Chamsaz Mahmoud, Arbab-Zavar Mohammad Hossien, Darroudi Abolfazl, Salehi Thiery
Department of Chemistry, Faculty of Science, Ferdowsi University of Mashhad, Mashhad, Iran.
J Hazard Mater. 2009 Aug 15;167(1-3):597-601. doi: 10.1016/j.jhazmat.2009.01.019. Epub 2009 Jan 16.
A simple single drop liquid-phase microextraction (SDME) technique, combined with electrothermal atomic absorption spectroscopy (ETAAS) is developed both to preconcentrate and determine thallium (I) ions in aqueous solutions. The ions were transferred from 10.0 ml of aqueous sample (donor phase) containing 0.5 ml of 1% picric acid as the ion-pair agent into a 3 microl microdrop of nitrobenzene (acceptor phase) containing dicyclohexano-18-crown-6 as the complexing agent. The latter will help to improve the extraction efficiency of the analyte. After the ions have been extracted, the acceptor drop was directly injected into a graphite furnace for thallium (I) determination. Several parameters such as the extracting solvent, extraction time, temperature, concentration of picric acid and crown ether, drop volume and stirring rate were examined. Under the optimized experimental conditions, the detection limit (L.O.D.) was 0.7 ng ml(-1). The relative standard deviation for five replicate analysis of 10 ng ml(-1) of thallium (I) was 5.1%. The calibration curve was linear in the range of 3-22 ng ml(-1). The results for determination of thallium in reference material, spiked tap water and seawater demonstrated the accuracy, recovery and applicability of the presented method. The enrichment factor was 50.
开发了一种简单的单滴液相微萃取(SDME)技术,并将其与电热原子吸收光谱法(ETAAS)相结合,用于预富集和测定水溶液中的铊(I)离子。将含有0.5 ml 1%苦味酸作为离子对试剂的10.0 ml水样(供体相)中的离子转移到含有二环己基-18-冠-6作为络合剂的3微升硝基苯微滴(受体相)中。后者有助于提高分析物的萃取效率。离子萃取后,将受体微滴直接注入石墨炉中进行铊(I)的测定。考察了萃取溶剂、萃取时间、温度、苦味酸和冠醚浓度、微滴体积和搅拌速率等参数。在优化的实验条件下,检测限为0.7 ng ml⁻¹。对10 ng ml⁻¹铊(I)进行五次重复分析的相对标准偏差为5.1%。校准曲线在3 - 22 ng ml⁻¹范围内呈线性。参考物质、加标自来水和海水中铊的测定结果证明了该方法的准确性、回收率和适用性。富集因子为50。