In this paper, a sensitive and simple zirconium nanoparticles (Zr-NPs) based vortex assisted ligandless dispersive solid phase extraction (VA-LDSPE) method was developed for the preconcentration of lead from wastewater samples for the determination by slotted quartz tube–flame atomic absorption spectrometry (SQT-FAAS). Zr-NPs were synthesized using zirconium (IV) chloride salt as a starting material through a simple reduction process with sodium borohydride, and used as selective adsorbent for the extraction of lead ions from aqueous medium. Single variant experiments were carried out for all optimizations of sorption/desorption steps including pH of solution, amount of nanoparticles, mixing type/period and eluent type. An SQT with five round slots was placed onto the burner of FAAS to increase the interaction between lead atoms and light from radiation source to enhance the absorbance signals. Under the determined optimum conditions, analytical figures of merit were evaluated and the limit of detection and quantification (LOD/LOQ) values were calculated as 5.2 and 17.3 µg L^− 1, respectively. The developed method showed a linear calibration range between 25 and 250 µg L^− 1 with a good regression coefficient value (0.9995). Recovery studies were also performed with domestic wastewater samples spiked at three concentrations and percent recovery values obtained in the range of 97%–102% validated the developed method’s applicability and accuracy.

本文开发了一种灵敏且简单的锆纳米粒子（Zr-NPs）涡流辅助无配体分散固相萃取（VA-LDSPE）方法，用于预富集废水样品中的铅，用于开槽石英管-火焰原子吸收法的测定。光谱法（SQT-FAAS）。以氯化锆 (IV) 盐为起始材料，通过简单的硼氢化钠还原工艺合成 Zr-NPs，并用作选择性吸附剂从水介质中提取铅离子。对吸附/解吸步骤的所有优化进行了单一变体实验，包括溶液的 pH 值、纳米颗粒的量、混合类型/周期和洗脱液类型。在 FAAS 的燃烧器上放置一个带有五个圆形槽的 SQT，以增加铅原子与辐射源光之间的相互作用，从而增强吸收信号。在确定的最佳条件下，评估分析品质因数，计算出检测和定量限 (LOD/LOQ) 值分别为 5.2 和 17.3 µg L^{- 1}，分别。开发的方法显示线性校准范围介于 25 和 250 µg L ^{- 1}之间，具有良好的回归系数值 (0.9995)。还对添加三种浓度的生活废水样品进行了回收率研究，在 97%–102% 范围内获得的回收率值验证了所开发方法的适用性和准确性。