The microwave induced plasma with optical emission spectrometry (MIP–OES) in 23 elements determination in geological samples P. Niedzielski a,n , L. Kozak a,b , M. Wachelka a,c , K. Jakubowski a , J. Wybieralska d a Adam Mickiewicz University in Poznań, Faculty of Chemistry, Department of Analytical Chemistry, 89B Umultowska Street, 61-614 Poznan, Poland b Poviat Sanitary and Epidemiological Station in Poznań, Department of Food, Nutrition and Food Contact Materials, 10 Sieroca Street, 61-771 Poznan, Poland c Selwa-Lab, 56 Okopowa Street, 01-042 Warsaw, Poland d Adam Mickiewicz University in Poznan, Faculty of Chemistry, Environmental Laboratory of Unique Analytical Instrumentation, 89B Umultowska Street, 61-614 Poznan, Poland article info Article history: Received 4 July 2014 Received in revised form 28 September 2014 Accepted 8 October 2014 Available online 19 October 2014 Keywords: Microwave induced plasma optical emission spectrometry X-ray fluorescence Atomic absorption spectrometry Multielemental analysis Geological samples abstract The article presents the optimisation, validation and application of the microwave induced plasma optical emission spectrometry (MIP–OES) dedicated for a routine determination of Ag, Al, B, Ba, Bi, Ca, Cd, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Mo, Na, Ni, Pb, Sr, Tl, Zn, in the geological samples. The three procedures of sample preparation has been proposed: sample digestion with the use of hydrofluoric acid for determination of total concentration of elements, extraction by aqua regia for determination of the quasi-total element concentration and extraction by hydrochloric acid solution to determine contents of the elements in acid leachable fraction. The detection limits were on the level 0.001–0.121 mg L À1 (from 0.010–0.10 to 1.2–12 mg kg À1 depend on the samples preparation procedure); the precision: 0.20–1.37%; accuracy 85–115% (for recovery for certified standards materials analysis and parallel analysis by independent analytical techniques: X-ray fluorescence (XRF) and flame absorption spectrometry (FAAS)). The conformity of the results obtained by MIP–OES analytical procedures with the results obtained by XRF and FAAS analysis allows to propose the procedures for studies of elemental composition of the fraction of the geological samples. Additionally, the MIP–OES technique is much less expensive than ICP techniques and much less time-consuming than AAS techniques. & 2014 Elsevier B.V. All rights reserved. 1. Introduction The microwave induced plasma optical emission spectrometry (MIP–OES), besides different spectrometric techniques as inductively coupled plasma optical emission spectrometry (ICP–OES), inductively coupled plasma mass spectrometry (ICP–MS), atomic absorption spe ctrometry (AAS) or atomic fluorescence spectrometry (AFS) techni- ques has been designed for elements determination in various samples [1]. The relatively short history (the first analytical applica- tion in 1963 [2]) and late (2011) commercialization of instruments [3] caused a small popularity of the technique. The application of determination of selected elements as e.g. Na [4], Cu, Cr, Mn, Fe, Cd, Zn, Ni, Au [5], Ag, Pd, Pt [6], Hg [7], K, Ca, Mg, Sr [8], Cl, Br [9], Si [10], Ba, Pb [11] first of all have based on laboratory-made analytical instruments. The different plasma gases has been used in MIP–OES technique: argon [5,6] or helium [7,9], but the use of nitrogen [12] (generating from atmospheric air) allowed significantly decrease the operating costs [10] and made the technique competitive to induc- tively coupled plasma based techniques [3]. The most of MIP–OES studies were concentrated on the optimi- sation of the analytical systems to obtain the lowest detection limits with satisfactory precision and accuracy [7]. The more efficient nebulisers (as ultrasonic nebuliser (US)) [13], the hydride generation and introducing in the plasma, connected with the US nebulizer [14,15] or direct solid samples introduction as a slurry [16–18] have been applied. The MIP–OES spectrometry (besides ICP–OES, ICP–MS, AAS or AFS techniques) has been successfully used as chromatographic detector in hyphenated techniques [19,20]. Both in gas chromato- graphy (GC) [21,22], capillary electrophoresis (CE) [23,24] or high performance liquid chromatography (HPLC) [25] the MIP–OES detectors allowed to determine elements (e.g. Se, [22] Cu, [23] As, [24] Cr [25]) species. Commercialisation of GC–MIP–OES instrumen- tation made this hyphenated techniques the most popular utiliza- tion of MIP–OES technique [26]. The article presents the application of the new analytical tech- nique of MIP–OES to multielemental analysis of geological samples using Agilent 4100 MP-AES spectrometer, the first commercially Contents lists available at ScienceDirect journal homepage: www.elsevier.com/locate/talanta Talanta http://dx.doi.org/10.1016/j.talanta.2014.10.009 0039-9140/& 2014 Elsevier B.V. All rights reserved. n Corresponding author. E-mail address: pnied@amu.edu.pl (P. Niedzielski). Talanta 132 (2015) 591–599