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氧化石墨烯/硫杂杯芳烃复合材料富集分离-石墨炉原子吸收法测定痕量铊 被引量:10

Determination of Trace Thallium by Graphite Furnace Atomic Absorption Spectrometry after Preconcentration with Graphene Oxide / Thiacalixarene Composites Material
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摘要 自制了一种新型氧化石墨烯/硫杂杯芳烃复合材料,用扫描电镜、红外光谱、元素分析、热分析对合成产品进行表征,用于痕量铊的富集,提出了氧化石墨烯/硫杂杯芳烃复合材料分离预富集,石墨炉原子吸收光谱法测定痕量铊的一种新方法,探讨了溶液pH值、温度、洗脱条件及干扰离子对痕量铊分离富集的影响,结果发现该材料对Tl3+具有较大吸附量.在pH 8.0,温度为(23±1)℃条件下,铊可被该材料定量吸附,其吸附容量为73.1 mg/g.吸附的铊可被5.0 mL酸性硫脲(0.5 mol/L HCl+ 1.0 mol/L硫脲)完全洗脱,方法的线性范围为0.012~15 μg/L,检出限(3σ)为0.008 μg/L,对0.50μg/L T13+工作液测定的RSD(n =7)为2.3%,加标回收率为93.6%~104.1%.此法用于生物样品和环境水样中痕量铊的测定,结果满意. A new grapheme oxide/thiacalixarene composites material was synthesized.The characterization of this material was performed by SEM,FT-IR,Element analysis and thermal analysis.A new method for the determinaon of trace thallium was developed by graphite furnace atomic absorption spectrometry(GFAAS) with the grapheme oxide/thiacalixarene composites material as adsorbent.The optimal experimental conditions (e.g.pH value of solution,temperature,elution condition) and the adsorbing principle for the determination were studied.It was found that thallium could be adsorbed on grapheme oxide/thiacalixarene composites material at pH 8.0 and temperature of (23 ± 1) ℃,and the adsorption capacity was 73.1 mg/g.The determination of trace thallium was performed by GFAAS after it was eluted with 5 mL 0.5 mol/L HC1-1.0 mol/L thiurea.The linear range of thallium ranged from 0.012 μg/L to 15 μg/L.The detection limit(3σ) was 0.008 g/L.The RSD(n =7) for 0.50 μg/L Tl3+ standard solution was 2.3%.The spiked recoveries of thallium were in the range of 93.6%-104.1%.The method was applied in the determination of trace thallium in environmental samples with satisfactory results.
出处 《分析测试学报》 CAS CSCD 北大核心 2013年第10期1242-1246,共5页 Journal of Instrumental Analysis
基金 湖南省自然科学基金项目(13JJ4102)
关键词 氧化石墨烯 硫杂杯芳烃复合材料 分离富集 石墨炉原子吸收法 grapheme oxide/thiacalixarene composites material separation/preconcentration graphite furnace atomic absorption thallium
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