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Silicon determination in Portland cement by fluoride generation,using flame atomic absorption spectrometry
Institution:1. Department of Chemical Engineering and Energy Sustainability, Faculty of Engineering, Universiti Malaysia Sarawak, 94300 Kota Samarahan, Sarawak, Malaysia;2. Nigerian National Petroleum Corporation, NNPC Corporate Headquarters, Abuja, Nigeria;3. Department of Mechanical and Manufacturing Engineering, Faculty of Engineering, Universiti Malaysia Sarawak, 94300 Kota Samarahan, Sarawak, Malaysia;4. Polymer Technology Section, Universiti Kuala Lumpur Malaysia – Institute of Chemical Bioengineering Technology, 78000 Alor Gajah, Malaysia;1. “Scienze del Farmaco e Prodotti per la Salute” Department, University of Messina, viale Annunziata, 98168 Messina, Italy;2. Department of Food Science, University of Udine, Via Sondrio 2A, 33100 Udine, Italy;3. University Campus Bio-Medico of Rome, Via Álvaro del Portillo, 21, 00128 Roma, Italy;4. Chromaleont s.r.l., c/o “Scienze del Farmaco e Prodotti per la Salute” Department, University of Messina, viale Annunziata, 98168 Messina, Italy
Abstract:A new method for the determination of silicon in Portland cement, based on the generation of volatile species without sample pre-treatment, is proposed. The method reduces operational complexity and time without loss of precision and with similar accuracy as the current methods. It employs microwave-assisted (domestic microwave oven) digestion to produce volatile silicon fluorides by reaction of the sample with a fluorinated salt (CaF2) in the presence of H2SO4 (98% w/w), using a Teflon® (PFA) reactor. The volatile fluorides are flushed out by a dry nitrogen stream and collected in 0.3 mol l−1 NaOH solution where they dissolve. Silicon is determined in this solution by flame atomic absorption spectrometry (FAAS). The recoveries are between 98 and 102%, and the precision is better than 2.5% relative standard deviation (R.S.D).
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