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建立了使用大气压电解液阴极辉光放电发射光谱测定水中金属离子的检测装置,并建立了测定锂的实验方法。锂浓度在0.03125~0.5 mg/L范围内,线性关系良好,方法检出限为0.01 mg/L,浓度为0.05 mg/L和0.5 mg/L时的相对标准偏差分别为4.9%和2.2%(n=7)。测试了市售天然矿泉水中锂浓度,样品不同浓度水平加标回收率在100.0%~104.0%之间。测试了浓度为1%(V/V)的HNO_3,HCl和H_2SO_4等不同种类酸化剂对发射强度的影响。HCl的发射强度低,H_2SO_4的稳定性差,HNO_3整体效果较好。测试了加入浓度为1%的不同有机酸或溶剂,如乙酸、柠檬酸、抗坏血酸、甲醇及丙酮等对发射强度的影响,结果表明:除乙酸外,其他有机试剂对锂的测定干扰较为显著。
A detection device for the determination of metal ions in water by cathodic glow discharge emission spectrometry was established and an experimental method for the determination of lithium was established. The linearity was good with the lithium concentration ranging from 0.03125 mg / L to 0.5 mg / L with the detection limit of 0.01 mg / L and the relative standard deviations (RSDs) were 4.9% and 2.2% at concentrations of 0.05 mg / L and 0.5 mg / n = 7). The lithium concentration in commercial natural mineral water was tested. The recoveries of spiked samples at different concentrations ranged from 100.0% to 104.0%. The effects of different kinds of acidifiers, such as HNO3, HCl and H2SO4, at a concentration of 1% (V / V) on the emission intensity were tested. The emission intensity of HCl is low, the stability of H 2 SO 4 is poor, and the overall effect of HNO 3 is better. The effect of adding different organic acids or solvents with concentration of 1% such as acetic acid, citric acid, ascorbic acid, methanol and acetone on the emission intensities was tested. The results showed that the interference of other organic reagents on the determination of lithium was significant except acetic acid.