Abstract
Potassium hexacyanoferrate(II) trihydrate, K4Fe(CN)6·3H2O, was heated under controlled conditions of mass and rate in a derivatograph in the presence of oxygen. The heating was stopped at different temperatures and Mössbauer spectra and X-ray diffractograms were taken on the quenched material at room temperature. The reaction pathway was studied in this way and the advantages and drawbacks of each of the techniques are described. At different stages of the thermal process we were able to show the presence of K4Fe(CN)6,α-Fe2O3, Fe3O4, Fe3C, Fe, FeO, KFeO2,Β-FeOOH, KOCN, K2CO3 and KCN.
Resumé
Le ferrocyanure de potassium trihydraté, K4Fe(CN)6·3H2O, a été chauffé en présence d'oxygÊne dans un Derivatograph, dans des conditions bien déterminées de masse et de vitesse de chauffage. Le chauffage a été interrompu à diverses températures et les spectres Mössbauer ainsi que les diffractogrammes de rayons X ont été enregistrés aprÊs trempe du matériau à la température ambiante. On a étudié de cette faÇon le déroulement de la réaction; on décrit les avantages et les inconvénients de chacune de ces techniques. On a pu déceler la présence de K4Fe(CN)6,α-Fe2O3, Fe3O4 Fe3C, Fe, FeO, KFeO2,Β-FeOOH, KOCN, K2CO3 et KCN aux différentes étapes du traitement thermique.
Zusammenfassung
Kaliumhexacyanoferrat(II)trihydrat, K4[Fe(CN)6.3H2O wurde unter kontrollierten Bedingungen in einem Derivatographen in Gegenwart von Sauerstoff erhitzt. Das Aufheizen wurde bei verschiedenen Temperaturen gestoppt und Mössbauer-Spektren, sowie Röntgendiffraktogramme aufgenommen. Der Reaktionsweg wurde auf diese Weise untersucht und die Vor- und Nachteile jeder der Techniken beschrieben. Bei den verschiedenen Stufen des thermischen Vorganges konnten K4[Fe(CN)6],α-Fe2O3, Fe3O4, Fe3C, Fe, FeO, KFeO2,Β-FeOOH, KOCN, K2CO3 und KCN nachgewiesen werden.
РЕжУМЕ
тРИгИДРАт гЕксАцИАН О-жЕлЕжО (II)-кИслыИ кАлИИ-к4FЕ/сИ)6. 3Н3О-Был Н АгРЕт В ДЕРИВАтОгРАФЕ В пРИ сУтстВИИ кИслОРОДА п РИ кОНтРОлИРУЕМОИ МАсс Е И скОРОстИ. НАгРЕВАН ИЕ пРЕкРАЩАлОсь пРИ РАж лИЧНых тЕМпЕРАтУРАх И ИжМЕРьлИсь МЕссБАУЁРОВскИЕ спЕ ктРы И РЕНтгЕНОВскИЕ ДИФФ РАктОгРАММы ОхлАжДЕ ННОгО ДО кОМНАтНОИ тЕМпЕРАтУ Ры МАтЕРИАлА. тАкИМ ОБРАжОМ БылО Иж УЧЕНО пРОтЕкАНИЕ РЕА кцИИ И ОпИсАНы пРЕИМУЩЕстВ А И НЕДОстАткИ кАжДОгО Иж ЁтИх МЕтОД ОВ. БылО ВОжМОжНыМ пОк АжАть НА РАжлИЧНых стАДИьх тЕ РМИЧЕскОгО пРОцЕссА пРИсУтстВИ Е K4Fe(CN)6, α-Fe2O3, Fe3O4, Fe3C, Fe, FeO, KFeO2,Β-FeOOH, KOCN, K2CO3 И KCN.
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This research was performed with financial support from the Conselho Nacional de Desenvolvimento Científico e TecnolÔgico (CNPq) and Financiadora de Estudos e Projetos (FINEP). We are grateful to Profs. A. Bristoti, J. Danon, P. J. Aymonino, E. Baran and M. A. Blessa for valuable suggestions and criticisms, and Miss E. A. Veit for performing the thermal measurements at the Pontificia Universidade Católica, Porto Alegre. This work was submitted in partial fulfilment of the conditions for the degree of “Livre Docente“ by one of us (J. I. K.).
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Kunrath, J.I., Müller, C.S. & Frank, E. Thermal decomposition of potassium hexacyanoferrate(II) trihydrate. Journal of Thermal Analysis 14, 253–264 (1978). https://doi.org/10.1007/BF01915163
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DOI: https://doi.org/10.1007/BF01915163