# Questions About My First Batch Of Nitric Acid



## viacin (Oct 25, 2008)

I'm making my first batch of nitric acid as I type this (it's cooling to room temp), and I believe I have a problem. My sodium nitrate did not disolve completely. Heres what I did:

1. I added 200ml of distilled water to a beaker, and brought it to a semi-boil. 
2. while boiling, I added 170g of sodium nitrate, and stirred untill the solution was clear.
3. I then added another 164g (was aiming for 170, technical dificulties forced me to move on) of sodium nitrate (by now my solution was not boiling), and stired for about 20 minutes. 3/4's of the total 334g of sodium nitrate disolved, the other 1/4 refuses. I got a odd film on the top of the solution, and the undisolved sudium nitrate settled to the bottom as powder.
4. I decided to continue, and added 112ml of "amazing liquid fire" drain cleaner straight from the bottle. sulfuric content is unknown to me, but I was told it was 98% or so by members of the forum. (could anyone confirm?)
5. I stirred as I added. The solution turned a nice yellow, with the sodium nitrate still sitting at the bottom. I stirred for about two minutes.
6. I decided to let it sit to room temperature at this point, so I came in and checked the forum for possible answers. Someone mentioned that they stirred the solution after adding the sulfuric for about ten minutes, so I went back outside to stir. My solution at this point was clear, with the powder settled to the bottom.
7. I stirred for about ten minutes. The solution was still producing steam as I stirred. I washed down the sides of the beaker with a spray bottle, stirred a bit more, and came in. It is clear, no color at all. (I thought it would be yellow?)

Could my problem be that I did not allow the water to come to a complete boil before adding the sodium nitrate? Should I have brought it back to a boil before adding the second 164g? I was beginning to lose water (about a line thickness on my beakers 100ml graduated scale), so I decided to move on. Or am I even expierencing anything abnormal here?


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## viacin (Oct 25, 2008)

An update: I let it sit for about a hour now in a salt/ice/water bath. It's so cold the condensation on my bowl is turning to frost 

My solution is clear, and completely colorless. I have a large amount of white power in the bottom in a solid mass. I hope it is the salt, but I suspect it is mainly the undisolved sodium nitrate. Surely I did something wrong here, isn't nitric acid at these concentrations a yellow color?

When I first poured in my sulfuric acid, it turned yellow immediately, but after stirring it turned clear. I'm lost, any answers?

I think I will pour it off and give it a test with some base metal, see if I get a reaction.

EDIT! A Sudden Change: I went outside, and checked on it again. I now have three little solid mounds of a yellowish looking salt on the bottom. I poked at them a bit with a stir rod, they are pretty solid. And minutes later little particles began forming throughout the solution. Perhaps it is just now reaching -5c? It's been almost 2 hours in the bath.


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## Redders (Oct 25, 2008)

I wish I could help. Please continue recounting this experiment.... I will have a go at this soon, myself. 

What kind of product was the sodium nitrate that you procured.. (fertiliser? cake mix?)

good luck to you....

I hope that the 'gun players' pitch in on your thread.


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## lazersteve (Oct 25, 2008)

Everything sounds fairly normal.

Relying on a normal beakers graduation marks is not the most accurate way to go. I use a graduated cylinder to measure my liquids. Perhaps you had too little water until you sprayed the beaker down.

My nitric varies from clear to yellowish depending on the sunlight exposure and other conditions. More often then not, it tends to be clear with a slight tint of yellow. If your sulfuric was colored thats most likely where you got the yellow from. 

Using distilled water and boiled down battery acid or lab grade sulfuric acid is the best way to go for good clear nitric. Even then the color can lean towards pale yellow sometimes.

Keep the liquid on ice until no more precipitate forms.


Steve


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## qst42know (Oct 25, 2008)

It takes a strong boil to get the nitrate into so little water. It may be of unknown concentration but should work well enough. I left one batch over night and the remaining salt was solid and very easy to separate from the nitric acid. All the color was grabbed by the remaining salt. The remaining acid was water clear and worked fine. Don't panic just yet.


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## viacin (Oct 25, 2008)

I finished everything up just a few minutes ago. My final liquid was crystal clear, colorless, and smells like clorox. I still cannot get the smell out of my nose. uuhg. I doubled everything on steves cold process, but did not get double the nitric. I got aprox 150ml, measured by the beaker.

This is my thinking, the final 1/3 (111g) of sodium nitrate I put in did not disolve (I had a obvious layer on the bottom, under the salt), so this can only mean that I added 1/3 (40ml) too much sulfuric acid, since it had nothing to react with. What does this mean for my final solution?

A Few Notes:
I used a graduated cylinder to measure all liquids
I used a .1g scale to measure all weights
My water was distilled
My sulfuric acid was "amazing liquid fire" straight out of the bottle


Redders: My sodium nitrate was purchased off of ebay, it came in a ziplock bag. It could be sugar for all I know. It is supposed to be technical grade, in 1/2mm pellets. Here is a picture of the bag. http://www.bodyworkzsupply.com/chem004.jpg

For full details on this procedure, please read lazersteves cold nitric process, for I am only copying it. Here is a link: http://goldrefiningforum.com/phpBB3/viewtopic.php?p=2572#2572


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## viacin (Oct 26, 2008)

I made another batch this morning. It's in ice now. Everything turned out perfect! I made sure it was fully boiling this time and all the sodium nitrate mixed in, after about 10-15 mins of stirring.

I did experience some strange things however, and was wondering if they are normal.

1. after adding the sulfuric acid, I stirred for about 10 minutes. 5 minutes into the stirring the yellow color began to fade and the liquid became cloudy with a white powder. This power slowly settled to the bottom. Is this normal?

2. after about 30 minutes all the cloud settled. My liquid was again crystal clear and colorless. The fine power that settled on the bottom formed a very hard, pure white crystallin mass with "christmas trees" standing up. I do not think this is the salt byproduct because it formed while the solution was still hot from the boiling and exothermic process. Also the salt has a yellowish tint to it, this is pure white. What could it be?

EDIT NOTE: The unknown substance is also impossible to remove from the bottom of my beaker without filling it with water and boiling for a few minutes. Eventually the bubbles break it up a bit and I can work at it with my stir rod. 

Also, is there a post on disposal of the salt and whatnot from this process? There's gotta be something better than taking it to the landfill.

Here's a good laugh for you all. The first day it took me 6.5 hours from start to completion, working hard too. Today it took about 3 hours, and I sat around for about a hour of that just waiting for it to cool. Maybe next time I can get it down to something reasonable, like 30 minutes to a hour.


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## qst42know (Oct 26, 2008)

I believe this is the remaining salt. If you wiki this its added to animal feeds, and occurs naturally in spring waters. I could be wrong but I don't see any issues in sending it to the land fill. It would be nice to have a use for it though.

http://www.jtbaker.com/msds/englishhtml/S5022.htm


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## viacin (Oct 26, 2008)

ty for the info qst. I agree, I wish we could use this. But then again it would be another chemical I would have to store for long periods of time.

I think this unknown substance I'm getting is a salt, but I'm not so sure it is the salt produced from this reaction, because I get that when I chill everything down. This unknown salt appears after the sulfuric acid is fully disolved into the mix. I just wonder if I am the only one getting this.

Also, I have a big problem here. I am exactly doubling lazersteves formula, but I am only getting about 150-160ml of nitric. It should be 320ml. This is a serious problem (waste not, want not), and I must solve it. 

It makes me wonder if I am not adding enough sulfuric acid, and this unknown "salt" I'm getting is actually sodium nitrate coming back out of the solution, if this is even possible? This would explain my missing nitric.


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## qst42know (Oct 26, 2008)

Anything indicated on the label of the drain cleaner as to additives, buffers, etc.?

I had used a drain cleaner listed to have 12 buffers the yield seemed low but I hadn't measured it. I had contributed the low yield to too short of time on the ice. The salt was fine grained and did not solidify into large flakes. It was difficult to get the fluid from the salt.

When using concentrated battery sulfuric the salt begins forming fairly quickly while stirring and after a time did solidify into a coarse crystalline mass before I put it on ice. The yield seemed higher but again I didn't measure it.

In each case the nitric acid seemed to work well enough but they were not tested side by side.


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## viacin (Oct 26, 2008)

no, the label lists nothing, not even sulfuric acid. The only way you can even tell it's in there is from the warnings. Nor can I find a MSDS on it, I have searched and searched.

I would agree with you qst, as this seems the most likely answer. But it seems to they are two different substanced. The unknown is pure white, hard as a rock when settled, and very fine. It also has little "chrismass trees" sprouting all over it reaching upward. The salt that forms after freezing is yellowish, somewhat easily crumbles, and is corse. The yellow salt is on top of the unknown substance.


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## butcher (Oct 27, 2008)

the salt should be Na2SO4 (you can test it to see if it contains nitrate).
I save my chemical byproducts for other uses.why throw away good chemicals.


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## qst42know (Oct 27, 2008)

butcher said:


> the salt should be Na2SO4 (you can test it to see if it contains nitrate).
> I save my chemical byproducts for other uses.why throw away good chemicals.



What do you use sodium sulfate for? What purpose have you found for the remains.


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## Lou (Oct 27, 2008)

Sodium sulfate is a great drying agent (dessicant) for gases and in particular, organic compounds.

High capacity for water.


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## qst42know (Oct 27, 2008)

I don't have anything I need to mummify however.

I have been doing some more reading and was wondering if one of the more chemically oriented members would explain this formula. 

From the Wiki

"Sodium sulfate reacts with an equivalent amount of sulfuric acid to give an equilibrium concentration of the acid salt sodium bisulfate[5][6]:

Na2SO4(aq) + H2SO4(aq) ⇌ 2 NaHSO4(aq) "

Could this waste salt be converted to sodium bisulfite to drop gold?


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## Platdigger (Oct 27, 2008)

That's "bisulfate" not "ite"

but hey! There are plenty of uses for that.
Randy


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## qst42know (Oct 27, 2008)

OOPS. Slight chemical dyslexia. 

One entry in the wiki may be of interest.

"Lately, sodium sulfate has been found effective in dissolving very finely electroplated micrometre gold that is found in gold electroplated hardware on electronic products such as pins, and other connectors and switches. It is safer and cheaper than other reagents used for gold recovery, with little concern for adverse reactions or health effects.[citation needed]"

Does anyone here know this process they are referring to? Or is this one of the unfounded false wiki entries?


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## Platdigger (Oct 27, 2008)

Oh well, I am glad you brought that up.

Perhaps I won't have to buy any more sodium bisulfate!


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## viacin (Oct 27, 2008)

I have read that before somewhere qst, but no idea where. I'll see if I can find it.

I just wonder what the extra salt could be. And, more importantly, why in the world I'm getting such a low ammount of nitric acid. From a non-chemisty expert's point of view (and I stress this), I would think it has something to do with the amount of sulfuric moles I'm putting in, since I'm getting exactly half, which is also what I would get if I followed steves cold process to "T" - 160ml.


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## qst42know (Oct 27, 2008)

If the sulfuric in the drain cleaner is diluted you could try boiling it first. Water is driven off well below the boiling point of sulfuric. Your drain cleaner is the big unknown.


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## butcher (Oct 28, 2008)

your byproduct salt has many uses in chemistry, can also be converted back to sodium nitrate, with a nitrate like calcium.or copper nitrate (then that byproduct can be used in another reaction, or used as a product you probbaby pay big money for (sewerline root killer or the coppersulfate for that passive stripping system mentioned on this forum or gardening ect)most chemicals we purchase are usually byproducts of some industrial processes, including sulfuric and nitric ect ect.
Viasin if you have a Napa auto store can get new Battery acid there cheap gallon or 5 gal. boil this down boiling out the water(water boils out first sulfuric boiling point is much higher and will not boil out till >98%), can get it to 98% when you see white fumes,this can be used for your cold poormans HNO3, and is much purer than the drain cleaner.
I find it also seems to make better nitric.
although I hardly ever make it poor man style as distilling for me is easy, and I dont use labware just household items ( searce my earlier post for a hard reading discription,
{ if distilling my nitric with it I dont boil all the water out as some water will help to convert the nitrate fertilyzer, and the sodium sulfate forme in reaction helps to act as dehydrator keeping water from boiling out with the NO2 gas making a stronger nitric.
it helps to look up the formulas and learn to write them and balance them then search for uses for your byproduct, you will start finding all kinds of uses for your byproducts.
edit to add another thought


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## viacin (Oct 28, 2008)

Yes, I need to try other sources of sulfuric. Buy ya know, I'm not so certian it's profitable to make my own. I was doing the math today. This actually costs me MUCH more than if I would just bought a 2.5L bottle of nitric and used the amount I produced. For the 300ml of nitric I produced, I spent a rough total of $11.75 on chemicals (1/4 of my bottle of sulfuric, and 1.5lbs of sodium nitrate), plus the 11 hours of work. I could have bought a bottle for $56, took two seconds to pour it out, and only spend $4 for that amount. Of cource, I wouldn't have learned all I did either, so i'm still glad I did it.

Now if I was buying my nitrate by the 50lb bag, and my sulfuric by the gallon, it would be a little better. Plus the 11 hours I spent on two batches was obvious noob time. I figure it should actually take about a hour per batch (you must still wait for it to cool, ya know).

I've found some nitric acid for $10/L, but it's only about 35%. Either way, this would have to be the best way to go if you don't have access to 55 gallon drums.


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## Platdigger (Oct 28, 2008)

If you don't mind sharing, were did you find 35 percent nitric for 10$/L?
Randy


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## butcher (Oct 28, 2008)

I get fertilizer and sulfuric fairly cheap compared to nitric and shipping, or driving cost, can by at local mining shop but $$$$. or drive to sandy Oregun$$$, even if I use stump remover still cheaper than buying nitric,and alot of people are finding it almost impossible to get nitric nowadays.


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## viacin (Oct 29, 2008)

Platdigger said:


> If you don't mind sharing, were did you find 35 percent nitric for 10$/L?
> Randy



Nah, I don't mind. It was sold on ebay. Here's a pic of the product
[img:154:392]http://forums.cannabisculture.com/forums/uploads/996631-pHDown.jpg[/img]

I'm finding out that there are a lot of hydroponic "ph down" products that contain nitric acid. This one is supposed to be 35%. There are several others that are anywhere from 10-40% nitric, with the other % being water or other acids depending on the brand. Most go for about $10-$25 a liter. But, as always the higher the percentage, the higher the price. Here's one I found a few minutes ago: http://www.growell.co.uk/p/1221/Nitric-Acid-pH-Down.html

You have got to find a MSDS on them first however, and check the percentage and other chemicals added.

The problem is shipping. Most of the sites I've seen are Canadian or UK and do not ship USA. I have found a few on ebay, but they charge a premium. The best bet is to cruise your local hydroponic shop. 

Now that I think about it, it seems like I've read this before. Skippy has mentioned that hydroponic stores sell nitric back in March. If he's still around, maybe he would be kind enough to fill us in on a good brand.


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## qst42know (Oct 29, 2008)

If this is the brand it's only 5-10%.

http://www.n-g-w.com/ngw/literature/technaflora_phdown.pdf


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## viacin (Oct 29, 2008)

nah, it's not that one. the one you found is this one ("ph down" on right):

[img:365:300]http://www.allseasonsnashville.com/graphics/technaflora%20ph.jpg[/img]

I looked into it last night. It does have a low price ($9.95/L), I wonder if it could be boiled down. And more importantly, how the price-to-nitric content compares to 70% for $65.


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## Anonymous (Oct 29, 2008)

Thanks for that link Viacin, I will need to check the concentration with them but it looks like you may have found my Nitric supply for me. :lol: 
If anyone else in the UK is interested this company charge the same postage if you order 1 or 50 bottles (£5.95 P+P). I will post the concentration when I have spoken to them tomorrow.


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## qst42know (Oct 29, 2008)

You cannot boil it down it must be distilled. Others have done this (distilled nitric acid) I'm sure they will respond.


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## Anonymous (Oct 30, 2008)

For those members resident in the UK, I contacted Growell Hydroponics, the company Viacin linked to in an earlier post on this thread, to find the Nitric concentration of their Nitric acid ph down. Its is 38% Nitric acid so it could be distilled if you wanted concentrated Nitric but most threads on the forum ask for 50/50 Nitric/water so it isn't far of the resulting concentration, I suppose it depends what the other 62% of the bottle is.
I would have thought that this could at the very least be used for gold recovery even if it isn't the best option for final refining.

Your thoughts and advice are welcomed


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## lazersteve (Oct 30, 2008)

Marty,

50/50 nitric is made with 1 part water 1 part 70% nitric. 

This means 50/50 is 35% nitric acid.

Steve


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## Anonymous (Oct 30, 2008)

Steve, thats what I was getting at, I realised that the percentage would be about correct, I was more concerned with what else may be in the solution, buffers etc and if they could be a problem to the reactions we would want to perform with it.
Marty


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