中孔分子筛SBA-15-NH_2分离富集火焰原子吸收光谱法测定烟花中痕量钯的研究与应用  

Separation/Preconcentration of Mesoporous SBA-15-NH_2 Material for Trace Pd(Ⅱ) in Fireworks and Its Determination by Flame Atomic Absorption Spectrometry

作　　者：周乐舟[1] 付胜[1] 高寿泉[1] 周方钦[2] 

机构地区：[1]湖南省劳动卫生职业病防治所,湖南长沙410007 [2]湘潭大学化学学院,湖南湘潭411105

出　　处：《分析测试学报》2009年第2期173-176,180,共5页Journal of Instrumental Analysis

基　　金：湖南省自然科学基金资助项目(05JJ40024)

摘　　要：建立了中孔分子筛SBA-15-NH2分离富集火焰原子吸收光谱法测定痕量钯的新方法,探讨了中孔分子筛SBA-15-NH2材料吸附钯的原理和最佳条件。在pH 3.0、温度为（15±1）℃的条件下,钯可被该材料定量吸附,其吸附容量为1.21mg/g。吸附的钯用饱和硫脲溶液洗脱,并用火焰原子吸收法测定洗脱的钯。该方法测定钯的检出限为0.59μg/L（3σ,n=11）,线性范围为0.002～1.2 mg/L,加标回收率为98%～107%。对0.05 mg/L的Pd^2＋溶液平行测定7次,RSD为2.24%。方法用于烟花中痕量钯的测定,结果满意。A flame atomic absorption spectrometry（FAAS） method was developed for the determination of trace palladium （ Ⅱ ） by using mesoporous SBA-15-NH2 material as sorbent. The adsorbing principle and optimal conditions of mesoporous SBA-15-NH2 material for Pd（Ⅱ） were investigated. Under the optimized conditions of pH 3.0 buffer and （ 15 ± 1 ）℃ , palladium could be adsorbed by mesoporous SBA-15-NH2 material with a adsorption capacity of 1.21 mg/g. After eluted by saturated thiourea, the elute was determined by FAAS. The calibration curve showed a good linearity in the range of 0. 002 - 1.2 mg/L with a detection limit of 0.59 μg/L （3σ, n - Ⅱ ）. The recoveries of Pd （ Ⅱ ） from fireworks sample spiked with three concentration levels at 0.20, 0.40 and 0. 80 μg/L ranged from 98% to 107%. The RSD for determination of 0.05 mg/L Pd（ Ⅱ ） was 2.24% （n =7）. The proposed method was applied for the determination of trace Pd （ Ⅱ ） in fireworks sample with satisfactory results.

关 键 词：中孔分子筛 SBA-15-NH2 分离 富集 火焰原子吸收光谱法(FAAS) 钯(Ⅱ) 

分 类 号：O657.31[理学—分析化学] O614.823[理学—化学]