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woelen
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I tried to make the yellow/ochre compound in somewhat larger quantities, but this is very hard. If I use a concentration of thiocyanate and nitric
acid in which this compound is formed quickly, then the reaction becomes very violent when scaled up, and even when I only use 20 ml of liquid in a
500 ml beaker, most of the liquid is lost as fumes, smokes and bubbles. If I use lower concentrations, then the reaction does not give the yellow
compound but a pale yellow and clear liquid is obtained and a lot of colorless gas. The best run I had so far is appr. 100 mg from 5 grams of NH4SCN,
which is really pathetic. I already spent 15 grams of NH4SCN and I still have less than 200 mg of the yellow solid. Given the fairly high price of
NH4SCN (appr. EUR 15 per 250 grams) this is quite disappointing.
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bfesser
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I assume you've tried drop-wise addition of one of the reagents by addition funnel? Does the reaction still proceed if the reagents are chilled?
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Random
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Somewhat offtopic but there is a topic where I posted about thiocyanate synthesis from ferrocyanide you might want to check if it is working method
and since ferrocyanide is maybe cheaper it would be useful.
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Nicodem
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Some articles in regard to (SCN)2, its polymer and the related chemistry thiocyanate oxidation products:
The chemistry of (ECN)2 (E = S, Se) and related compounds
Burchell, Colin J., Aucott, Stephen M., Robertson, Stuart D., Slawin, Alexandra M. Z. and Woollins, J.
Derek
Phosphorus, Sulfur, and Silicon and the Related Elements, 179, 865-868. DOI: 10.1080/10426500490427619
Zur Kenntnis des Rhodans und seiner Verbindungen
Fritz Seel, Erich Müller
Chemische Berichte, 88, 1747–1755. DOI: 10.1002/cber.19550881125
Beiträge zur Chemie des Schwefels, 49. Über die homologe Reihe der Cyansulfane Sn(CN)2
Franz Feher, Helmut Weber
Chemische Berichte, 91, 642–650. DOI: 10.1002/cber.19580910326
Acidic Aqueous Decomposition of Thiocyanogen
Jon J. Barnett, Michael L. McKee, and David M. Stanbury
Inorg. Chem., 43, 5021-5033. DOI: 10.1021/ic049356s
Attachment: 725589262.pdf (89kB)
This file has been downloaded 1233 times
Attachment: Zur Kenntnis des Rhodans und seiner Verbindungen.pdf (632kB)
This file has been downloaded 462 times
Attachment: phpU7JGK8 (549kB)
This file has been downloaded 404 times
Attachment: Acidic Aqueous Decomposition of Thiocyanogen.pdf (287kB)
This file has been downloaded 494 times
…there is a human touch of the cultist “believer” in every theorist that he must struggle against as being
unworthy of the scientist. Some of the greatest men of science have publicly repudiated a theory which earlier they hotly defended. In this lies their
scientific temper, not in the scientific defense of the theory. - Weston La Barre (Ghost Dance, 1972)
Read the The ScienceMadness Guidelines!
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Nicodem
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... and the oxidation of thiocyanates by HNO3:
Oxidation of metal thiocyanates by nitric and nitrous acids. Part I. Products
G. Stedman and P. A. E. Whincup
J. Chem. Soc. A, 1969, 1145-1148. DOI: 10.1039/J19690001145
The second part of the study is DOI: 10.1039/J19690001148 (about reaction kinetics).
Attachment: Oxidation of metal thiocyanates by nitric acid.pdf (542kB)
This file has been downloaded 642 times
…there is a human touch of the cultist “believer” in every theorist that he must struggle against as being
unworthy of the scientist. Some of the greatest men of science have publicly repudiated a theory which earlier they hotly defended. In this lies their
scientific temper, not in the scientific defense of the theory. - Weston La Barre (Ghost Dance, 1972)
Read the The ScienceMadness Guidelines!
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papaya
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I don't really know if this belongs to there, but just found it could be useful.
http://www.oocities.org/capecanaveral/campus/5361/chlorate/r...
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