Analytical Sciences

Abstract − Analytical Sciences, 30(3), 389 (2014).

Preconcentration and Determination of Trace Silver Ion Using Benzothiazole Calix[4]arene Modified Silica by Flow Injection Flame Atomic Absorption Spectrometry
Department of Chemistry, Faculty of Science, Chulalongkorn University, Bangkok 10330, Thailand
The silica gel modified with benzothiazole calix[4]arene (APS-L1) via Schiff’s base reaction was applied as a sorbent in an online system for preconcentration and determination of silver ion by flame atomic absorption spectrometry (FAAS). APS-L1 was used as an effective sorbent for solid phase extraction (SPE) of silver(I) ion in both batch and column methods. The optimum experimental parameters such as pH, eluent type, sample flow rate, eluent volume and eluent flow rate including the effect of interfering ions were investigated. Silver(I) ion was determined at pH 6 – 7. The capacity of APS-L1 sorbent was found to be 12.2 mg/g of sorbent. The high affinity was obtained without interference from the interfering ions. The optimum conditions of the online flow injection preconcentration coupled with the FAAS (FI-FAAS system) were evaluated. The sample flow rate was 3.0 mL min−1 using sample volume of 5 – 10 mL. Elution was performed with 250 μL of 0.1 mol L−1 thiosulfate at the flow rate of 1.5 mL min−1. The analytical characteristics and performance of the FI-FAAS system were studied under optimum conditions using a solution spiked with standard silver(I) ion at 20 and 50 μg L−1. The detection limit of 0.44 μg L−1 was obtained. The accuracy of the proposed method was evaluated and percentages of recovery at 20 and 50 μg L−1 were 100.2 and 99.5%, respectively. The percent relative standard deviations (%RSD) at 20 and 50 μg L−1 were 6.1 and 3.3%, respectively. The developed method was successfully applied to determine trace silver(I) ion in drinking and tap water samples.