PMID- 33621935 OWN - NLM STAT- PubMed-not-MEDLINE DCOM- 20210323 LR - 20210323 IS - 1873-3557 (Electronic) IS - 1386-1425 (Linking) VI - 253 DP - 2021 May 15 TI - Efficiency enhancement of the spectrophotometric estimation of cobalt in waters and pharmaceutical preparations using dispersive liquid-liquid microextraction and microcells with long optical paths. PG - 119552 LID - S1386-1425(21)00128-1 [pii] LID - 10.1016/j.saa.2021.119552 [doi] AB - In this paper, dispersive liquid-liquid microextraction (DLLME), long optical path microcells, and a selective chromogenic reagent were employed to improve the analytical efficiency of cobalt determination by spectrophotometry. The methodology proposed in the present study is based upon the microextraction of a cobalt(II) complex with 1-[4-[(2-hydroxynaphthalen-1-yl)methylideneamino] phenyl]ethanone (HNE) by DLLME and measurement of the absorbance of the sedimented phase using a microcell with an optical path length of 50 mm (Microcell-50). DLLME was performed using a binary mixture containing 900 muL of methanol as a dispersing solvent and 400 muL of CHCl(3) (extraction solvent) at pH 6-8 adjusted by a mixture of HCl and NaOH. The electronic spectrum of the dark brown complex recorded in the sedimented phase using Microcell-50 shows a well-defined peak at lambda(max) 324 +/- 3 nm with a molar absorptivity of 1.08 x 10(6) M(-1) cm(-1). Cobalt was monitored at a detection limit (LOD) of 0.08 mug L(-1) and in the linear concentration range of 0.45-10 mug L(-1), while the limit of quantitation (LOQ), relative standard deviation (RSD), and the enhancement factor (EF) were 0.264, 1.6 mugL(-1), and 223, respectively. Our method was evaluated by determining cobalt in certified reference materials and experimental samples, and the results were compared with ICP-MS measurements. Moreover, the chemical structure of the [Co(C(38)H(28)O(2)N)(2)] complex was suggested through using different characterization techniques such as Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), thermal analysis, and powder X-ray diffraction. CI - Copyright (c) 2021 Elsevier B.V. All rights reserved. FAU - Al-Saidi, Hamed M AU - Al-Saidi HM AD - Department of Chemistry, University College in Al - Jamoum, Umm Al-Qura University, 21955 Makkah, Saudi Arabia. Electronic address: hmsaidi@uqu.edu.sa. FAU - Alharthi, Salman S AU - Alharthi SS AD - Department of Chemistry, College of Science, Taif University, P.O. Box 11099, Taif 21944, Saudi Arabia. LA - eng PT - Journal Article DEP - 20210205 PL - England TA - Spectrochim Acta A Mol Biomol Spectrosc JT - Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy JID - 9602533 SB - IM OTO - NOTNLM OT - Characterization OT - Cobalt OT - Determination OT - Microcell OT - Spectrophotometry COIS- Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. EDAT- 2021/02/24 06:00 MHDA- 2021/02/24 06:01 CRDT- 2021/02/23 20:14 PHST- 2020/10/13 00:00 [received] PHST- 2021/01/09 00:00 [revised] PHST- 2021/01/26 00:00 [accepted] PHST- 2021/02/24 06:00 [pubmed] PHST- 2021/02/24 06:01 [medline] PHST- 2021/02/23 20:14 [entrez] AID - S1386-1425(21)00128-1 [pii] AID - 10.1016/j.saa.2021.119552 [doi] PST - ppublish SO - Spectrochim Acta A Mol Biomol Spectrosc. 2021 May 15;253:119552. doi: 10.1016/j.saa.2021.119552. Epub 2021 Feb 5.