Issue 11, 2023

Analysis of PbBi eutectic after matrix separation by acid induced dispersive liquid–liquid microextraction followed by HR-CS-ETAAS determination

Abstract

A simple acid-induced surfactant assisted dispersive liquid–liquid microextraction procedure, AI-SA-DLLME, is delineated to detect trace impurities in lead–bismuth eutectic, LBE, using ETAAS after simultaneous separation of the major matrix elements such as lead and bismuth. In this process, matrix elements form reactive anionic iodide species, PbI42− and BiI4 in the presence of mixed mineral acids and iodide. These species simultaneously react with cationic head groups of cetyl trimethyl ammonium bromide (CTAB) hydrophilic dispersing micelles and form extractable hydrophobic ion-associates, PbI42−-(CTAB)2 and BiI4-CTAB. These ion associates are extracted from the bulk aqueous phase into a small micelle rich organic phase in the presence of sulphuric acid using chloroform. The extraction efficiency of lead and bismuth is found to be more than 99.4%. The trace impurities such as As, Be, Cd, Cr, Cu, Fe, Mn, Ni, Sb, Te and Tl in the aqueous phase are determined using ETAAS. The parameters affecting the process are optimized. Under the optimized conditions, the spike recoveries of impurities are found to be between 90 and 104%, and relative standard deviations within and between the processes are between 2% and 10%; and 6% and 15%, respectively. The accuracy of the procedure is verified by comparing the values obtained from ETAAS with those of ICP-OES. The good agreement between values indicates the validity of the procedures. The limits of detection obtained for Cd, Cr, Cu, Fe, Ni, As, Be, Mn, Sb, Te and Tl are 3, 120, 300, 360, 40, 30, 1, 2, 80, 90 and 40 ng g−1 respectively. This procedure is applied to real Pb–Bi eutectic matrices.

Graphical abstract: Analysis of PbBi eutectic after matrix separation by acid induced dispersive liquid–liquid microextraction followed by HR-CS-ETAAS determination

Article information

Article type
Paper
Submitted
01 Yan 2023
Accepted
31 Mha 2023
First published
11 Ndz 2023

J. Anal. At. Spectrom., 2023,38, 2332-2341

Analysis of PbBi eutectic after matrix separation by acid induced dispersive liquid–liquid microextraction followed by HR-CS-ETAAS determination

K. Madhavi, G. Venkateswarlu, N. N. Meeravali and A. C. Sahayam, J. Anal. At. Spectrom., 2023, 38, 2332 DOI: 10.1039/D3JA00036B

To request permission to reproduce material from this article, please go to the Copyright Clearance Center request page.

If you are an author contributing to an RSC publication, you do not need to request permission provided correct acknowledgement is given.

If you are the author of this article, you do not need to request permission to reproduce figures and diagrams provided correct acknowledgement is given. If you want to reproduce the whole article in a third-party publication (excluding your thesis/dissertation for which permission is not required) please go to the Copyright Clearance Center request page.

Read more about how to correctly acknowledge RSC content.

Social activity

Spotlight

Advertisements