Kara Derya, Fisher Andrew, Hill Steve J
Department of Chemistry, Art and Science Faculty, Balikesir University, 10100 Balikesir, Turkey.
Analyst. 2006 Nov;131(11):1232-40. doi: 10.1039/b607300j. Epub 2006 Sep 11.
XAD copolymer resins may be functionalized with heavy metal ion-selective ligands either by covalent linkage to the polymer backbone or by impregnation. These resins may be tailored to be specific for certain heavy metals by adjusting the retention and elution parameters. For the synthesis of immobilized Amberlite XAD-4 copolymer resins that are expected to preconcentrate a number of transition and heavy metals, the Schiff base method was chosen. For this purpose the copolymer was nitrated, reduced to the corresponding amine and converted to the imine compounds via a Schiff base reaction using different organic aldehyde compounds. The interactions of 8 elements (Cd, Co, Cu, Mn, Ni, Pb, U and Zn) with the resins were qualitatively investigated. Optimal pH for retention was typically 6-8 for most resins although one could be used at pH 5 and elution was achieved using 0.1 M HNO3. The resins were characterized by FTIR, SEM and elemental analysis. It was demonstrated that the resins could be used to preconcentrate ultra-trace analytes from natural waters, and analysis of environmental certified reference materials using FI-ICP-MS showed good agreement with the certified values. Metal retention capacities were also calculated using a batch system and were found to compare favorably with other resins reported in the literature.
XAD共聚物树脂可以通过与聚合物主链共价连接或浸渍的方式,用重金属离子选择性配体进行功能化。通过调整保留和洗脱参数,可以使这些树脂针对特定的重金属进行定制。为了合成预期能预富集多种过渡金属和重金属的固定化Amberlite XAD - 4共聚物树脂,选择了席夫碱法。为此,先将共聚物硝化,还原为相应的胺,然后使用不同的有机醛化合物通过席夫碱反应转化为亚胺化合物。对8种元素(镉、钴、铜、锰、镍、铅、铀和锌)与树脂的相互作用进行了定性研究。大多数树脂保留的最佳pH值通常为6 - 8,不过也可以在pH值为5时使用,洗脱则使用0.1 M硝酸。通过傅里叶变换红外光谱(FTIR)、扫描电子显微镜(SEM)和元素分析对树脂进行了表征。结果表明,这些树脂可用于预富集天然水中的超痕量分析物,使用流动注射电感耦合等离子体质谱(FI - ICP - MS)对环境标准参考物质进行分析,结果与认证值吻合良好。还使用分批系统计算了金属保留容量,发现与文献中报道的其他树脂相比具有优势。