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叶陆芳, 宋小华, 余代顺, 杨小慢, 谢文根, 吴少尉. 固相萃取掺氧空气-乙炔火焰原子吸收光谱法测定水和植物样品中的痕量镓[J]. 岩矿测试, 2020, 39(2): 243-250. DOI: 10.15898/j.cnki.11-2131/td.201905280073
引用本文: 叶陆芳, 宋小华, 余代顺, 杨小慢, 谢文根, 吴少尉. 固相萃取掺氧空气-乙炔火焰原子吸收光谱法测定水和植物样品中的痕量镓[J]. 岩矿测试, 2020, 39(2): 243-250. DOI: 10.15898/j.cnki.11-2131/td.201905280073
YE Lu-fang, SONG Xiao-hua, YU Dai-shun, YANG Xiao-man, XIE Wen-gen, WU Shao-wei. Determination of Trace Ga in Water and Plant Samples by O2-doped Air-Acetylene FAAS with Solid Phase Extraction Preconcentration[J]. Rock and Mineral Analysis, 2020, 39(2): 243-250. DOI: 10.15898/j.cnki.11-2131/td.201905280073
Citation: YE Lu-fang, SONG Xiao-hua, YU Dai-shun, YANG Xiao-man, XIE Wen-gen, WU Shao-wei. Determination of Trace Ga in Water and Plant Samples by O2-doped Air-Acetylene FAAS with Solid Phase Extraction Preconcentration[J]. Rock and Mineral Analysis, 2020, 39(2): 243-250. DOI: 10.15898/j.cnki.11-2131/td.201905280073

固相萃取掺氧空气-乙炔火焰原子吸收光谱法测定水和植物样品中的痕量镓

Determination of Trace Ga in Water and Plant Samples by O2-doped Air-Acetylene FAAS with Solid Phase Extraction Preconcentration

  • 摘要: 目前研究萃取分离富集镓大多偏向在强酸性体系中,一定程度上给操作带来安全风险,另需耐酸器皿设备,易污染,空白背景值高。本文开发了一种在弱酸性条件下萃取分离富集痕量镓的方法。以大孔吸附树脂为载体,十六烷基三甲基溴化铵调节其表面极性,热固化负载2-乙基己基磷酸(2-乙基己基)酯,制备了镓的萃取树脂。动态考察了固相萃取镓的吸附容量,优化选择固相萃取分离富集条件,实验表明萃取条件温和,分离富集痕量镓效果理想。当溶液酸度为pH 2.5时,Ga(Ⅲ)达到最大的回收率99%,并确定了掺氧空气乙炔火焰原子吸收光谱法(FAAS)测定镓的最佳参数,提升了常规空气乙炔FAAS测定镓的灵敏度。方法检出限(3σ)为2.6ng/mL,相对标准偏差(RSD,n=7)为2.87%,加标回收率在95.7%~102.0%之间,理论富集倍数为40。本方法已应用于自来水、中药材和水培蔬菜样品中痕量镓的测定,简便、快速、可靠。

     

    Abstract:
    BACKGROUNDAt present, research on the extraction separation and enrichment of gallium is mostly biased to the strong acidic system, which brings a safety risk to the operation and needs acid-proof apparatus. Furthermore, the procedure is easily contaminated, resulting in high background values.
    OBJECTIVESTo develop a method for extraction separation and preconcentration of trace Ga under weakly acidic condition.
    METHODSSolid phase extraction medium for Ga was prepared by using modified large porous adsorption resin with cetyl-trimethyl-ammonium bromide and loading it with 2-ethylhexyl phosphonic acid-2-ethylhexyleste. The separation and enrichment conditions of solid phase extraction were studied in detail.
    RESULTSExperiments showed that the separation and enrichment of trace gallium was ideal when the extraction conditions were mild. The maximum recovery (99%) of Ga was achieved in sample solution with pH of 2.5. The determination parameters of gallium were optimized for oxygen doped air-acetylene flame atomic absorption spectrometry (FAAS), and the sensitivity was improved on that of the current method. The detection limit of the overall method (3σ) was 2.6ng/mL by IUPAC definition and the relative standard deviation (RSD, n=7) was 2.87%. The recoveries for spiked solution ranged from 95.7% to 102.0%, and a theory enrichment factor of 40 was obtained.
    CONCLUSIONSThis method has been successfully applied to the determination of trace gallium in tap water, Chinese medicine and hydroponic vegetable samples. It is simple, quick and reliable.

     

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