de Sousa Juliana Menezes, Baptista Cruz Graziela Fregonez, Dos Santos Luiza Gomes, Cassella Ricardo J
Department of Analytical Chemistry, Fluminense Federal University, Outeiro de São João Batista s/n Centro, Niterói, RJ 24020-141, Brazil.
J Anal Methods Chem. 2023 May 30;2023:9624637. doi: 10.1155/2023/9624637. eCollection 2023.
In this work, a separation/preconcentration method is proposed for the determination of Cd(II) and Pb(II) in swimming pool waters, using ammonium pyrrolidine dithiocarbamate (APDC) as a complexing agent and unloaded polyurethane foam (PUF) as a sorbent. The proposed method was optimized, and the defined optimal conditions were a pH of 7, 30 min of shaking time, 400 mg of PUF, and 0.5% (m/v) of the APDC solution. The release of Cd(II) and Pb(II) from the solid phase was achieved through the total digestion of PUF using a microwave-assisted acid approach with a 10.5 mol·L HNO solution. The methodology was applied to four samples of swimming pool water for the determination of Cd(II) and Pb(II) using graphite furnace atomic absorption spectrometry (GF AAS). The limits of detection and quantification obtained were 0.02 and 0.06 g·L for Cd(II) and 0.5 e 1.8 g·L for Pb(II), respectively. We analyzed four samples of swimming pool waters, finding Cd concentrations between 0.22 and 1.37 g·L. On the other hand, only one sample presented Pb concentration above the limit of quantification (11.4 g·L). Recovery tests were performed by spiking the samples with known concentrations of the analytes, and recovery percentages between 82% and 105% were obtained.
在本研究中，提出了一种分离/预富集方法，用于测定游泳池水中的镉（II）和铅（II），该方法使用吡咯烷二硫代氨基甲酸铵（APDC）作为络合剂，以负载的聚氨酯泡沫（PUF）作为吸附剂。对所提出的方法进行了优化，确定的最佳条件为pH值7、振荡时间30分钟、400毫克PUF和0.5%（m/v）的APDC溶液。通过使用10.5摩尔·升硝酸溶液的微波辅助酸法对PUF进行完全消解，实现了镉（II）和铅（II）从固相中释放。该方法应用于四个游泳池水样品，采用石墨炉原子吸收光谱法（GF AAS）测定镉（II）和铅（II）。获得的检测限和定量限分别为镉（II）0.02和0.06微克·升，铅（II）0.5至1.8微克·升。我们分析了四个游泳池水样品，发现镉浓度在0.22至1.37微克·升之间。另一方面，只有一个样品的铅浓度高于定量限（11.4微克·升）。通过向样品中加入已知浓度的分析物进行回收率测试，获得的回收率在82%至105%之间。
