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A simple and automated sample preparation system for subsequent halogens determination: Combustion followed by pyrohydrolysis.
Pereira, L S F; Pedrotti, M F; Vecchia, P Dalla; Pereira, J S F; Flores, E M M.
Affiliation
  • Pereira LSF; Departamento de Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS, Brazil.
  • Pedrotti MF; Departamento de Engenharia Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS, Brazil.
  • Vecchia PD; Departamento de Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS, Brazil.
  • Pereira JSF; Departamento de Química Inorgânica, Universidade Federal do Rio Grande do Sul, 91501-970, Porto Alegre, RS, Brazil.
  • Flores EMM; Departamento de Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS, Brazil. Electronic address: ericommf@gmail.com.
Anal Chim Acta ; 1010: 29-36, 2018 Jun 20.
Article de En | MEDLINE | ID: mdl-29447668
ABSTRACT
A simple and automated system based on combustion followed by a pyrohydrolysis reaction was proposed for further halogens determination. This system was applied for digestion of soils containing high (90%) and also low (10%) organic matter content for further halogens determination. The following parameters were evaluated sample mass, use of microcrystalline cellulose and heating time. For analytes absorption, a diluted alkaline solution (6 mL of 25 mmol L-1 NH4OH) was used in all experiments. Up to 400 mg of soil with high organic matter content and 100 mg of soil with low organic matter content (mixed with 400 mg of cellulose) could be completely digested using the proposed system. Quantitative results for all halogens were obtained using less than 12 min of sample preparation step (about 1.8 min for sample combustion and 10 min for pyrohydrolysis). The accuracy was evaluated using a certified reference material of coal and spiked samples. No statistical difference was observed between the certified values and results obtained by the proposed method. Additionally, the recoveries obtained using spiked samples were in the range of 98-103% with relative standard deviation values lower than 5%. The limits of quantification obtained for F, Cl, Br and I for soil with high (400 mg of soil) and low (100 mg of soil) organic matter were in the range of 0.01-2 µg g-1 and 0.07-59 µg g-1, respectively. The proposed system was considered as a simple and suitable alternative for soils digestion for further halogens determination by ion chromatography and inductively coupled plasma mass spectrometry techniques.
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Texte intégral: 1 Collection: 01-internacional Base de données: MEDLINE Langue: En Journal: Anal Chim Acta Année: 2018 Type de document: Article Pays d'affiliation: Brésil

Texte intégral: 1 Collection: 01-internacional Base de données: MEDLINE Langue: En Journal: Anal Chim Acta Année: 2018 Type de document: Article Pays d'affiliation: Brésil