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Talanta. 2016 Jul 1;154:416-22. doi: 10.1016/j.talanta.2016.03.096. Epub 2016 Mar 31.

Selective extraction by dissolvable (nitriloacetic acid-nickel)-layered double hydroxide coupled with reaction with potassium thiocyanate for sensitive detection of iron(III).

Author information

1
Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore.
2
Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore Environmental Research Institute, T-Lab Building #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore; Tropical Marine Science Institute, National University of Singapore, S2S, 18 Kent Ridge Road, Singapore 119227, Singapore. Electronic address: chmleehk@nus.edu.sg.

Abstract

A highly selective method has been proposed for the determination of iron cation (Fe(3+)). (Nitriloacetic acid-nickel)-layered double hydroxide ((NTA-Ni)-LDH) was successfully synthesized and used as dissolvable sorbent in dispersive solid-phase extraction to pre-concentrate and separate Fe(3+) from aqueous phase. Since Fe(3+) has a larger formation constant with NTA compared to Ni(2+), subsequently ion exchange occurred when (NTA-Ni)-LDH was added to the sample solution. The resultant (NTA-Fe)-LDH sol was isolated and transferred in an acidic medium containing potassium thiocyanate (KSCN). Since (NTA-Fe)-LDH could be dissolved in acidic conditions, Fe(3+)was released and reacted with SCN(-) to form an Fe-SCN complex. The resulting product was measured by ultraviolet-visible spectrometry for quantitative detection of Fe(3+). Extraction factors, including sample pH, reaction pH, extraction temperature, extraction time, reaction time and concentration of KSCN were optimized. This method achieved a low limit of detection of 15.2nM and a good linear range from 0.05 to 50μM (r(2)=0.9937). A nearly 18-fold enhancement of signal intensity was achieved after selective extraction. The optimized conditions were validated by applying the method to determine Fe(3+) in seawater samples.

KEYWORDS:

dissolvable sorbent; ferric iron; layered double hydroxide; nitriloacetic acid; selective extraction

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