Pérez-Quintanilla Damián, Sánchez Alfredo, del Hierro Isabel, Fajardo Mariano, Sierra Isabel
Departamento de Química Inorgánica y Analítica, ESCET, Universidad Rey Juan Carlos, C/Tulipán s/n, 28933 Móstoles, Madrid, Spain.
J Hazard Mater. 2009 Jul 30;166(2-3):1449-58. doi: 10.1016/j.jhazmat.2008.12.065. Epub 2008 Dec 24.
A SBA-15 mesoporous silica has been chemically modified with 5-mercapto-1-methyltetrazole. The newly synthesized material (MTTZ-SBA-15) has been characterized, by powder X-ray diffraction, N(2) adsorption, FT-IR, (13)C NMR spectroscopy and elemental analysis, and used to preconcentrate Zn(II) in water samples. The effect of some variables on the adsorption capacity has been studied using the column techniques. The adsorption capacity of the prepared material followed the order: Zn>>Cu>Cd>>Mn, and under optimized conditions the maximum adsorption value for Zn(II) was 0.96+/-0.01 mmol/g with the adsorption efficiency of 0.76. In column experiments, adsorption was quantitative for 1000 mL of 7.65 x 10(-4)mM of Zn(II) solution and adsorbed ions were eluted out by 5 mL of 1M HCl (preconcentration factor of 200). Spiked tap water and mineral water were used for the preconcentration and determination of Zn(II) by flame atomic absorption spectrometry (FAAS), and a 102+/-2 and 98+/-3% recoveries were obtained. The LOD and LOQ values of the proposed method were found to be 8.0 x 10(-6) and 1.23 x 10(-5)mM, respectively. The relative standard deviation for four preconcentration experiments was found to be <or=4% in all cases.
一种SBA - 15介孔二氧化硅已用5 - 巯基 - 1 - 甲基四唑进行了化学修饰。通过粉末X射线衍射、N₂吸附、傅里叶变换红外光谱、¹³C核磁共振光谱和元素分析对新合成的材料（MTTZ - SBA - 15）进行了表征，并用于对水样中的Zn(II)进行预富集。使用柱技术研究了一些变量对吸附容量的影响。所制备材料的吸附容量顺序为：Zn>>Cu>Cd>>Mn，在优化条件下，Zn(II)的最大吸附值为0.96±0.01 mmol/g，吸附效率为0.76。在柱实验中，对于1000 mL 7.65×10⁻⁴ mM的Zn(II)溶液，吸附是定量的，吸附的离子用5 mL 1M HCl洗脱（预富集因子为200）。加标自来水和矿泉水用于通过火焰原子吸收光谱法（FAAS）对Zn(II)进行预富集和测定，回收率分别为102±2%和98±3%。该方法的检测限和定量限分别为8.0×10⁻⁶和1.23×10⁻⁵ mM。在所有情况下，四次预富集实验的相对标准偏差均≤4%。
