Jaysus
Harmless
Posts: 2
Registered: 28-1-2013
Member Is Offline
Mood: No Mood
|
|
Beginner needs help with nitric acid
I have just started and escrapping side business with my scrap yard for precious metal recovery and am going to need to synthesize nitric and
hydrochloric acids pretty regularly. What distillation setup would be best for someone with minor training in chemistry. ive done some research and
believe that distillation provides what i need for aqua regia in sufficient supply. I have already purchased a fume hood and safety equipment. I also
need advice on storage of these chemicals. Thanks for any help.
|
|
|
kristofvagyok
National Hazard
Posts: 659
Registered: 6-4-2012
Location: Europe
Member Is Offline
Mood: No Mood
|
|
May I ask that if you could buy a fume hood, a lot safety equipment and labware, than how is that you have to make nitric and hydrochloric acid by
yourself? They are the cheapest acids, usually could be bought in HDPE cans for no money.
But if you are willing to make them, the best would be to start from sulfuric acid (could you get that?) and make the acids from the corresponding
salts, e.g.: NaCl and NaNO3 or KNO3. The generated HCl should be adsorbed in distilled water, the HNO3 should be distilled from the mixture of H2SO4
and KNO3. Use a large distilling flask with a large neck, because it is more easy to get out the sodium sulfate what will remain.
But everything have been written down several times, search a bit.
I have a blog where I post my pictures from my work: http://labphoto.tumblr.com/
-Pictures from chemistry, check it out(:
"You can’t become a chemist and expect to live forever." |
|
|
Jaysus
Harmless
Posts: 2
Registered: 28-1-2013
Member Is Offline
Mood: No Mood
|
|
First off thanks for the reply Kristof. I live in the USA where the government will put you in jail for buying nitric acid of any dilution. After 911
it became tightly controlled and you have to have a business to order it online. I've had to make nitric acid before in Iraq, but that was a very
improvised method. The chemicals to make it are easy enough to get. I can buy nitrates at the feed store and sulfuric acid at tye hardware store. I'm
just wondering if a glass on glass distillation kit is required or if one of the cheaper setups could be used
|
|
|
Magpie
lab constructor
Posts: 5939
Registered: 1-11-2003
Location: USA
Member Is Offline
Mood: Chemistry: the subtle science.
|
|
Quote: Originally posted by Jaysus  | | I live in the USA where the government will put you in jail for buying nitric acid of any dilution. After 911 it became tightly controlled and you
have to have a business to order it online. |
Where did you get that idea?
The single most important condition for a successful synthesis is good mixing - Nicodem
|
|
|
Vargouille
Hazard to Others
Posts: 380
Registered: 16-4-2012
Member Is Offline
Mood: No Mood
|
|
Sorry, am I living in a different US? Because I can buy reagent-grade concentrated nitric acid from an online place, though I have to pay for HAZMAT
shipping. Home Depot also sold a concrete etchant composed of nitric acid, phosphoric acid, and water. Myst did a video on getting the nitric acid out
of it.
|
|
|
kadriver
Hazard to Others
Posts: 196
Registered: 7-11-2012
Location: United States
Member Is Offline
Mood: Thankful
|
|
Jaysus - you can buy hydrochloric acid at Lowes in the USA for about $7.50 a gallon. It is sold under the brand name of Crown and it is called
muriatic acid (don't buy the "safer" muriatic - it is diluted).
kadriver
|
|
|
kadriver
Hazard to Others
Posts: 196
Registered: 7-11-2012
Location: United States
Member Is Offline
Mood: Thankful
|
|
| Quote: Originally posted by Vargouille | | Sorry, am I living in a different US? Because I can buy reagent-grade concentrated nitric acid from an online place, though I have to pay for HAZMAT
shipping. Home Depot also sold a concrete etchant composed of nitric acid, phosphoric acid, and water. Myst did a video on getting the nitric acid out
of it. |
I get nitric acid from GFS Chemical, 6 - 2.5 liter bottles for about $220 delivered to my business address.
They will not deliver to a residence.
Vargouille, if you get a better price then would you be willing to share your source?
Thank you,
kadriver
|
|
|
Vargouille
Hazard to Others
Posts: 380
Registered: 16-4-2012
Member Is Offline
Mood: No Mood
|
|
I don't have a place that has a better price than that, but I know places that sell in much lower quantities. Elemental Scientific sells 16 fl. oz. of
ACS grade 70% HNO3 for $9.99, and HAZMAT shipping is about $27.50 added to the standard shipping charge. Duda Diesel is a good source for higher
quantities of 67.2%.
|
|
|
wireshark
Harmless
Posts: 28
Registered: 21-1-2013
Member Is Offline
Mood: No Mood
|
|
You can build a Birkeland-Eyde apparatus. Nitric acid is produced from nothing but air, water, and electricity. The big difficulty is the engineering.
I'm going to try my hand at this soon.
|
|
|
hissingnoise
International Hazard
Posts: 3940
Registered: 26-12-2002
Member Is Offline
Mood: Pulverulescent!
|
|
The production of HNO3 by the travelling arc of a "Jacob's Ladder" is very slow . . .
|
|
|
wireshark
Harmless
Posts: 28
Registered: 21-1-2013
Member Is Offline
Mood: No Mood
|
|
True, but the alternative requires nitrate salts, which I wouldn't be caught dead ordering. The alternative is superior. It'll be time consuming, but
it's possible to design a Birkeland-Eyde reactor that runs continuously and safely, producing maybe 100 mL per day at a great energy cost.
Anyway, as I just realized, aqua regia requires anhydrous nitric acid. Correct me if I'm wrong. So the Birkeland-Eyde technique will not work. You can
only purify dilute nitric to 70% or so due to the azeotrope. I also wanted nitric in order to make aqua regia, so forget trying to build a BE reactor.
|
|
|
wireshark
Harmless
Posts: 28
Registered: 21-1-2013
Member Is Offline
Mood: No Mood
|
|
Okay, after a little bit of searching, I found that nitrates can be found OTC  .
Just read MSDSes.
|
|
|
elementcollector1
International Hazard
Posts: 2684
Registered: 28-12-2011
Location: The Known Universe
Member Is Offline
Mood: Molten
|
|
How pure are they?
Elements Collected:52/87
Latest Acquired: Cl
Next in Line: Nd
|
|
|
MrHomeScientist
International Hazard
Posts: 1806
Registered: 24-10-2010
Location: Flerovium
Member Is Offline
Mood: No Mood
|
|
Ammonium nitrate from instant cold packs has been plenty pure enough for my purposes, just need to dissolve in water and filter off some "gunk"
(probably anti-caking agents). I use that to make potassium nitrate fairly often.
And to answer one of the original questions, yes nitric acid distillation must be done in an all-glass apparatus. The hot acid vapors will corrode
rubber stoppers found in cheaper kits.
|
|
|
binaryclock
Hazard to Others
Posts: 121
Registered: 9-4-2013
Location: Canada
Member Is Offline
Mood: Organic
|
|
| Quote: Originally posted by MrHomeScientist | Ammonium nitrate from instant cold packs has been plenty pure enough for my purposes, just need to dissolve in water and filter off some "gunk"
(probably anti-caking agents). I use that to make potassium nitrate fairly often.
And to answer one of the original questions, yes nitric acid distillation must be done in an all-glass apparatus. The hot acid vapors will corrode
rubber stoppers found in cheaper kits. |
Cold packs in Canada contain either Calcium Ammonium Nitrate or urea. It melts when you try to heat it up :p
[Edited on 10-4-2013 by binaryclock]
|
|
|
Steve_hi
Hazard to Others
Posts: 196
Registered: 4-12-2010
Member Is Offline
Mood: No Mood
|
|
| Quote: |
Cold packs in Canada contain either Calcium Ammonium Nitrate or urea. It melts when you try to heat it up :p
|
I buy in canada. You can buy a green house grade Ammonium nitrate or potasium nitrate very clean stuff for 53$ + taxes.
from agrisyn here in Quebec but it must be available in the rest of canda as easily, you just need to find the right place.
They also have NH4NO3 that has brown gunk all over it and mixed with CaCO3 you have to do a lot of recrystalising to get it clean. This is sold
to the farmers who buy it by the ton.
|
|
|
paw_20
Harmless
Posts: 32
Registered: 14-8-2012
Location: United States
Member Is Offline
Mood: Curious
|
|
| Quote: Originally posted by Jaysus | | I live in the USA where the government will put you in jail for buying nitric acid of any dilution. After 911 it became tightly controlled and you
have to have a business to order it online. |
I'd be a lot more worried about ordering KI or I2 online, which are controlled for reasons totally unrelated to 9/11, and people still seem to do it
all the time on ebay.
Also there's a couple of other businesses besides Duda that sell conc. nitric and other basic chemicals in smaller quantities, most of them list on
ebay as well as having their own site.
|
|
|
Funkerman23
Hazard to Others
Posts: 416
Registered: 4-1-2012
Location: Dixie
Member Is Offline
Mood: No Mood
|
|
To answer some of the OP's questions: Yes , for distilling/ making nitric acid you need a ground glass setup.you can use a little sulfuric acid as
joint grease.If possible , and only if you need it, try to use a ground jointed thermometer in your setup as anything rubber will be attacked. Retorts
have been used but it isn't sealed and the vapors are unpleasant to say the least. For storing them remember that Nitric acids is usually if not
always stored separate from other acids in acid resistant cabinets. As a general rule if you have a lockable acid cabinet you are doing better than
average but I have seen members here with that who put the bottles in plastic bags as an extra measure( keeps smells down too I hear).
[Edited on 10-4-2013 by Funkerman23]
" the Modern Chemist is inundated with literature"-Unknown
|
|
|
zed
International Hazard
Posts: 2277
Registered: 6-9-2008
Location: Great State of Jefferson, City of Portland
Member Is Offline
Mood: Semi-repentant Sith Lord
|
|
If you have a legitimate business enterprise, obtaining common chemicals should pose no real problems. Nitric acid? No big deal.
Scrap yard? Want to scavenge platinum or palladium, from catalytic converters.....AOK.
State or local officials might come around occasionally to talk to you, but if you aren't involved in anything sketchy, there should be no real
problems.
Some of the guys run suspicious looking little experiments that irritate LE.
|
|
|
paw_20
Harmless
Posts: 32
Registered: 14-8-2012
Location: United States
Member Is Offline
Mood: Curious
|
|
| Quote: Originally posted by wireshark |
Anyway, as I just realized, aqua regia requires anhydrous nitric acid. Correct me if I'm wrong. So the Birkeland-Eyde technique will not work. You can
only purify dilute nitric to 70% or so due to the azeotrope. I also wanted nitric in order to make aqua regia, so forget trying to build a BE reactor.
|
http://www.epa.gov/nsr/ghgdocs/nitricacid.pdf
There exist industrial process for producing 98-99% nitric acid, but I'm pretty sure aqua regia does not require such "anhydrous" nitric acid. It does
lose potency over time though, but that just means you mix it up on demand. Conc. nitric is powerful enough, I didn't even know that stronger nitric
existed until I looked it up just now
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
