碱熔-离子色谱法同时测定玻璃中的氟和硫
Simultaneous Quantification of Fluorine and Sulfur in Glass by Ion Chromatography with Alkali Fusion
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摘要: 玻璃样品中加入氢氧化钠,在700℃马弗炉中加热熔融,热水浸提,所得溶液通过OnGuard Ⅱ Ag/H柱后上机测定,消除加入的氯和碱的干扰,再经IonPac AG14柱和AS14柱分离,采用小体积的定量环直接进样,离子色谱法测定氟离子和硫酸根的含量。氟离子和硫酸根的线性范围分别为0.1~2 μg/mL和0.5~20 μg/mL,方法检出限氟为2.0 mg/kg和硫为1.0 mg/kg,测定结果的相对标准偏差(RSD)小于5.0%。实际玻璃样品用离子色谱法和化学法测定,两种分析方法的结果无显著性差异。Abstract: A method was developed for the determination of fluorine and sulfur in glass by ion chromatography coupled with alkali fusion. The glass samples were calcined with solid NaOH in a muffle furnace at 700℃, then extracted by hot water. The extracted solution was loaded through the OnGuard Ⅱ Ag/H cartridges before being injected into the Ion Chromatography system in which fluorine and sulfur were separated by the Ionpac AG14 and AS14 column and detected by conductometry. The linear range for the determination of fluorine and sulfur were 0.1-2 μg/mL and 0.5-20 μg/mL with detection limits of 2.0 mg/kg and 1.0 mg/kg, respectively. The relative standard deviation was less than 5.0%. The results of Ion Chromatographic ethod and chemical method have no significant difference for the determination of glass samples.