Abstract

This study deals with B, S, and P determination in mineral fertilizer and S in commercial sulfur-formulation using inductively coupled plasma optical emission spectrometry. According to multivariate optimization using a Doehlert matrix, the analytes extraction in fertlizer can be conducted in open flask and heating on hot plate or in closed flask in microwave oven. However, when S is present in its elemental form in the fertilizer, the sample must be decomposed in closed flask in microwave oven for accurate S quantification. The uncertainties of the method were estimated according to the bottom-up approach, which were 7.1, 4.3, and 7.8% for B, S and P, respectively. The main sources of uncertainty identified were the intermediate precision, accuracy, regression of the calibration curve and errors originated from volumetric flasks and pipettes. Satisfactory results were obtained in the analysis of certified reference materials and sample from inter-laboratory programs as well as S recovery in a commercial elemental sulfur sample.

Highlights

  • Mineral fertilizer is the seventh most imported product in Brazil, corresponding to 3.7% of imports in 2014, or about 8.5 billion dollars.[1]

  • In 2006 the Association of Analytical Communities (AOAC) International proposed an official method of analysis (OMA) for determination of As, Cd, Co, Cr, Pb, Mo, Ni and Se by inductively coupled plasma optical emission spectrometry (ICP OES).[13]

  • The AOAC International has proposed the determination of B,14 P15 and S16 by means of ICP OES

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Summary

Introduction

Mineral fertilizer is the seventh most imported product in Brazil, corresponding to 3.7% of imports in 2014, or about 8.5 billion dollars.[1]. The Brazilian National Standards Organization (Associação Brasileira de Normas Técnicas, ABNT) has not published any standard on this subject yet.[12] in 2006 the Association of Analytical Communities (AOAC) International proposed an official method of analysis (OMA) for determination of As, Cd, Co, Cr, Pb, Mo, Ni and Se by ICP OES.[13] The AOAC International has proposed the determination of B,14 P15 and S16 by means of ICP OES These proposals are not yet official methods (at least in Brazil) and the use of ICP OES is still being discussed by AOAC.[17]

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