Nidias91
Harmless
Posts: 4
Registered: 18-1-2006
Member Is Offline
Mood: No Mood
|
|
[Alkali Earth Metal] Nitrite
I have found many syntheses for various alcoholic nitrites, and they all have the basic formula of:
Nitrous Acid + Alcohol
Well, I know that Nitrous Acid is made with H2SO4 and a nitrite salt. The one that all of the syntheses I have read is NaNO2. I was just wondering,
how would I produce NaNO2 or KNO2 from their respective nitrates?
By the way, this is my first post at ScienceMadness. Make suggestions if you want I guess. All help is appreciated.
|
|
|
The_Davster
A pnictogen
Posts: 2861
Registered: 18-11-2003
Member Is Offline
Mood: .
|
|
The procedure is the exact same, just do some calculations to ensure the mass of KNO2 used contains the same number of moles of NO2- ions as the mass
of NaNO2 called for in the procedure.
EDIT: OOps...I misread what you were asking, but we have a thread dedicated to making nitrites from nitrates and Pb, Magpie has semi-recently posted
a very nice description of it with pictures.
[Edited on 19-1-2006 by rogue chemist]
|
|
|
Nidias91
Harmless
Posts: 4
Registered: 18-1-2006
Member Is Offline
Mood: No Mood
|
|
Sorry if I was vague before, I figured that I would be. I was asking how I would produce NaNO2 or KNO2 from NaNO3 and KNO3 respectively.
I remember something about producing KNO2 from KNO3 by heating KNO3 at several hundred degrees for a few hours.. I'm not really sure though.
|
|
|
Lambda
National Hazard
Posts: 566
Registered: 15-4-2005
Location: Netherlands
Member Is Offline
Mood: Euforic Online
|
|
Heating KNO3 to several hundred Degrees Celcius (?)
Dear Nidias91, heating KNO3 to a melt of several hundred Degrees Celcius is a big NO !! NO !!. The melt is known to even Detonate !! (Bretherick ???).
In the laboratory, Lead (Pb) is used to reduce the KNO3 or NaNO3 to the corresponding Nitrites. I have the procedure in Dutch, and I wil have to
translate it for you from "Chemische Preparaten" by Drs. L. P. Edel (Kluwer).
Please have patients, and give me two days to find the book and do the translation.
|
|
|
chemoleo
Biochemicus Energeticus
Posts: 3005
Registered: 23-7-2003
Location: England Germany
Member Is Offline
Mood: crystalline
|
|
Please consult the following thread for more details, and continue the discussion there.
https://sciencemadness.org/talk/viewthread.php?tid=52
Please search in the future to avoid double posts.
[Edited on 19-1-2006 by chemoleo]
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
|
|
|
Nidias91
Harmless
Posts: 4
Registered: 18-1-2006
Member Is Offline
Mood: No Mood
|
|
Lambda thank you VERY much. I'm not sure if my email is in my profile so : nidias91 at gmail.com
and chemoleo, i will gladly do that, thank you
|
|
|
Polverone
Now celebrating 21 years of madness
Posts: 3186
Registered: 19-5-2002
Location: The Sunny Pacific Northwest
Member Is Offline
Mood: Waiting for spring
|
|
There is little danger in heating KNO3 as hot as you please, so long as it is pure. However, it is not a very good method for nitrite production: the
equilibrium does not tend very far toward nitrite with simple heating in air.
PGP Key and corresponding e-mail address
|
|
|
Lambda
National Hazard
Posts: 566
Registered: 15-4-2005
Location: Netherlands
Member Is Offline
Mood: Euforic Online
|
|
IIRC "Bretherick" makes mention of KNO3 detonating at ~1100 Degrees Celsius.
Melting KNO3 should not present any kind of problem, just like Polverone has mentioned. But want's the melt has cooled down, only to find out that
hardly, if any KNO2 has been formed. Trying to then superheat the melt inorder to push the equation in favor of KNO2, may lead to an explosion, as
mentioned in the above hazardous situation.
KNO3, is used in some old "Gun Blueing" recipes in it's melted form, at controlled temperatures.
Reducing KNO3 to KNO2 via a procedure with molten Lead, not only can take place at a much lower heating temperature, but has the advantage of an
easily controlled, high yield manner of cheap OTC chemicals synthesis.
KNO2 is relatively expensive to buy, and can be made so cheap !
|
|
|
S.C. Wack
bibliomaster
Posts: 2419
Registered: 7-5-2004
Location: Cornworld, Central USA
Member Is Offline
Mood: Enhanced
|
|
That is much much too hot. I have mentioned temperature ranges before, and the reason why some have had no success. Even at that temperature range, O2
evolution continues for quite some time, though you need to look very carefully to see it at the surface. Loss of nitrogen is very small at these
temps, and I doubt that there is any danger from explosions or NO2.
[Edited on 19-1-2006 by S.C. Wack]
|
|
|
Lambda
National Hazard
Posts: 566
Registered: 15-4-2005
Location: Netherlands
Member Is Offline
Mood: Euforic Online
|
|
Potassium Nitrite - KNO2
Here you are Nidias91, the synthesis of Potassium Nitrite.
Kaliumnitriet - KNO2 (Nederlands = Dutch)
In een ijzeren kroes smelt men 100 gram kaliumnitraat (KNO3) en voegt dan onder roeren met een ijzeren spatel in kleine porties 204 gram lood (Pb) bij
de smelt. De oxydatie van het lood verloopt zeer levendig en in een half uur (30 minuten) kan de reactie ten einde zijn. Men giet de nu dikvloeibare
massa op een groot blik uit om de massa gemakkelijker klein te kunnen maken. Het reactieprodukt wordt in een mortier zo fijn mogelijk gestoten en
enige keren met weinig kokend water uitgetrokken. De verkregen oplossingen worden onmiddellijk heet door een vouwfilter gefiltreerd. In het nog hete
filtraat leidt men gedurende korte tijd koolzuur (CO2) om het lood dat in oplossing gegaan is als carbonaat neer te slaan. De oplossing wordt weer
gefiltreerd en op een waterbad ingedampt. De oplossing wordt eerst met iets salpeterzuur (HNO3) geneutraliseerd en men laat afkoelen. Het
uitgekristalliseerde kaliumnitraat (KNO3) wordt afgezogen, de vrij zuivere oplossing van kaliumnitriet (KNO2) wordt tot droog ingedampt en het
verkregen zout wordt op de vrije vlam to smelten gebracht. Het nu watervrije zout wordt weer op een blik uitgegoten, klein gemaakt en nog warm in een
goed sluitbare fles gedaan.
Bron:
Chemische Preparaten
Derde Druk
Drs. L. P. Edel
Kluwer - 1965
Deventer - Antwerpen
Bladzijde: 64
Potassium Nitrite - KNO2 (Translated text from Dutch to English)
In an Iron crucible, melt 100 grams of Potassium Nitrate (KNO3), and add wile stirring with an Iron spoon, in small portions 204 grams of Lead (Pb)
into the smelt. The oxidation of the Lead goes very lively, and in about a half an hour (30 minutes) the reaction may have finished. Pour the now
pasty mass, onto a large Iron sheet metal plate, in order to be able to easily crush it up into small pieces. In a mortar, these small pieces are
ground down as fine as possible, and extracted a few times by means of a small amount of boiling Water (H2O). The resulting extract, is immediately
filtered through a folded filter while it is still hot. Through the still hot filtrate, and during a short period of time, Carbon Dioxide gas (CO2) is
bubbled so that the Lead that was still present in solution may now precipitate as the Carbonate. The solution is again filtered and evaporated by
means of a hot Water bath (100 Degrees Celsius). The now resulting solution is neutralized by means of a small amount of Nitric Acid (HNO3) and left
to cool down. Crystallized Potassium Nitrate (KNO3) is removed from the solution by means of suction filtration, and the now rather pure solution of
Potassium Nitrite (KNO2) is evaporated to dryness, and melted by means of the open flame. The now Water-Free salt is again poured onto an Iron sheet
metal plate, crushed up into small pieces, and while it is still warm, put into a well sealed bottle.
Source:
Chemische Preparaten
Third Edition
Drs. L. P. Edel
Kluwer - 1965
Deventer - Antwerp
Page: 64
|
|
|
woelen
Super Administrator
Posts: 8030
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
|
|
You use iron tools for mixing and also as surface, where the melt is allowed to cool down. Don't you expect contamination with the iron? I can imagine
that the molten nitrate also reacts with iron and that you get iron (III) contamination in the melt, which may be hard to remove.
|
|
|
neutrino
International Hazard
Posts: 1583
Registered: 20-8-2004
Location: USA
Member Is Offline
Mood: oscillating
|
|
Assuming the iron surface is clean of oxide and the melt from the reaction solidifies as soon as it touches the cold metal, there shouldn't be any
significant contamination. The Fe contamination from the iron tools used in the reaction should precipitate with the lead as the carbonate.
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
