DETERMINAÇÃO DE POTÁSSIO EM ROCHAS SILICÁTICAS POR ESPECTROMETRIA DE EMISSÃO ATÔMICA COM CHAMA APÓS DISSOLUÇÃO ASSISTIDA POR ULTRASSOM
This work presents the development of an analytical method for sample preparation aiming at the K determination in silicate rocks (basalt, monzogranite and shale fines) following ultrasound dissolution and analysis by F AES. Sample preparation method was optimized by using fractional factorial designs. The following optimal conditions were obtained for each silicate rock: 0.1 g of sample mass for any of the three samples, and volumes of HNO3, HCl and HF, respectively, of 2.5, 0.8 and 2.5 mL for basalt; 3.5, 0.8 and 2.5 mL for monzogranite, and 2.5, 1.0 and 2.0 mL for shale fines. Sample dissolution was achieved by using the ultrasound bath at room temperature (25 °C) for 1 hour. The accuracy was evaluated through the analysis of two certified reference materials, for which there was no statistical difference between the certified and the found K concentration values (95% confidence level). The K concentrations determined were: 1.45 ± 0.01 for basalt; 4.19 ± 0.03 for monzogranite and 1.60 ± 0.02 for shale fines. The developed method presented accurate and reliable results for K amounts in silicate rocks and is simple and safe, which are important features for the implementation of a methodology as a routine analysis.
| Main Authors: | , , , , , |
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| Format: | Digital revista |
| Language: | Portuguese |
| Published: |
Sociedade Brasileira de Química
2018
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| Online Access: | http://old.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422018001001095 |
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| Summary: | This work presents the development of an analytical method for sample preparation aiming at the K determination in silicate rocks (basalt, monzogranite and shale fines) following ultrasound dissolution and analysis by F AES. Sample preparation method was optimized by using fractional factorial designs. The following optimal conditions were obtained for each silicate rock: 0.1 g of sample mass for any of the three samples, and volumes of HNO3, HCl and HF, respectively, of 2.5, 0.8 and 2.5 mL for basalt; 3.5, 0.8 and 2.5 mL for monzogranite, and 2.5, 1.0 and 2.0 mL for shale fines. Sample dissolution was achieved by using the ultrasound bath at room temperature (25 °C) for 1 hour. The accuracy was evaluated through the analysis of two certified reference materials, for which there was no statistical difference between the certified and the found K concentration values (95% confidence level). The K concentrations determined were: 1.45 ± 0.01 for basalt; 4.19 ± 0.03 for monzogranite and 1.60 ± 0.02 for shale fines. The developed method presented accurate and reliable results for K amounts in silicate rocks and is simple and safe, which are important features for the implementation of a methodology as a routine analysis. |
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