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Master's Dissertation
DOI
https://doi.org/10.11606/D.75.2007.tde-14052007-103912
Document
Author
Full name
Milena Pinotti Segato
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
São Carlos, 2007
Supervisor
Committee
Cavalheiro, Eder Tadeu Gomes (President)
Chierice, Gilberto Orivaldo
Crespi, Marisa Spirandelli
Title in Portuguese
"Estudos termoanalíticos do ácido algínico e dos alginatos de metais alcalinos, alcalino-terrosos, amônio, mono-, di- e trietanolamônio"
Keywords in Portuguese
ácido algínico
alginato
análise térmica
Abstract in Portuguese
Os alginatos de metais alcalinos (Li+, Na+ e K+), alcalino-terrosos (Mg2+, Ca2+, Sr2+ e Ba2+), de amônio, mono-, di- e trietanolamônio foram sintetizados por neutralização do ácido algínico com os respectivos hidróxidos, ou carbonatos, e com as aminas. Os sais foram caracterizados por análise elementar e espectroscopia na região do infravermelho, confirmando as sínteses. Após caracterização, os compostos foram submetidos à análise térmica (TG/DTG, DTA e DSC) para avaliar seu comportamento térmico e seus resíduos de decomposição, que foram caracterizados por IR e XRD. Os alginatos de amônio e etanolamônio se decompuseram com liberação de amônia ao final do experimento. Os alginatos de metais alcalinos foram convertidos nos seus respectivos carbonatos, enquanto os alginatos de metais alcalino-terrosos se decompuseram formando carbonatos, em seguida óxidos. Foi feita uma avaliação de procedimentos de secagem por estufa a vácuo a 40 ºC e liofilização; e o último método mostrou-se mais eficaz. A água residual, não-congelável, sai associada à decomposição do material e não foi possível definir exatamente seu teor. Um método de medir o grau de substituição nos sais das aminas foi desenvolvido com base em 13C ? NMR em fase sólida.
Title in English
Thermal analytical studies of alginic acid and its alkaline, earth-alkaline, ammonium, mono-, di- and triethanolammonium alginates
Keywords in English
alginate
alginic acid
thermal analysis
Abstract in English
The alkaline (Li+, Na+ and K+), earth-alkaline (Mg2+, Ca2+, Sr2+ and Ba2+), ammonium, mono-, di- and triethanolammonium alginic acid salts were obtained from the neutralization reaction between alginic acid and the respective hydroxides or carbonates, and the amines, The salts were characterized by elemental analysis and infrared spectroscopy, confirming the synthesis. After the characterization, the compounds were submitted to thermal analysis (TG/DTG, DTA and DSC), in order to evaluate their thermal behavior. The thermal decomposition residues were characterized by IR and/or XRD. The NH4+ and ethanolammonium alginates decomposed via NH3 release without residue in the crucible at the end of the experiment. The alkaline alginates were converted to the respective carbonates, and the earth-alkaline decomposed with production of the carbonates followed by convertion to the oxides. An evaluation of drying procedures involving heating under vaccum up to 40°C and lyophilization were performed, pointing better results in the last case. The residual water, of the non-freezing type, was completely released only during the decomposition of the biopolymer, and it was not possible to define its exact content in the samples. An attempt to estimate the substitution degree in the ethanolammonium salts using 13C ? NMR data, in solid state, was also described.
 
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Publishing Date
2007-05-17
 
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