000132282 001__ 132282
000132282 005__ 20260112133216.0
000132282 0247_ $$2doi$$a10.1039/d3ja00271c
000132282 0248_ $$2sideral$$a137530
000132282 037__ $$aART-2024-137530
000132282 041__ $$aeng
000132282 100__ $$0(orcid)0000-0001-9582-6283$$aRua-Ibarz, Ana$$uUniversidad de Zaragoza
000132282 245__ $$aA comparison of calibration strategies for quantitative laser ablation ICP-mass spectrometry (LA-ICP-MS) analysis of fused catalyst samples
000132282 260__ $$c2024
000132282 5060_ $$aAccess copy available to the general public$$fUnrestricted
000132282 5203_ $$aIn the field of petrochemistry, the quantitative determination of trace elements in catalysts is crucial for optimizing various types of processes. Catalyst poisoning, resulting from the presence of contaminants, can lead to decreased performance and efficiency, even when these are present at trace level only. Inductively coupled plasma-mass spectrometry (ICP-MS) is a powerful technique for trace elemental analysis, but its application to catalysts is challenging due to their physicochemical characteristics challenging straightforward dissolution. Laser ablation (LA) coupled to ICP-MS (LA-ICP-MS) has emerged as a valuable approach for direct analysis of solid samples. However, developing an appropriate calibration strategy for reliable quantitative LA-ICP-MS analysis of catalyst samples remains a challenge. In this work, different calibration strategies for quantitative LA-ICP-MS analysis of fused catalyst samples were evaluated. The traditional strategy relied on external calibration against certified reference materials (CRMs) combined with internal standardization and was considered the reference approach. When using this approach, the relative bias with respect to the reference value was found to be <15%. Two novel calibration strategies were introduced and compared: a so-called multi-signal calibration approach and a solution-based calibration approach. The multi-signal calibration strategy involved varying the laser repetition rate (20, 30, 40 and 50 Hz) or laser beam diameter (10, 12, 15 and 20 μm), allowing a calibration curve to be constructed by comparing the analytical signal intensity for a single solid CRM with that for the sample, thus partially overcoming the shortage of CRMs for quantitative LA-ICP-MS analysis. The solution-based calibration approach was used for quantitative multi-element analysis without the need for any solid standard and required only minor hardware modifications to accommodate the introduction of aqueous standard solutions for calibration. Various glass certified reference materials were used for method development, calibration, and validation purposes. Furthermore, two fused alumina catalyst samples (used in the context of petroleum refining processes) were successfully analyzed as a proof-of-concept application. For both the multi-signal (matrix-matched conditions) and the solution-based calibration approaches, the average relative bias between the experimentally determined and certified/reference concentrations varied between −9% and +7%.
000132282 536__ $$9info:eu-repo/grantAgreement/ES/DGA/E43-20R$$9info:eu-repo/grantAgreement/EC/H2020/101034288/EU/International Fellowship Programme for Talent Attraction to the Campus of International Excellence Campus Iberus/IberusExperience$$9This project has received funding from the European Union’s Horizon 2020 research and innovation program under grant agreement No H2020 101034288-IberusExperience$$9info:eu-repo/grantAgreement/ES/MICINN/PID2021-122455NB-I00$$9info:eu-repo/grantAgreement/ES/MICINN/RYC2021-031093-I
000132282 540__ $$9info:eu-repo/semantics/openAccess$$aby$$uhttps://creativecommons.org/licenses/by/4.0/deed.es
000132282 590__ $$a3.1$$b2024
000132282 592__ $$a0.618$$b2024
000132282 591__ $$aSPECTROSCOPY$$b9 / 44 = 0.205$$c2024$$dQ1$$eT1
000132282 593__ $$aSpectroscopy$$c2024$$dQ2
000132282 591__ $$aCHEMISTRY, ANALYTICAL$$b44 / 111 = 0.396$$c2024$$dQ2$$eT2
000132282 593__ $$aAnalytical Chemistry$$c2024$$dQ2
000132282 594__ $$a5.7$$b2024
000132282 655_4 $$ainfo:eu-repo/semantics/article$$vinfo:eu-repo/semantics/publishedVersion
000132282 700__ $$aVan Acker, Thibaut
000132282 700__ $$0(orcid)0000-0002-1856-2058$$aBolea-Fernández, Eduardo$$uUniversidad de Zaragoza
000132282 700__ $$aBoccongelli, Marina
000132282 700__ $$aVanhaecke, Frank
000132282 7102_ $$12009$$2750$$aUniversidad de Zaragoza$$bDpto. Química Analítica$$cÁrea Química Analítica
000132282 773__ $$g39, 3 (2024), 888-899$$pJ. anal. at. spectrom.$$tJournal of Analytical Atomic Spectrometry$$x0267-9477
000132282 8564_ $$s1450676$$uhttps://zaguan.unizar.es/record/132282/files/texto_completo.pdf$$yVersión publicada
000132282 8564_ $$s2658450$$uhttps://zaguan.unizar.es/record/132282/files/texto_completo.jpg?subformat=icon$$xicon$$yVersión publicada
000132282 909CO $$ooai:zaguan.unizar.es:132282$$particulos$$pdriver
000132282 951__ $$a2026-01-12-12:44:04
000132282 980__ $$aARTICLE