管式炉燃烧-红外吸收光谱法快速测定含钒液体中硫量
Rapid Determination of Sulfur in Liquid Sample Containing Vanadium by Combustion with Resistance-Type Tubular Furnace-IR Absorption Spectrometry
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摘要: 提出了管式炉燃烧-红外吸收光谱法快速测定含钒液体试样中硫含量的方法。优化试验条件如下:① 选择氮气为载气;② 炉温为1 250 ℃;③ 三氧化钨(0.3 g)为助熔剂;④ 样品取样量为100 μL。硫的质量浓度分别在0.10~2.00,2.00~16.00 g·L-1之间与吸收值呈线性关系。方法用于含钒液体试样中硫含量的测定,结果与重量法分析结果相符。测定值的相对标准偏差(n=8)在0.73 %~2.0%之间。Abstract: A method for the rapid determination of sulfur in liquid sample containing vanadium by IR absorption spectrometry with combustion of sample in resistance-type tubular furnace was proposed. The optimum experimental conditions were found as follow: ① carrier gas: N2; ② temperature of furnace: 1 250 ℃; ③ amount of WO3 (as flux): 0.3 g; ④ amount of sample: 100 μL. Linear relationship between values of absorption and mass concentration of sulfur was kept in the range of 0.10-2.00 and 2.00-16.00 g·L-1. The proposed method was applied to the determination of sulfur in liquid sample containing vanadium, giving results in consistency with the values obtained by gravimetric method. Values of RSD′s (n=8) were found in the range of 0.73%-2.0%.