Questions about lazersteve's cold nitric acid recipe

[lazersteve]

Yes, potassium nitrate will work. Be sure to use the correct amount of nitrate as required by the molar weight of the compound.

Steve

 

[golddigger2]

I have tried this recipe using PH down and sulphuric acid. When i used the PH down I got the same results as you with the slushy precipitate. When i used the sulphuric I got the nice long crystals as shown in your pictures. I have placed some copper in the finished nitric but it doesn't seem to be very reactive. I used the sulphuric by weight ie 140grams of sulphuric to 100mls potassium nitrate and then heated untill combined as per the recipe. I then put in the freezer and chilled to -5 degrees C. I believe I have followed the recipe and think the only place I could have gone wrong is with the amount of sulphuric.

 

[lazersteve]

When using bisulfate, it is used in place of the sulfuric acid. The bisulfate is best used to distill with the nitrate. One mole of bisulfate to one mole of nitrate will give one mole of nitric acid, where as sulfuric acid will give two.

If you like I can show the math on the bisulfate process.

Steve

 

[philddreamer]

When using bisulfate, it is used in place of the sulfuric acid. The bisulfate is best used to distill with the nitrate. One mole of bisulfate to one mole of nitrate will give one mole of nitric acid, where as sulfuric acid will give two.
Steve[/size]

So if we use bisufate w/nitrate, there will be no sulfhate crystals @ the end of the distilling? Or, we just get a better nitric?
I'm gett'n ready to distill nitric & need the updated method. Please direct me to the posts.

Thanks!
philddreamer

 

[lazersteve]

So if we use bisufate w/nitrate, there will be no sulfhate crystals @ the end of the distilling? Or, we just get a better nitric?
I'm gett'n ready to distill nitric & need the updated method. Please direct me to the posts.

No, there will be left over sulfate. Bisulfate forms a combination of sulfuric acid and sodium sulfate when water is added. This is where the acid comes from. The left overs are exactly the same as the sulfuric acid reaction.

Steve

 

[philddreamer]

Thank you Steve!

Is there a post with a diagram of what the set-up for distilling looks like. From what I've read, I have a general idea, but better safe than sorry.
I don't want to use ware not suited for the process.

phil

 

[lazersteve]

Thank you Steve!

Is there a post with a diagram of what the set-up for distilling looks like. From what I've read, I have a general idea, but better safe than sorry.
I don't want to use ware not suited for the process.

phil

All glassware distillation rig with water cooled condenser.

Simple Distillation Apparatus

Steve

 

[philddreamer]

Excellent!

Thank you Steve.

Phil

 

[nimrood]

Am i missing something, wheres the Sulfuric Acid? This is great news for me because Sulfuric Acid is hard to get here in Australia.

Steve, can i substitute Sodium Nitrate for Potassium Nitrate instead?

And can i pickle my silver in the Sodium Bisulfate also?

The sodium bisulfate is used in place of sulfuric acid.

Bisulfate in water can be used as a substitute for dilute sulfuric acid in many instances and should work for pickling gold.

The bisulfate provides the acidic hydrogen needed to convert the sodium nitrate into nitric acid.

I have not tried this reaction with potassium nitrate. Give it a try and let us know what you find.

Steve

hi. this is my first post to the forum. i've been lurking and reading for several weeks and finally created an account a few days ago.

i hail from georgia, the nw-atlanta-metro area. one might think it wouldn't be difficult to find a local supply of sodium nitrate in a southern farming state.... but i've looked all over and can't find a reasonably close local supply. KNO3, however, is all over the place. i didn't see anyone respond regarding the substitution of potassium nitrate for sodium nitrate in the bisulfate/nitrate cold recipe. so, i'm giving it a go!

based on what i've read, i made up the following mixture:
1) 108g NaHSO4 dissolved in 150ml of water @ ~85-95C (sol. vol. increased to ~200ml)
2) dissolved 77g of KNO3 into the NaHSO4/H2O solution @ ~85-95C (sol. vol. increased to ~250ml)
3) filtered hot solution into a long neck, flat-bottom 250ml flask
4) stoppered the flask and put it in the freezer (about -17C to -15C)

i checked the solution about 3.5hrs later and noticed a fair amount of long clear crystals. i decanted, measured (~125ml), and tested the solution on a piece of copper. i didn't observe an immediate reaction w/ the copper as i expected (maybe it was too cold?). crystals appeared to still be forming on the surface of solution, so i popped it back in freezer for another 30min.

i checked the solution again, measured it (~100ml), and i am performing another copper test. this time i will let the copper test sit outside to warm up. i lost 25ml of solution in about 30mins, so i decided to decant it and put the flask in the refrigerator which is about 1-2C. the color of the solution is clear with a very faint amber tint, and it does not have a familiar odor (not much of an odor at all, actually)...at least not as cold as it is right now.

at the time of this posting, still no reaction with the copper.... so must come to one of these conclusions: (a) KNO3 isn't a good/valid substitute for NaNO3; (b) i didn't do something correctly; (c) it produced a very very weak nitric.

 

[jimdoc]

Is this place near you? They ship if not, I have ordered from them.

http://www.maconfeedandseed.com/product_info.php/products_id/103

Jim

 

[nimrood]

Is this place near you? They ship if not, I have ordered from them.

http://www.maconfeedandseed.com/product_info.php/products_id/103

Jim

i consider macon an unreasonable distance--about 1.75hrs drive south of my location. i don't think my wife would tolerate that kind of day trip. 8) however, we do go through macon when we go to visit the in-laws deep south GA, but there's no telling when the next trip will be as i don't particularly like my in-laws!

 

[nimrood]

based on what i've read, i made up the following mixture:
1) 108g NaHSO4 dissolved in 150ml of water @ ~85-95C (sol. vol. increased to ~200ml)
2) dissolved 77g of KNO3 into the NaHSO4/H2O solution @ ~85-95C (sol. vol. increased to ~250ml)
3) filtered hot solution into a long neck, flat-bottom 250ml flask
4) stoppered the flask and put it in the freezer (about -17C to -15C)

i checked the solution about 3.5hrs later and noticed a fair amount of long clear crystals. i decanted, measured (~125ml), and tested the solution on a piece of copper. i didn't observe an immediate reaction w/ the copper as i expected (maybe it was too cold?). crystals appeared to still be forming on the surface of solution, so i popped it back in freezer for another 30min.

UPDATE: i tested the solution some more this morning and had a reaction with copper after applying heat. so the conclusion is i made a very very weak nitric by substituting KNO3. i wondered to myself "maybe must not be a 1:1 relationship here." a few calculations later, and it appears i didn't use enough KNO3:

77g KNO3 = 0.761 moles
77g NaNO3 = 0.906 moles

therefore: 91.5g of KNO3 == 77g of NaNO3.... time to try this again with the new formula.

 

[GOLDMAN1234]

I have dissolved roughly 30 cpu in a 3 -1 mixture of hydrocloric and nitric acid,after 2 days the good pins have not fully dissolved,which acording to my guide the should have ,what should my next stage be i have been told to add 100ml of AR to strip the plating of the gold pins.NEED HELP GUYS PLEASE PLEASE PLEASE

 

[Harold_V]

I have dissolved roughly 30 cpu in a 3 -1 mixture of hydrocloric and nitric acid,after 2 days the good pins have not fully dissolved,which acording to my guide the should have ,what should my next stage be i have been told to add 100ml of AR to strip the plating of the gold pins.NEED HELP GUYS PLEASE PLEASE PLEASE

Lets start with what you've been reading. Has it been Hoke? Do you understand the ramifications of using AR and not completely dissolving all of the metal?
Do you know what stannous chloride is, and for what it is used?

We can help you with your project, but it's more important, right now, that you help yourself by addressing some of the basics of refining. Don't discard anything---and if you have a safe place to store your material while you do some reading, do so. Remember, the fumes are quite corrosive, so don't store anything in your garage or anywhere you have things of value that can rust.

If you don't know about Hoke's book, do a search for Palladium. In his sig line you will find a link that permits a download of Hoke's book.

Read Hoke.
Read Hoke again.
Read Hoke until you understand what she teaches. At that point in time, you shouldn't have any questions about what's going on with your project, and if you do, we'll be here for you.

Harold

 

[dtectr]

If you don't know about Hoke's book, do a search for Palladium. In his sig line you will find a link that permits a download of Hoke's book.

Read Hoke.
Read Hoke again.
Read Hoke until you understand what she teaches. At that point in time, you shouldn't have any questions about what's going on with your project, and if you do, we'll be here for you.

Harold

I might add here - take the time to conduct her Familiarization Experiments to the extent possible for you. Nothing is actually lost if you follow the instructions, & based on my own brief experience, it can literally save you months of stumbling around in the dark.
dtectr

 

[ExNuke]

I haven't posted before on the Forum but I've been reading it extensively for several months now. Is this thread too old to hope for a reply? My question is would lazersteve's recipe work ok for distilling and would that give Nitric acid that was suitable for silver without giving me a bunch of silver chloride? I'm only doing small batch hobby level recovery and refining of silverand the cost of commercial Nitric Acid is a pain in the wallet.

 

[maynman1751]

Yes, Lazersteves recipe will work if you distill first. It must be distilled in order to work properly with silver. Just make sure to use all safety precautions when distilling and using Nitric. You are new here and need to understand the dangers of using these hazardous chemicals. Be safe!!!!!

 

[ExNuke]

Yes, Lazersteves recipe will work if you distill first. It must be distilled in order to work properly with silver. Just make sure to use all safety precautions when distilling and using Nitric. You are new here and need to understand the dangers of using these hazardous chemicals. Be safe!!!!!

Thanks for the reply. I understand the safety caution and need for it, I'm new to refining but not to working with less than safe chemicals and use a pretty complete suite of safety gear. Other than the cost of Nitric Acid my biggest problem is finding enough scrap silver to justify setting up my cell, So far I've produced ~750 grams of pretty nice crystal from salvaged electrical contacts with a stainless bowl cell , so far my biggest expense with refining has been a liter of HNO3 with the Hazardous Shipping Fee. The rest of my gear has been re-purposed or home made, that is half the fun.

 

[JRB3]

And IF I could find a source of nitric that did not cost an arm, leg, and other body parts I am fond of I would certainly not bother making it.

Virgil

I also am a Noobie to this sight and haven't been able to walk away from it since I recently joined. I had some info for you rearding to buy or to make nitric acid. So not sure what a body part goes for on the black markrt nowadays ( whether it's your favorite one or not ) but I just purchased a 1L of 50% for just over 70.00 with tax and shipping to my door the GRAINGER.
I'm not thrilled with having it delivered to my door, as well as a paper trail also leading to my door, not that I'm doing anything illegal I just don't care for everyone knowing my business 24/7. I had already spent that amount getting ready to make my own etc when I came across it in their catalog ( BOOK , if I added 15 more dollars I could have bought 2.5L but it comes in a wine box looking container, at least the one I bought comes in the appropriate amber bottle. The larger amount compelled me to buy amber bottles to house that amount of Acid which would double the cost. So if you have the glass or can see using that amount in 24 months it really is cheap. They also sell a 500 ml for around 50 out the door. Oh last catch 2 week wait time for delivery at least out here to Ca., it comes from idaho so shipping time could be less if live closer than I do.
So thats it I am about to go make my own since I can't seem to wait for the snail mail to arrive. Thank you everybody who has made this forum and site what it is today.
Lastly I do alot of reading on the computer no so much blogging or answering topic questions, So I probably didn't do this right and if that's the case allow me to apologize in advance and please excuse my mistakes - Jim

 

[ExNuke]

New Question. How does anyone go about cleaning the salts out of your reaction vessel after cooling? After pouring off the newly made acid the salts are like a rock, I'm sure people aren't just throwing away glassware. ( The Acid works fine! ) I found Hy-Yield Nitrate of Soda at the local garden center @ $9.00 for 4 pounds. Even with Walmart Drain Cleaner sulfric acid it's a lot cheaper to make HNO3 than to pay the Hazmat shipping fee.