur compound that showed sufficient sensitivity and thermal stability to be used for calibration purposes under the conditions established for biological materials was thiourea. A pyrolysis temperature of at least 900 ℃ could be used and the optimum vaporization temperature was 2500 ℃. Under optimized conditions a limit of detection of 0.015 μg S absolute or 0.03 mg g~(-1)S in the solid sample, based on a sample mass of 0.5 mg could be obtained; the characteristic mass was m_0= 18 ng. Five certified biological reference materials have been analyzed using direct solid sampling and calibration against aqueous standards; the results were in agreement with the certified values on a 95% confidence interval.