Multivariate optimization and simultaneous determination of hydride and non-hydride-forming elements in samples of a wide pH range using dual-mode sample introduction with plasma techniques: application on leachates from cement mortar material

Mulugeta, Mesay; Wibetoe, Grethe; Engelsen, Christian J.; Asfaw, Alemayehu
February 2009
Analytical & Bioanalytical Chemistry;Feb2009, Vol. 393 Issue 3, p1015
Academic Journal
Analytical methods have been developed for the simultaneous determination of hydride-forming (As, Sb) and non-hydride-forming (Cr, Mo, V) elements in aqueous samples of a wide pH range (pH 3–13). The methods used dual-mode (DM) sample introduction with ICP-AES and ICP-MS instruments. The effect of selected experimental variables, i.e., sample pH and concentrations of HNO3, thiourea, and NaBH4, were studied in a multivariate way using face-centered central composite design (FC-CCD). Compromised optimum values of the experimental parameters were identified using a response optimizer. The statistically found optimum values were verified experimentally. The methods provided improved sensitivities for the hydride-forming elements compared with the respective conventional nebulization (Neb) systems by factors of 67 (As) and 64 (Sb) for ICP-AES and 36 (As) and 54 (Sb) for ICP-MS. Slight sensitivity improvements were also observed for the non-hydride-forming elements. The limits of detection (LOD) of As and Sb were lowered, respectively, to 0.8 and 0.9 μg L−1 with the DM-ICP-AES system and to 0.01 and 0.02 μg L−1 with the DM-ICP-MS system. The short-term stabilities of both methods were between 2.1 and 5.4%. The methods were applied for the analysis of leachates of a cement mortar material prepared in the pH range 3–13. The elemental concentration of the leachates determined by the two DM methods were statistically compared with the values obtained from Neb-ICP-MS analysis; the values showed good agreement at the 95% confidence level. Quantitative spike recoveries were obtained for the analytes from most of the leachates using both DM methods. [Figure not available: see fulltext.]


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