Tesis
Determinação de iodo por espectrometria de emissão óptica com plasma acoplado indutivamente com configuração axial
Fecha
2009-01-23Registro en:
OLIVEIRA, Adriana Alice de.Determination of iodine by inductively coupled plasma optical emission spectrometry with axial viewing. 2009. 92 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2009.
Autor
Oliveira, Adriana Alice de
Institución
Resumen
In this work it was evaluated the performance of an inductively coupled plasma spectrometer with axial viewed configuration for determining iodine in seafood and table salts. The emission lines of iodine were evaluated based on parameters such as signalto-background ratio (SBR), background equivalent concentration (BEC) and limit of
detection (LOD). Interference effects caused by Na+, K+, and P in the emission signals of iodine and the occurrence of memory effects in nitric acid and in water-soluble tertiaryamines (CFA-C) media were also evaluated. Factorial design 2³ + Central Point + Star, was applied for evaluating the operational conditions of the ICP OES with axial configuration and also for an other equipment with radial configuration both applied for iodine determination. An optimum instrument operational condition was established for
axial configuration and two optimum conditions for radial configuration. The axial configuration was five fold more sensitive than the radial configuration. The applicability of ICP OES with axial configuration for iodine determination was investigated. Both matrix matching and standard additions method were used for iodine quantification. For most samples, it was obtained a good agreement between both methods. Recoveries at 104 to 114 % range were reached even for samples that did not show values in
agreement when applying matrix matching or the standard additions method. Iodine determination in seafood using ICP OES with axial configuration was also investigated. Sample preparation was based on alkaline extraction (CFA-C 10% v v-1 pH 8) with ultrasound bath for 3 h at a temperature of 80 ºC. Recoveries for oyster tissue (NIST 1566b) and non-fat milk powder (NIST 1549) certified reference materials were 113 and 102 %, respectively.