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Description of experiment
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experiment.
Needed compounds: ----------------- sodium sulfide : Na2S . 3H2O hydrochloric acid : HCl nitric acid : HNO3 antimony sesquioxide : Sb2O3
Class: ------ elem=S,Cl,Sb precipitation redox
Summary: -------- Antimony trioxide does not dissolve in concentrated nitric acid, not even when the liquid is heated to boiling. When some hydrochloric acid is added as well, then it quickly dissolves, producing a colorless gas as well. It is oxidized to the +5 oxidation state. When this solution is diluted, then a white precipitate is formed. This white precipitate must be hydrous Sb2O5. When a dilute solution of sodium sulfide is added to this still strongly acidic solution, then H2S bubbles out of solution, but also a lot of precipitate is formed, which has a beautiful bright orange/red color.
Description: ------------ Add some concentrated nitric acid (appr. 60% HNO3 by weight) to solid antimony trioxide: No reaction occurs. Even when the liquid is heated, still no reaction occurs. No brown gas is produced, the white solid does not change.
Add an equal volume of concentrated hydrochloric acid (appr. 30% HCl by weight) to the still hot liquid: The white solid quickly dissolves and a colorless gas is produced. The liquid turns orange/yellow and an orange/brown gas mix is produced above the liquid. This orange/yellow and orange/brown color most likely is due to formation of nitrosyl chloride. The colorless gas probably is NO.
Dilute the liquid by adding approximately two times its volume of water: The orange/yellow color of the solution disappears at once. The liquid becomes totally clear and colorless. This quick disapearance of the yellow/orange color confirms that this color is due to nitrosyl chloride. Nitrosyl chlorid very easily hydrolyses in water. However, a few seconds later, it becomes milky white. This change from clear to white/opaque is not an instantaneous reaction, but it takes several seconds.
Add a dilute solution of sodium sulfide to this white and still strongly acidic liquid: Some colorless gas escapes (bad smell, H2S). A lot of yellowish/brown precipitate is formed, which quickly turns bright orange/red and becomes flocculent. The precipitate fairly quickly settles as a bright orange/red layer with a still somewhat turbid yellow liquid above it.
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Antimony trioxide is not easily oxidized by nitric acid, but things change when also hydrochloric acid is present in the mix. The antimony(III) then quickly is oxidized to the +5 oxidation state. Antimony in oxidation state +5 is quickly hydrolysed just like antimony(III). With hydrogen sulfide, this forms the beautifully colored compound antimony pentasulfide. The pentasulfide probably is not a true pentasulfide, but some compound of indeterminate stoichiometry, which contains antimony and sulphur in a 2
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