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Synthesis, characterization, and application of novel Zn(II)-ionic imprinted polymer for preconcentration of Zn(II) ions from aqueous solution

机译:新型Zn(II)离子印迹聚合物的合成,表征和应用用于水溶液中Zn(II)离子的前浓缩

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Preparation of a new Zn~(2+) ion-imprinted polymer (Zn-IIP) is presented in this report. The Zn-IIP are prepared by precipitation polymerization using 8-hydroxyquinoline (8HQ) as a ligand, methacrylic acid (MAA) as functional monomer, and ethylene glycol dimethacrylate (EGDMA) as a cross-linker has been prepared. The benzoyl peroxide and ethanol/acetonitrile (2:1) mixture were used as initiator and porogen, respectively. Precipitation polymerization was carried out by heating in a water bath at 60°C for 8 hours. After polymerization, cavities in the polymer particles corresponding to the Zn~(2+) ions were created by leaching the polymer with 2 mol L~(-1) HNO3. The polymer was washed with aquabidest and dried in an oven at the temperature of 60°C for 24 hours. The Zn-IIP was characterized by Fourier Transform Infrared Spectrophotometry (FT-IR) and Scanning Electron Microscopy (SEM). The synthesized Zn-IIP was used as a new adsorbent for solid phase extraction (SPE) of Zn(II) prior to Flame Atomic Absorption Spectrometry (FAAS) determination. The experimental parameters for SPE, such as pH of the sample, loading rate, and elution volume, have been optimized. The effect of pH of the sample on the extraction of analyte was studied in batch mode. The effects of loading rate and elution volume on the extraction of analyte were studied in dynamic mode by loading of the sample through HP-SPE cartridge containing 100 mg of the synthesized Zn-IIP. The imprinted polymer (Zn-IIP) have bands at 3433.06 cm~(-1) (O-H), 1508.23 cnr~1 (C=N aromatics), 1284.5 cm~(-1) (C-N aromatics), 1056.9 cm~(-1) (C-O phenol), 1724.24 cm~(-1) (OO), and 1639.38 cm~(-1) (conjugated C=0 with C=C). The Scanning Electron Microscopy (SEM) images of IIP and IIP show that the IIP is seen to have more cavities than NIP. The optimum pH for quantitative Zn(II) retention was 5.5, and the elution was completed with 2 mL of 1.0 mol L~(-1) nitric acid. The optimum loading rate was 0.5 mL min~(-1). The recovery of Zn(II) from solution samples after its SPE extraction on IIP with 50-fold theoretical preconcentration was 94.60-104.50%. The LOD and LOQ with 50-fold theoretical preconcentration obtained were 0.0073 mg L~(-1) and 0.0244 mg L~(-1), respectively.
机译:本报告中提出了新的Zn〜(2+)离子印迹聚合物(Zn-IIP)的制备。通过使用8-羟基喹啉(8HQ)作为配体,作为功能单体的甲基丙烯酸(MAA)作为功能单体,并制备作为交联剂的乙二醇二甲基丙烯酸酯(EGDMA)的沉淀聚合来制备Zn-IIP。过氧化苯甲酰和乙醇/乙腈(2:1)混合物分别用作引发剂和孔胶。通过在60℃的水浴中加热8小时,进行沉淀聚合。聚合后,通过将聚合物与2mol L〜(-1)HNO3浸出,产生与Zn〜(2+)离子对应的聚合物颗粒中的空腔。将聚合物用AquabIDEST洗涤,并在60℃的温度下在烘箱中干燥24小时。 Zn-IIP的特征在于傅里叶变换红外分光光度法(FT-IR)和扫描电子显微镜(SEM)。在火焰原子吸收光谱(FAAS)测定中,合成的Zn-IIP用作Zn(II)的固相萃取(SPE)的新吸附剂。已经优化了SPE的实验参数,例如样品,装载速率和洗脱体积的pH。在分批模式中研究了样品对样品对萃取的影响。通过含有100mg合成的Zn-IIP的HP-SPE盒在动态模式下研究了加载速率和洗脱体积对分析物提取的影响。印迹聚合物(Zn-IIP)具有3433.06cm〜( - 1)(OH),1508.23 CNR〜1(C = N芳烃),1284.5cm〜(-1)(CN芳烃),1056.9cm〜( - 1)(CO苯酚),1724.24cm〜(-1)(OO)和1639.38cm〜(-1)(用C = C缀合C = 0)。 IIP和IIP的扫描电子显微镜(SEM)图像表明IIP被认为具有比辊隙更多的空腔。定量Zn(II)保留的最佳pH为5.5,用2mL 1.0mol L〜(-1)硝酸完成洗脱。最佳加载率为0.5ml min〜(-1)。在具有50倍理论前浓缩的IIP对IIP的SPE提取后,从溶液样品中回收Zn(II)的回收率为94.60-104.50%。得到50倍理论前浓缩的LOD和LOQ分别为0.0073mg L〜(-1)和0.0244mg L〜(-1)。

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