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roXefeller
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I just vented my HNO3 again today, and I get that same feeling. Not so much crippled by fear, but the necessary thought of precautions, taking a
moment to think and then proceeding with respect.
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hissingnoise
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You can be a bit over-cautious!
I have fuming NA in bottles for years without ever venting . . .
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roXefeller
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Thanks for tangenting my original warning of sodium azide toxicity into the mockery of a (overly) cautious man. Hopefully you won't downplay the
warning into nothing more than voices in my head. 
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Hawkguy
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Has anyone heard of the NaN3 prep through Sodium Amide and Hydrazine Sulfate? I was checking out some old book on chemistry preparations and found a
condensed procedure...
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Metacelsus
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Huh? I thought that sodium amide was reacted with nitrous oxide, not hydrazine.
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Shivachemist
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Yeah, Cheddite is right, it is the easiest route to obtain Sodium azide.
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Hawkguy
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Whoops sorry my bad. They were both preps for NaN3, and I thought they were one. The Hydrazine one was different, a reaction with Nitrous Acid or
whateva
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Rhodanide
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Quote: Originally posted by Polverone  | | Quote: | | Obviously the ammonium chloride is going to react with sodium hypochlorite to liberate chlorine gas. |
In that case, I'd be a bit wary; ammonium salts plus Cl2 will produce nitrogen trichloride. I've experienced a hideous scent and some
violent popping before when mixing ammonium salts and calcium hypochlorite. |
Sounds like fun.
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chloric1
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| Quote: Originally posted by Tetra | | Quote: Originally posted by Polverone | | Quote: | | Obviously the ammonium chloride is going to react with sodium hypochlorite to liberate chlorine gas. |
In that case, I'd be a bit wary; ammonium salts plus Cl2 will produce nitrogen trichloride. I've experienced a hideous scent and some
violent popping before when mixing ammonium salts and calcium hypochlorite. |
Sounds like fun. |
I concur. A wonderful way to pass a late summer afternoon. Be sure to do micro amounts and stay upwind!
Fellow molecular manipulator
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Rhodanide
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| Quote: Originally posted by uchiacon | Hey guys,
I was just thinking about whether or not I should make the hydrazine hydrate or purchase it, which is an option to me. For 250g of hydrazine hydrate,
it'd be $50 or about $40USD. I don't have copper/silver/teflon coated labware, and I know the HS and NaOH reaction will eat away at glass due to the
amount of hydrazine hydrate formed.
Presuming that this hydrazine hydrate is of a relatively high concentration, do you think that it's just better for me to purchase the material?
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Depends. Where do you plan to purchase yours?
I have seen some on EBay at 64% in water. Is this what you are talking about?
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Rhodanide
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| Quote: Originally posted by grndpndr | Ah yes,my mistake! China is the very humanitarian state that censors all aspects of life and responsible for tienamen Square ANd roving execution vans
that harvests innmates organs upon execution according to need for foriegn transplants.Yes that paragon of human rights state known as China ,Those
brave souls. Unles your a resident of NK I would cease and desist Sonongashira..
Hmm sonagashira,sounds japanese, the superior race of the asian east if not the world.I wondered where the superior attitude came from.
[Edited on 16-1-2010 by grndpndr] |
From Sodium Azide to Chinese internet censorship.
Only on ScienceMadness. 
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James Ikanov
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I hate to practice the dark art of necromancy, but while it's here, how would such a procedure be complete? Bubbling through a solution, or simple
exposure?
“To do good work one must eat well, be well housed, have one's fling from time to time, smoke one's pipe, and drink one's coffee in peace” -
Vincent Van Gogh
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Thraxx
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In the year 2004 there was in an discussion told ,that the sodium azide could be manufactured through easy reaction between Hydrazin sulfate,Sodium
nitrite and Barium hydroxid.
Reaction:
N2H6SO4(aq) + NaNO2(aq) + BaO2H2(s) -----> NaN3(aq) + BaSO4(s) + 4H2O(l)
130(2,86/100/OC) + 69(71,4/100/0C)+171,34(1,67/100ml/0C)------5gNaN3 …..etc.
10gHS in 400ml watter+ 5,3g NaNO2 in 10mlwatter + 13,2g Ba(OH)2
Making Barium hydroxide:
Ba(OH)2:
30 g of Ba(NO3)2 with solubility 10,5/100/25C or 34/100/100C + 9g of NaOH in 150ml watter boiled and after cooled to 0C and filtrate it.The Ba (OH)2
is watter solubile 1,67g/100ml/0C.
Making the reaction
Filtrate with Ba(OH)2 add to 10 g of HydrazineSulfate in 400ml watter and add there 5,5g-7g NaNO2 in10ml watter.Because is not known under such
condition should this reaction go,I put it 12 h in freezer and after I boiled it for to evaporace its volume on to 100 ml .After was this volume
reached,I cooled it and filtered.Liquid was there 50 ml .I precipitate it with ethanol and filtered.
There was 3 g of white something and reaction with AgNO3 gave something black.
-------------------------------------------------------------------------------- About used chemicals :
Ba(OH)2 :: mol=171,34anh. Or 315,46 octahydrate
Solubility watter -1,67g/100ml/0C
3,89g/100ml/20C
20,94g/100ml/60C
101,4g/100ml/100C
Other solvents low
--------------------------------------------------------------------------------
NaNO2:: mol=68,995,m.p.271C
Solubility watter-71,4g/100ml/0C
84,8g/100ml/25C
160g/100ml/100C
Methanol-4,4g/100ml,ethanol=solubile,ether=0,3g/100ml
--------------------------------------------------------------------------------
NaOH :: mol= 39,99 m.p. =318 C,density=2,13g/cm3
solubility – watter 485,7g/100ml/0C
-glycerol ?,
-alcohol:
Ethanol= 13,9g/100ml/0C,methanol= 23,8g/100ml/0C
--------------------------------------------------------------------------------
BaSO4:: mol=233,38 -solubility in watter =insolubile,in alkohol= insolubile
-------------------------------------------------------------------------------
Hydrazine sulphate:: solid,mol= 130,13, m.p. 254 C
solubility in watter at 20 C =30g/l or 2,86 /100 ml,
at 80 C= 14,39g/100ml
Insoluble in alkohol
Ethanol = 0,04g/l00ml/28C
H2N-NH3xHSO4
[Edited on 15-10-2016 by Thraxx]
[Edited on 15-10-2016 by Thraxx]
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PHILOU Zrealone
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| Quote: Originally posted by Thraxx | In the year 2004 there was in an discussion told ,that the sodium azide could be manufactured through easy reaction between Hydrazin sulfate,Sodium
nitrite and Barium hydroxid.
Reaction:
N2H6SO4(aq) + NaNO2(aq) + BaO2H2(s) -----> NaN3(aq) + BaSO4(s) + 4H2O(l)
130(2,86/100/OC) + 69(71,4/100/0C)+171,34(1,67/100ml/0C)------5gNaN3 …..etc.
10gHS in 400ml watter+ 5,3g NaNO2 in 10mlwatter + 13,2g Ba(OH)2
Making Barium hydroxide:
Ba(OH)2:
30 g of Ba(NO3)2 with solubility 10,5/100/25C or 34/100/100C + 9g of NaOH in 150ml watter boiled and after cooled to 0C and filtrate it.The Ba (OH)2
is watter solubile 1,67g/100ml/0C.
Making the reaction
Filtrate with Ba(OH)2 add to 10 g of HydrazineSulfate in 400ml watter and add there 5,5g-7g NaNO2 in10ml watter.Because is not known under such
condition should this reaction go,I put it 12 h in freezer and after I boiled it for to evaporace its volume on to 100 ml .After was this volume
reached,I cooled it and filtered.Liquid was there 50 ml .I precipitate it with ethanol and filtered.
There was 3 g of white something and reaction with AgNO3 gave something black.
-------------------------------------------------------------------------------- About used chemicals :
Ba(OH)2 :: mol=171,34anh. Or 315,46 octahydrate
Solubility watter -1,67g/100ml/0C
3,89g/100ml/20C
20,94g/100ml/60C
101,4g/100ml/100C
Other solvents low
--------------------------------------------------------------------------------
NaNO2:: mol=68,995,m.p.271C
Solubility watter-71,4g/100ml/0C
84,8g/100ml/25C
160g/100ml/100C
Methanol-4,4g/100ml,ethanol=solubile,ether=0,3g/100ml
--------------------------------------------------------------------------------
NaOH :: mol= 39,99 m.p. =318 C,density=2,13g/cm3
solubility – watter 485,7g/100ml/0C
-glycerol ?,
-alcohol:
Ethanol= 13,9g/100ml/0C,methanol= 23,8g/100ml/0C
--------------------------------------------------------------------------------
BaSO4:: mol=233,38 -solubility in watter =insolubile,in alkohol= insolubile
-------------------------------------------------------------------------------
Hydrazine sulphate:: solid,mol= 130,13, m.p. 254 C
solubility in watter at 20 C =30g/l or 2,86 /100 ml,
at 80 C= 14,39g/100ml
Insoluble in alkohol
Ethanol = 0,04g/l00ml/28C
H2N-NH3xHSO4
[Edited on 15-10-2016 by Thraxx]
[Edited on 15-10-2016 by Thraxx] |
May I ask what is your age and education level in chemistry?
You provide really a lot of informations into this post, but most of the information is not so important for the purpose of the making of NaN3...so
you end up by leading us onto side ways instead of keeping us on track (Thraxx  ).
If I read your procedure, I may conclude that mixing NaNO2 with N2H5OH will result into the making of NaN3...
This is something possible because I have experienced that mixing N2H5OH with phenol-phtalein (PP) makes a fushia solution...when PP is put into NaNO2
solution nothing happens (what is normal because NaNO2 is nor basic nor acidic so solution remains neutral).
When mixing fushia N2H5OH/PP solution with NaNO2 solution...discoloration occurs...not a single bubble of N2
This proves something happens to the basic stuff into the solution and that is hydrazine; the only possibility is via formation of NaN3 (via
hydrazine nitrite? and immediate recombination into hydrazoic acid + water....?)
H2N-NH2 + H2O <-aq-> H2N-NH3(+) + OH(-)
NaNO2 -aq-> Na(+) + NO2(-)
H2N-NH3(+) + NO2(-) --?--> H2N-NH-N=O + H2O
H2N-NH-N=O <--> H2N-N=N-OH --> HN3 + H2O
HN3 <-aq-> H(+) + N3(-)
OH(-) + H(+) --> H2O
After simplification
H2N-NH2 + H2O + NaNO2--> NaN3 + H2O
Sadly at that time I didn't test for azide precipitation.
Into your procedure the Ba(OH)2 is only present because soluble base and source of Ba(2+) as precipitant for the SO4(2-) by forming white unsoluble
BaSO4(s) (the s means solid into the aqueous phase; thus a precipitate).
I write this because you seems surprised that there is a white precipitate.
Your all procedure don't need the first step of filtration to isolate Ba(OH)2 and separate it from NaNO3, since
Ba(NO3)2(aq) + 2 NaOH(aq) <--> Ba(OH)2(aq) + 2 NaNO3(aq)
Nothing to filtrate, no unsoluble.
Thus Ba(NO3)2 and NaOH can immediatelly be reacted with N2H4.H2SO4 and the resulting BaSO4 filtrated.
Ba(NO3)2 + 2 NaOH + N2H4.H2SO4 ---> BaSO4(s) + 2 NaNO3(aq) + N2H4(aq) + 2 H2O
After filtration you are left with N2H4(aq) and NaNO3(aq).
Those can be reacted with NaNO2 because Na(+) and NO3(-) are spectator (=not entering the equation) ions.
So you come to a simple addition of N2H4(aq) to NaNO2(aq)...exactly what I simply did.
Final remark, you do a lot of experiments but you never write the final testing of your azide...the only proof azide is present, is precipitation of
unsoluble azide (heavy metal), filtration recollection, drying and submitting to fire --> BOOM.
This last step is important, because many things may form a precipitate into your complex reaction scheme (too much reactants)...remember KISS KISS
KISS (not only your wife or girlfriend --> Keep It Short & Simple.
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Thraxx
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The iformation about properties of used chemicals is important for purifiing of NaN3(if there some is).Because if the sodium azide will not be
pure,then I cannot do its silver or lead salt.
This was the case of the filtration Ba(OH)2/NaNO3(+NaOH).
This reaction need to be purified with CO2 bubbling and now in this moment I am not able to do it.
End of reaction I would like to do with FeCl3,it should be red with azide.Unfortunatelly now I havent it.
For me is important to do reactions and to know properties of chemicals.To have or own some explosives is for me not important,I dont need it.I have
no education in chemistry,I only love it.
This reaction gave a very poor yield and its product is not able to do silver azide.I hesitate if it is really azide .May be that it is hydrazin
sulfate,which can be precipitate similar like azide.
----------------
((the Thiele/Stolle reaction I did yeasterday with good yield after I change the alcohol and added the IPN gradually))
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PHILOU Zrealone
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The purity is not important if you play it safe about cations and anions to take care that all ions except the azide won't make a precipitate. -->
Only N3(-) and Ag(+) will precipitate, nothing else --> purity is no concern because 100%.
But to be able to do this, you need more chemical experience or a better understanding of it (amongst other precipitation rules, acid-base, reaction
equilibriums (Lechatelier's rules, Henry rules, ...).
I'm not sure that azide chemistry is the best to start and aquire knowledge, because its is using and forming dangerous compounds (toxic, gaseous,
explosive, flamable).
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Thraxx
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| Quote: Originally posted by PHILOU Zrealone | | The purity is not important if you play it safe about cations and anions to take care that all ions except the azide won't make a precipitate. -->
Only N3(-) and Ag(+) will precipitate, nothing else --> purity is no concern because 100%. |
If only it were that simple,but I am sorry, I have here white powder,which give me with AgNO3 the black powder.At least two of used chemicals are able
do it...and then absent evidence,that there is some azide present.
[Edited on 15-10-2016 by Thraxx]
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PHILOU Zrealone
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Exactly what I wrote...you need more chemical basic knowledge.
It is sad that you waste so much valuable reactants into much experiments without succes because of this.
I hope you work on recovery too.
You probably stil have OH(-) (as Ba(OH)2 or as NaOH) and some N2H4 into solution...not easy if you add too much N2H6SO4, then the SO4(2-) will
precipitate with Ag(+) as Ag2SO4; if stil some Ba(OH)2 or exces NaOH then AgOH precipitation...so proces must be fine-tuned to avoid those anoying
anions.
Hydroxyde or hydrazine react with AgNO3 and do form black precipitate (Ag2O (2 AgOH --> Ag2O + H2O), and Ag silver foam (by reduction via
hydrazine)...
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Thraxx
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| Quote: Originally posted by PHILOU Zrealone | Exactly what I wrote...you need more chemical basic knowledge.
It is sad that you waste so much valuable reactants into much experiments without succes because of this.
I hope you work on recovery too. |
And what you would like Philou?Should I tell you,that I will waite untill I will have "more chemical basic knowlidges"?No,I did many wrong experiments
for to know,that the publicated way is wrong and now I am seeking such way,which does work.After I will sure,that it does really work,then I will
publicate it here.But because I see,that my experiments bother you,I will publicate only this one message and nothing more.
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PHILOU Zrealone
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You missed my point.
Sorry if you are offended.
This is not what I want...experimenting is good...but when working with dangerous stuffs, or expensive/valuable chemicals, it need a little
preparation.
Maybe before acting, ask here to someone that may read between the lines and put into evidence the important points of the process...it will spare you
time, bad results and loss of reactants.
N2H4.H2O + Butyl nitrite + KOH/NaOH works very well.
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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