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Sinteza in karakterizacija hidroksilamonijevega fluoroindata : disertacijaKristl, Matjaž▫$(NH_3OH)_3InF_6$▫ smo sintetizirali v sistemu ▫$In(OH)_3-NH_3OHF-HF$▫. ▫$NH_3OHF$▫ smo pridobili z reakcijo med etanolno raztopino hidroksilamina in 40% HF. ▫$In(OH)_3$▫ smo raztopili v vreli 40% ... HF, ohlajeni raztopini smo nato dodajali trden ▫$NH_3OHF$▫ v različnih množinskih razmerjih. S počasnim odparevanjem topila pri sobni temperaturi smo dobili bele kristale ▫$(NH_3OH)_3InF_6$▫. Kemijska analiza je pokazala naslednje masne deleže: ▫$NH_3OH^+$▫ = 30.5% (teor. 30.8%), ▫$In^3+$▫ = 34.4% (teor. 30.8%). ▫$F^-$▫ =33.7% (teor. 34.5%). Določili smo topnost dobljene spojine v vodi (20.0 g/100g), 40% HF (17.9 g/100g) in absolutnem etanolu (0.03 g/100g). Termični razkroj smo spremljali s termogravimetričnimi (TG) in diferencialno termičnimi (DSC) meritvami. ▫$(NH_3OH)_3InF_6$▫ razpade v treh stopnjah z maksimumi pri 235, 255 in 343 oC. Izgube mase na TG krivulji se dobro ujemajo s piki na DSC krivulji, ki so za vse stopnje endotermni. Produkte termičnega razkroja smo karaketrizirali z rentgenskimi praškovnimi posnetki. Strukturo spojine smo določili z rentgensko difrakcijo na monokristalu. Podatke smo zbirali na štirikrožnem difraktometru z ▫$MoK_\alpha$▫ radiacijo pri temeperaturi 20(1) oC. ▫$NH_3OH)_3InF_6$▫ kristalizira trigonalno, R3c, s parametri osnovne celice a=b=c=7.764(2) Å, ▫$\alpha=\beta=\gamma=97.21(4)^o$▫, ▫$D_x$▫=2.39 ▫$Mg/m^3$▫, ▫$D_m$▫= 2.411 ▫$Mg/m_3$▫, V=455.8(5) ▫$Å^3$▫, Z=2, R=0.025,▫$R_w$▫=0.019, 5346 merjenih uklonov. Strukturo sestavljajo izolirani oktaedri ▫$InF_6^3-$▫, pri čemer eden od oktaedrov leži v središču osnovne celice, drugi pa na ogliščih. Med oktaedri ležijo molekule ▫$NH_3OH^+$▫, ki povezujejo strukturo preko močnih vodikovih vezi N-H ...F in O-H ... F. Struktrne podatke smo primerjali z objavljenimi strukturami hidroksilamonijevega fluorogalata in amonijevih ter hidrazinijevih fluoroaluminatov, -galatov in -indatov. Ugotovili smo, da se vezne razdalje in koti dobro ujemajo z vrednostmi, znanimi iz sorodnih spojin.Type of material - dissertationPublication and manufacture - Maribor : [M. Kristl], 1999Language - slovenianCOBISS.SI-ID - 5172246
Author
Kristl, Matjaž
Other authors
Volavšek, Bogdan |
Golič, Ljubo
Topics
anorganska kemija |
hidroksilamonijev fluoroindat |
sinteza |
karaketrizacija |
struktura |
rentgenska analiza |
inorganic chemistry |
hydroxylammonium fluoroindate |
synthesis |
characterization |
structure |
x-ray analysis
Library/institution |
City | Acronym | For loan | Other holdings |
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Library of Technical Faculties, Maribor | Maribor | KTFMB |
reading room 1 cop.
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Database name | Field | Year |
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Links to authors' personal bibliographies | Links to information on researchers in the SICRIS system |
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Kristl, Matjaž | 14755 |
Volavšek, Bogdan | 00456 |
Golič, Ljubo | 00842 |
Source: Personal bibliographies
and: SICRIS
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