Refining Gold from Gold Filled Jewelry

[Oneal58]

Hi Butcher,
Butcher, for the life of me I can not find the step by step instructions of making the nitric with Lazersteve's method. I clicked on the link you sent me and the site takes me to the pages where everyone is discussing the method but I can't find the step by step instructions by Lazersteve?
I also have done many searches on Lazersteve's cold nitric method and each time I can find where everyone is discussing the method but I can never find the post by Lazersteve on the exact instructions? I guess this flu bug has effected my mind. But for the life of me I cannot find the link that is posted with the instructions on how to make the nitric with the method that you said to use? I don't understand this, I have looked many times and just can't find it.
Do I have to go to Lazersteve's site to find it? I have done that too with no luck.
I guess you will have to hit me between the eyes with it before I will see it today?
Thanks Butcher,
Oneal

 

[Oneal58]

Hi Butcher, after looking again I think I finally found a version of the method Steve said he was going to post. Steve posted on April the 23rd, 2007 the method below and then on the 25th of april he stated he had come up with a new method he would post later that was even better. I found the method he posted on the 23rd but I can't find the updated version he posted later that he announced 2 days later he was going to post? If you will for me, please just verify this is the latest/last post on the updated method that Steve uses for his cold nitric method. He said he was going to post an updated version but I just can't find it? So, I just don't know which one I have here.
Sorry to be such a bother Butcher. I just want to make sure I am on the right, updated version of the method. I need to spend more time surfing the site to get more familar with it for sure.
Thanks,
Oneal

Reaction:

-Bring 100 mL of Distilled Water in a 500 mL pyrex beaker to 100 C
-Add the Nitre of your choice (202 gm K / 170 gm Na)
-Stir until Nitre is completely dissolved, let cool below boiling
-SLOWLY add 56 mL conc (96%+) Sulfuric Acid to Hot Nitre solution while stirring, DON'T allow the solution to boil!
-Allow solution to cool to room temp (DO NOT SKIP - VESSEL WILL SHATTER IF PUT ON ICE WHILE HOT!!!)
-When vessel reaches room temp (25 °C) put the vessel in the freezer or on a salt water ice bath
-Let stand until temperature of mixture reaches -5 °C
-Let stand at -5 °C until all precipitate settles
-Pour the COLD solution off into glass container with tightly sealed lid DO NOT POUR OFF ANY OF THE SALT IN THE BOTTOM!!!
-Makes ~160 mL ~50% HNO3

 

[butcher]

Oneal that is the recipe to use, just follow the instructions, you are probably just looking too hard.
Pay close attention to how he says add chemicals, and cooling parts.

The only other recipee for nitric acid I can think of, was one Steve used, was where He used sodium bisulfate to act as H2SO4 in the reaction to make nitric acid with the nitrate salts.

Laser Steve's nitric acid recipe
-Bring 100 mL of Distilled Water in a 500 mL pyrex beaker to 100 C
-Add the Nitre of your choice (202 gm KNO3 Or 170 gm NaNO3)
-Stir until Nitre is completely dissolved, let cool below boiling
-SLOWLY add 56 mL conc (96%+) Sulfuric Acid to Hot Nitre solution while stirring, DON'T allow the solution to boil!
-Allow solution to cool to room temp (DO NOT SKIP - VESSEL WILL SHATTER IF PUT ON ICE WHILE HOT!!!)-
When vessel reaches room temp (25 °C) put the vessel in the freezer or on a salt water ice bath
-Let stand until temperature of mixture reaches -5 °C
-Let stand at -5 °C until all precipitate settles
-Pour the COLD solution off into glass container with tightly sealed lid DO NOT POUR OFF ANY OF THE SALT IN THE BOTTOM!!!
-Makes ~160 mL ~50% HNO3
(protect from light, light destroys nitric in storage)

you can make lager batches at once:
approximate six times as much for above formula above I use in a coffee pot on hot plate :
6 x 100ml boiling water = (600ml H2O)
6 x 202g KNO3 = (1212 grams KNO3)
or
6 x 170g NaNO3 = (1020 grams NaNO3)
6 x 56 ml (98%) H2SO4 = (336 ml 98% H2SO4)
to produce approx
6 x 160ml = 960 ml of about 50% HNO3

 

[maynman1751]

Could you then take this solution and evaporate it to get 68% Nitric?

 

[Oneal58]

Thank you Butcher, I have always been able to count on you, day in and day out. That means a lot to me and I will never forget it. I am truely thankful you are here!. As well as all the other members of this site!
Question 1-Butcher I noticed you have to use a little more Potassium Nitrate than you do Sodium Nitrate in the recipe? Why is that?
Question 2-Also, can I use one of the methods to clean up my Potassium Nitrate and will it make a difference in the final product if I do? Or will I just be spinning my wheels going to extra work for no returns. As you have said, In what we do I need nothing more than 50% nitric and If I get that from Steve's Recipe why go to any other steps, do you see it this way?
Butcher, I will probably finish up my gold filled Jewelry I have collected over the years in this next week or so. My final end goal has always been to get to the catalytic converters. There is just too much competition on the gold that is available and I don't want to have to run the roads to find it.
I have friends in the junk car business that sell to catalytic converter buyers that come by their junk yards almost on a daily basis. They then sell to a buyer that then sells to a refiner. I live in a very rural area, middle of no where really. There are salvage title car/truck rebuilders on every country road here. Mostly farmers who could no longer make it farming for a living. I can think of 4 within 5-10 miles of me and 8 within 20 miles. Large junk yards with hundreds of cars, trucks, Etc;. I know that the catalytic converters are long gone on those hundreds of vehicles sitting in the junk yard though. But these guys (owners) work slavage sales almost on a daily basis and bring in new inventory almost everyday.
I have talked to a couple of these yard owners and if I can cut out the middle men here I can offer them a little more for each converter. It's all about the money as you know and I could essentially cut out the buyers that do not do their own refinning. I hate to do that but my portion would be small and I would not put anyone out of a job or much of their income. I know they have to feed their family too.
Now, from what I have learned so far this (recovering PM's from catalytic converters)
is one of the best kept secrets in America. A lot of what I have read would take someone with a PHD to understand. I think it's written that way to discourage the regular guy from trying it. I pick up bits and pieces of how to go about refining converters but no where have I found the A-Z process.
Question 3-Is there a good book you could recommend or does Lazersteve's Video on converters get into the detail that I am needing to know before I get started?
I have been too busy trying to refine gold filled Jewelry to do much studying on the converters. This will change in a week or so. Do you have any advice on where and how I should start?
Thank Goodness for this site, it would have been impossible for me to have taken on any of this without your help and the other members of this site so freely giving information to the common guy to accomplish these task.
As Always, Thanks Butcher,
Oneal

 

[butcher]

Dilute nitric acid can be concentrated up to 68%, by evaporating off water, if not boiled fumes are high in water content,
(After 68% azeotrope is reached both fumes and acid in evaporating dish would be 68% until all of the nitric evaporated).

you need more potassium nitrate than sodium nitrate in the reaction, (because of Moles), nope not the little critters in holes in your garden, but the molecular weight of atoms of these metals (sodium and potassium metal) in the chemical reaction, I will not go into more detail now, but these formulas are calculated by molecular weight of substances.

You can re-crystallize a salt to make the crystals more pure, (very pure), dissolving an impure crystal in a solution it is soluble in, (this case water), then heat to drive off water as fumes, until crystals form (when salts crystallize they try to reject most impurity), removing the crystals and repeating the process you can get very pure crystals.

As far as the nitrate fertilizer I usually would not worry about re-crystallizing them, if much dirt in fertilizer you can filter the hot dissolved sodium nitrate, before adding the sulfuric (my fertilizer where usually so clean I did not worry about it),
If you had traces of chloride in the fertilizer and you were concerned you could add a few drops of silver nitrate to your nitric to remove the chloride (as insoluble silver chloride in the bottom of the nitric acid) (I did not mess with this for home-made nitric, I can just use store bought if I was concerned about purity). Most of what I use poor-mans nitric for a trace of impurity gives me no problems.
Distilling is a good way to get purer nitric (leaving unwanted salts behind) and if any chloride did distill over using AgNo3 to remove them.
Just like re-crystallizing a salt, redistilling a solution also can be used to purify the solution.

I would just make the nitric from the fertilizer as is, unless your using it for very high grade chemistry the little impurity you will not notice (except for sulfate salt and silver as mentioned in above posts).
Again let’s just keep it simple as possible.

Hoke's, the forum, and information from LOU, Harold, and Laser Steve,and other's, you should be able to recover and and refine most anything even cats
(not house cats, no hope for learning about recovering them on the forum, ask palladium about recovering them).

 

[Oneal58]

Thanks Butcher,
Butcher, what is the wattage rating on your burners on your stove? I ask because I find that a 900 Watt Burner is not big enough to bring a 800ml or greater solution up to steaming without giving it a lot of time. I have been looking for a double top solid burner for a couple of weeks or so. But every one that I am finding has only a 900 Watt Burner (large burner) on one side and a 600 or 750 watt burner (small burner) on the other. I have already exploded 2 clear pyrex casseroles on my stove, that's with a piece of thin stainless steel drilled full of holes used for an underplate on the element. I no longer use clear pyrex casseroles and use the white porcelain ones now after reading this happened to someone else on the site. I always use a catch basin under my container bearing my solution also, which steals heat away from the container with solution. Takes it a long time to heat up to steaming. I would like to find at least a 1200 Watt burner Stove on one side with a 600 Watt on the other side. This would still keep me within NEC Ratings for a continuous duty circuit, single phase 120V/20 amp breaker on #12 Guage wire. This would still leave me an amp to play with.
So, I guess what I am asking is what size (wattage rating) is your largest element on your stove and is it solid. Also, do you use a catch basin container of some kind beneath your solutions, even with the solid element? If you have a larger element (1200 watt double burner (largest element) where did you find it and do you like it?
One more question, if you have a spill of gold bearing AR and mop it up with a paper towel. If you dry and then burn this towel does the gold revert back into a solid or are the particles so minute that they just float away in the smoke? Would it be best to wash the paper towels in Hydrochloric a few times, using fresh Hydrochloric for each wash until they are white again? Is there a better way to recover the gold bearing liquid they hold?
I ask this because I have some nice yellow paper towels that doesn't match the decor in the room where I am working. I want to get the yellow back out of them/white goes better with everything in the room. :lol: I have the towels in a sealed container to keep them from drying out until I find out what to do or how to recover this gold.
One last Question, when cooling the solution for the cold nitric method, how critical is it to keep the solution at -5 degree Celcius. If in the freezer will it not tend to go lower than -5 degree C. Do I keep taking it in and out of freezer to maintain this temperature?
Thanks Butcher,
Oneal

 

[butcher]

The hotplates I use look just like these at sears, but I get mine at bi-Mart for a little over 20.00 new, much cheaper if I find it at second hand store.
http://www.sears.com/shc/s/p_10153_12605_SPM6296037902P?prdNo=7&blockNo=7&blockType=G7


I am not sure about wattage off the top of my head I can check later, but I measured the burner temperature before and I think it was something like 600 deg. F for large burner and 400 deg. F for small burner on high. (My guess around 1000 watt total)
The hotplates I use look like this, although I get mine at bi-Mart for a little over 20.00 new, much cheaper if I find it at second hand store.
I am not sure about wattage off the top of my head I can check later, but I measured the burner temperature before and I think it was something like 600 deg. F for large burner and 400 deg. F for small burner on high.

I will use Mr. coffee type coffee pots directly on the burner, but also I am very careful about thermally shocking the glass, I almost never have trouble with one cracking, unless I screw up, and change temperature to fast or try to heat with much salts or solids in bottom.

The white corning ware casserole dish will take much more abuse, and I can heat salts or layers of metals in the bottom of them or even incinerate in it.

If you are breaking vessels on hotplate then use a shallow pan with layer of sand (sand bath) between the burner and reaction vessel.

I also use a propane burner similar to camp stove, if I need higher heat, but for most things I like the electric burners.

do not change temperature of glass fast it thermally shocks it, also distributing the heat evenly helps so as not to create hot spots, also use thin glass made for heating (most thick glass is not made to heat).

your spill of gold chloride solution mopped up in paper towels is still gold chloride, burning the filters in my mind would be a mistake without first washing them in a dilute solution of sodium hydroxide, this will make the chlorides into table salt that is water soluble, and can be rinsed out, so that when you burn the filters the gold will not dissolve into the smoke. I am not sure if the smoke from chloride and gold is just chlorides or if it also forms chlorine gas, but it will dissolve gold and carry it away in fumes at these temperatures, neutralizing and washing away the chloride from the salt before incineration is what I do.
If you melt gold with table salt the fumes will carry off some gold, how much more would be carried of in the acidic chloride fume I do not know but would guess to say a considerable amount.
Just ask Harold' how much value he recovered from his fume hood.

The white corning ware casserole dish will take much more abuse, and I can heat salts or layers of metals in the bottom of them or even incinerate in it.

If you are breaking vessels on hotplate then use a shallow pan with layer of sand (sand bath) between the burner and reaction vessel.

I also use a propane burner similar to camp stove, if I need higher heat, but for most things I like the electric burners.

do not change temperature of glass fast it thermally shocks it, also distributing the heat evenly helps so as not to create hot spots, also use thin glass made for heating (most thick glass is not made to heat).

your spill of gold chloride solution mopped up in paper towels is still gold chloride, burning the filters in my mind would be a mistake without first washing them in a dilute solution of sodium hydroxide, this will make the chlorides into table salt that is water soluble, and can be rinsed out, so that when you burn the filters the gold will not dissolve into the smoke. I am not sure if the smoke from chloride and gold is just chlorides or if it also forms chlorine gas, but it will dissolve gold and carry it away in fumes at these temperatures, neutralizing and washing away the chloride from the salt before incineration is what I do.
If you melt gold with table salt the fumes will carry off some gold, how much more would be carried of in the acidic chloride fume I do not know but would guess to say a considerable amount.
Just ask Harold' how much value he recovered from his fume hood.

 

[Oneal58]

Hi Butcher, thanks for all your help. I will give you a rest tonight. I will follow your directions on everything you have answered for me today. I do really appreciate you.
BUY THE WAY, HAPPY NEW YEAR!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!
SEE YOU IN 2012, Wow, time is just a flying. Hopefully this time next year I will be answering some simple questions instead of asking, asking, asking all the time.
BUY THE WAY, HAPPY NEW YEAR TO EVERYONE HERE, ALL OF YOU ARE APPRECIATED. KEEP SAFE TONIGHT.
A Southern saying,
KEEP THE WHEELS BETWEEN THE DITCHES AND THE BOOGERS OUT OF YOUR BRITCHES!!!!!!!!!!!
Oneal

 

[Oneal58]

Hi Butcher/Everyone, I hope you'all had a wonderful holiday.
I have ran into some problems with the formula below and hope you can get me back on track, or try and find the problem.
I followed the recipe exactly you gave me, the one that is 10X's the amounts given in Steve's Recipe.
1-Measured out exactly the amounts needed X 10, brought the distilled water up to 100 degree's C.
2-Added the Potassium Nitrate, X10, and stirring until the KNOS had dissolved completely.
3-Lowered temperature below boiling on solution and added ROOTO Drain Cleaner, 94% sulphuric, X's 10
5-Stirred well and then took off heat.
6-Let cool outside untill temperature was 72 degrees F.
7-Put solution in freezer, lowered to -5 degrees C.
Butcher, I made 4 batches of this without stopping. I worked all night on it. Sun was coming up when I went to bed.
I only ended up with no more than 250ml of solution on every single batch? I tested the Nitric and it is good strong Nitric. But I am only getting 250ml of Nitric out of each batch, the rest turns to rock hard salts?
I end up with rock hard salt in the bottom of each vessel, How in the world do I get this salt out of the 4 vessels I have it locked up it. It (salt) is rock hard? I have 4-12 cup coffee pots full of rock hard salt?
Almost all, well all but 250ml turns into salt in the vessel.
I am using soluable KN03 (Potassium Nitrate). The fertilizer is clean as far as I can tell?
Butcher, I don't know what could be happening, I know I should be getting around 960ml out of each batch but I end up with mostly rock hard salts and 250ml of Nitric.
Do you have any idea of what is going wrong? I have checked and double checked the directions/amounts used and I have followed them exactly.
Do you possibly know what is going on?
How in the world do I get these rock hard salts out of my vessels?
Has anyone else experienced this with their method of making the Nitric?
Thanks Butcher,
Oneal

Oneal that is the recipe to use, just follow the instructions, you are probably just looking too hard.
Pay close attention to how he says add chemicals, and cooling parts.

The only other recipee for nitric acid I can think of, was one Steve used, was where He used sodium bisulfate to act as H2SO4 in the reaction to make nitric acid with the nitrate salts.

Laser Steve's nitric acid recipe
-Bring 100 mL of Distilled Water in a 500 mL pyrex beaker to 100 C
-Add the Nitre of your choice (202 gm KNO3 Or 170 gm NaNO3)
-Stir until Nitre is completely dissolved, let cool below boiling
-SLOWLY add 56 mL conc (96%+) Sulfuric Acid to Hot Nitre solution while stirring, DON'T allow the solution to boil!
-Allow solution to cool to room temp (DO NOT SKIP - VESSEL WILL SHATTER IF PUT ON ICE WHILE HOT!!!)-
When vessel reaches room temp (25 °C) put the vessel in the freezer or on a salt water ice bath
-Let stand until temperature of mixture reaches -5 °C
-Let stand at -5 °C until all precipitate settles
-Pour the COLD solution off into glass container with tightly sealed lid DO NOT POUR OFF ANY OF THE SALT IN THE BOTTOM!!!
-Makes ~160 mL ~50% HNO3
(protect from light, light destroys nitric in storage)

you can make lager batches at once:
approximate six times as much for above formula above I use in a coffee pot on hot plate :
6 x 100ml boiling water = (600ml H2O)
6 x 202g KNO3 = (1212 grams KNO3)
or
6 x 170g NaNO3 = (1020 grams NaNO3)
6 x 56 ml (98%) H2SO4 = (336 ml 98% H2SO4)
to produce approx
6 x 160ml = 960 ml of about 50% HNO3

 

[butcher]

Oneal,
A couple of things to consider, were all of the potassium nitrate salts dissolved in boiling hot water before adding concentrated sulfuric acid, (if some was crystals you may not have gotten a complete conversion and still have nitrates locked up in the sulfate crystals).

Potassium salts seem less soluble than sodium salts to me (if your crystals formed too quickly you may have not gotten complete conversion or crystals may have just locked up some nitric in crystals), did you slowly cool and separate salts from liquid before freezing?

Either way, I would separate the liquid (nitric you have now), from cold crystals, put the wet crystals back the reaction vessel add just a little water not much (I would also give it a little 3% hydrogen peroxide but not necessary) then add a little sulfuric acid,(remember the rule about the danger, Do not add water to concentrated sulfuric acid). (we are not trying to dissolve these salts till hot, (this first addition of liquid is just to keep salts wet till we get them warmed up, so we do not burn them, (we can add more liquid later if needed).

Heat, till salts dissolve again, (my goal would be to get any water then acid we added just to about 68%), (about 2ml H2O for every 1ml H2SO4 added), and only adding as much of this to dissolve the crystals at just under boiling temperature, so starting with just a small amount of liquid at first, start raising heat (slowly raise heat, till glassware temperature comes up, remembering not to thermally shock your vessel), as heat is raised you may see you need more dilute acid to get all crystals dissolve just below boiling with good stirring.

Once all of the salts dissolve, slowly start lowering heat on vessel. I would not just turn off heat, but lower it about half way down, after solution cools some you may see some crystals already begin to form, (the slower we form the crystals the purer they will be), then turn off heat, but we want to cool this as slow as possible so the crystals of potassium sulfate will grow slowly as possible, once cool to about room temp and well settled, decant liquid from crystals, the crystals I save for the potassium sulfate salts, the liquid now put in freezer and freeze out more salts, I would keep the first batch of nitric you made separate from this second batch, and test each batch, (in small vessel like test tube’s or cups maybe on a gold plated pin or small piece of copper see how each react on copper, if reaction is similar then I would not worry about putting both batches in one bottle.

(I will add this, but I do not want to confuse you more), (if you don’t understand forget this paragraph and just use instruction above)
Now you have several batches of this, I may add just a little water then acid to each batch of salts (just enough to wet so I could make a thick slurry of each. then when I heated the first batch and had it dissolved into liquid, (using instructions above) and all dissolved just under a boil, add more of the remaining slurry of salts a little at time, stir well to dissolve to this hot mix with stirring once I had starting to get about 1/2" layer of salt in bottom (still hot and good reaction time, that would not dissolve) I would decant this liquid into next batch of salts (slurry of next coffee pot), (but taking care not to thermally shock glass pot, so you will need to lower heat somewhat of the hot solution pouring into cooler pot), basically what we are trying to do is re-dissolve all of the salts and re-crystallize them (for higher purity salts) and get any nitrates into a solution of a fairly good concentration of nitric acid, with as little as more added liquid as possible, You could even use some of the nitric you made earlier to do this with (instead of adding as much new water and sulfuric acid).

I have a hard time explaining what I mean, it is easier for me to just see something and do it, than it is to explain to someone how I think, and explain to them how I may do it. (Trust me my mind is a jumbled mess of thoughts).

You may also find another explanation about how others have re-crystallized their salts

 

[qst42know]

I would guess some of your nitric is being held by capillary action in the salt crystals.

Something you could try on your next batch is to let your solution set at room temperature to allow some of the salt to form. Filter that out and then chill the solution. A more open crystal of the remaining salt may allow your nitric to drain out better.

You might try to gather some of the trapped nitric with ice cold water. Fill a vessel with ice and add some water. When it's good and cold pour some in the first coffee pot swirl it around a bit and drain into the next pot and then the next. Keep transferring the same water from pot to pot you should collect some dilute nitric with some dissolved salt.

The remaining salts in your coffee pots will be water soluble.

 

[Oneal58]

Thanks Fellows, I appreciate your help. With what yall have told me, I might have a clue what I did wrong but not sure?
Here is what I did!
1-Measured out everything I would need first for all 4 batches I was going to run,my plan was to run each lot behind the other as quickly as possible. I then brought distilled water to boil on first batch.
2-I then added KN03, all at one time, water temp droped immediately, I brought water temp back up, I noticed the KN03 salts wouldn't go into solution until the temperature reached about 90 degrees C.
3-Once salts dissapeared I continued on up to boiling, 100 degrees C., stirring constantly.
3-I lowered temp of solution to around 85 degrees C.. I then added the H2S04 while stirring constantly.
4-It was cold outside and wind was blowing so I put containers outside so the cold wind could help to get the temp to lower quicker. I watched the temp on the vessels untill they reached 25 degrees C. I was about 15 minutes between all 4 of the batches I ran. I mean (after) all 4 had cooled to 25 degrees C., that took a while, a long while. It amazes me how these salts hold heat so well?
5-I then took the vessels straight to the freezer, as soon as each solution hit 25 Degrees C., I did notice that salts were already growing in containers before I got solution to freezer.
6-As each solution hit -5 degrees Celcius I would go straight out and filter solution into HN03 Jug, within minutes. I knew the next one would be right behind the previous one. I did this one behind the other until I was through with all 4 batches.
As I said, I ended up with less than 1100ml out of all the 4 batches. These 4 batches sure worked my tail off!

Here are some possibilities of what I did WRONG! Let me know?
1-after salts dissolved in solution I carried the solution up to 100 degree C. and then added the KN03 quickly.
2-I did not let solutions cool (at) room temp, I cooled down (to) room temp (25 Degree C.) artificially, outside with a cold wind blowing. I sit each batch up on a shelf outside so the wind could help cool it down quickly.
3-I did not seperate liquid from salts before going into freezer, even though I already had salts forming/growing.
4-I did not allow any time between freezer and filtering into HN03 jug.

I did at least cover the salts with water hoping this was the right thing to do until I could find out what to do on the forum. There was not much room for much water, salts almost filled the coffee pots, (12 cup pots). I still have them sitting outside with water over the salts.
From what you are telling me it's still not too late to try and recover some of the Nitric locked up in the salts? Can I follow your directions now to try and salvage some of the Nitric that I can still see in the salts?
Question-Can you point to any 1 or maybe 2 or more things that I did that I shouldn't have done?
Thanks,
Oneal

 

[butcher]

Sounds pretty much like you covered anything I can think of.

Maybe I should have not told you about making big batch until you made a few small batch's first, to get the feel of things, it is usually better to learn to build a dog house before building the big house.

 

[Oneal58]

Hi Butcher, my personality traits I have gets me into trouble all the time. I will slow down to one lot at a time from now on. Doing just one lot correctly would have gave me the same return as working until the sun was coming up this morning.
I will take everything you posted to heart and spend the time dissolving, letting solution cool at room temp, decanting solution before freezer trip, Etc;.
As always, thank you so much for keeping me straight. I know, it's a hard job to teach someone with such a hard head! I ask my grandson all the time where he got his hard headedness from? I guess I have been in denial all my life?
Thanks again Butcher,
Oneal

 

[butcher]

Oneal, actually you’re a quick learner, and I enjoy trying to help the best I can.

We have a mule named Rosy, and as stubborn as she is she fits right in with me and my family, nope we are not stubborn in our family, we are just mule headed.

When Rosy was younger I was training here to pull a cart and to log, was training her to the reins, I would yell get up, after a few tries she did, darned ole mule took off running drug me around the field about twice before stubborn ole me come to my senses and let loose of the reins, I thought I could hold on and not let her get away, it does not work that a way, a mule can drag you around like a sack of potatoes bouncing behind her, the sack of potatoes (me), just scared her more, while she is trying to get away from that sack of potatoes chasing her. I could not walk for about a month after that, so she was smarter than me and my stubbornness, she got out of work for about a month, till I could walk again.

After that every time I would log with her and yell get up, she would first start off at a run, (I never could break her of that habit), (not so much trouble when your in a cart, but when logging, I would have to try and keep out of the way of that darn log, after she got the log going good she would slow down and just pull it, and we got the logs to where we needed them, she pulled the cart well,
(Well) she only tore it to pieces a couple of times when she got spooked.

Rosy is 28 years old now and my daughter keeps her, she don't have to work any more, she’s retired. Spends her time wondering when her next treat and meal will be ready

 

[Oneal58]

My goodness,
I never thought I would talk to someone who has followed a mule as I have. My father was a share cropper and us children, 5 of us, would have to hit the fields everyday after school and work in the fields until dark. We hand picked our cotton in the fall and after we finished picking our cotton I would pick for others in the community for 1 cent a pound. To make a $1 bill was an all day job for a boy my age. My hands would be so sore and cut up I could hardly move them. During the summer we (traded out) with the tobacco harvest (the money crop). That means that we would go help other neighbors gather their tobacco on harvest day and they would come help us on our harvest day. We traded out with 3 different families (lot of work in 8 acres of flue cured tobacco) each family. Daddy always traded with people who had the same amount or as near the same amount of tobacco as we had. That put us working every single day and on Sat. during the summer gathering tobacco for 9-10 long weeks (sometimes longer) back then. So, in total that put us gathering approximately 32-35 acres of tobacco a week. Hardest work I have ever done in my life. Getting up at 2:00 a.m. with Daddy on our gathering day to first haul pre-filled barrels of water to the barn and pour onto the dirt floor in the barn. The floor of the barn would be hot after shutting down the burners, curing the tobacco took all week long. You shut down the burners the morning of the day you gathered tobacco. This water would make steam when the cold water hit the hot floor of the barn. The reason for this was that this brought the tobacco in Order (meaning, tobacco soaked up the water vapor) so you could handle the tobacco without breaking it to pieces. Then to unload the barn and working until dark. Lots of times we had to hang the tobacco in the barn after it was croped, hand strung and stacked. Waiting on the men to come out of the field to hang the tobacco (only women at the barn/1 man to stack tobacco/unload the drags). Then later in the fall we would hand break all our corn, stack the corn in piles right on the dirt and then come back and load the corn on a wagon and take it to the Packhouse. Packhouse held all the corn to feed the animals through the winter,(mules, cows, hogs, chickens, Etc that wasn't sold. Plus it held all the dried tobacco which had to be taken off of wooden sticks and hand wraped in bundles and stacked perfectly. My father could make a good looking pallet of tobacco, every bundle exactly bundled and stacked on those pallets.
I could go on and on, I look back now and am thanful I was raised in such a manner. It sure made a man out of me at an early age.
Getting to the point though, I got carried away.
We had 2 mules that we used in the tobacco field, to plow land with, and all the other jobs you needed mule power. What I looked forward to was Sundays, I would ride Betsy all day long, from swimming hole to swimming hole. Something happened to Betsy one day and she would try to turn her head and bite me on my leg. I could not stop her doing this so I got off of her and was leading her to the barn. She came up behind me and bit me in the back, her teeth, thank goodness just did graze the skin, but I didn't take my eye off her again. I kept a close eye on her the rest of the way to the barn. She just didn't act right? The next day while I was leading her to the field she tried the same thing again. I told Daddy what was going on and he said she was just tired. He told me to unhook her and let her graze on the green grass for a while and use the other mule for that day. We used the mules to pull the drags of tobacco down the middle row in the tobacco field and a tractor to pull the drags of tobacco to the barn. But to tell you the ending of the story. My father asked a man that was trading out with us to go get Betsy and take her to the barn. As Freddie (man helping us) approached Betsy she lowered her head and ran straight towards Freddie. Betsy knocked Freddie down and was pawing him to death. My father seen what was happening and took up the swingle tree from the tobacco drag, quickly ran over and hit Betsy right between the eyes with it! My father was a big strong man and I could feel this hit myself from afar off! Well this must have knocked some sense into Betsy, she staggered a little and headed straight for the barn by herself. Freddie, on the other hand, went to the hospital for a couple of weeks. Many broken ribs, spleen damage, cuts, a concusion, Etc;. Daddy sold Betsy the following week. I felt bad for Betsy at the time, I never did care much for Freddie though. :lol: I for one missed the Sunday rides on her, she was the only one that you could ride. But I have followed a mule many, many times myself Butcher. I understand completely when you talk about how a mule operates and only too well the term muleheaded.
Well time for bed, didn't mean to get carried away.
Thanks Butcher,Talk at you later.
Oneal

 

[Oneal58]

Hi Butcher,
It warmed up above freezing today for just a short while. I noticed that the clear water that was sitting on the salts in the coffee pots have turned bronze colored and the salts had turned white? I had something to do today so it was late before I started to work on your instructions.
I poured off a little of the solution that was on top of the salts and put a piece of copper wire in the solution. I just wanted to see if there was any HN03 in this bronze colored solution.
Nothing happened, I then warmed the solution a little and could see some reaction, a very little, not much at all but the solution did have very dilute HN03 in it.
I poured off all of this solution from one pot, then added back 15ml of hot water. I also added just a little 3% Hydrogen Peroxide. Turned heat on low.
I was surprised to see that the salts dissolved very easily, quickly, without any addition of H2S04, expecting it to take a while I took my eye off solution just for a couple of minutes, when I went back the salts were dissolved,gone, without any stirring? Just when the solution warmed up a little the salts dissolved?
Then I lowered heat and added 25ml of H2S04.
Lowered heat to warm and and let solution cool, I did not bring solution to boil at any time.
I then took pot off burner, covered with a 5 gallon bucket and am letting the solution cool right now. I haven't been back out to check on the solution yet. I am going as soon as I finish here. It has been maybe 20 minutes. I have the room where solution is at 25 degree C. I am going to let solution slowly lower to 25 degree C. That's why I put the bucket over it. To slow the process of cooling down as much as possible.
I am going to wait untill solution has reached 25 degree C. or has grown 1.5-2.0 inches of salts, in bottom of pot and then I will decant solution and place in freezer.
Question 1- Why if I have a lot of salts form before solution reaches 25 degree C. Do I go ahead and decant or wait?
Question 2- If Nitric is left open to atmosphere will Nitric evaporate out of solution even if cold, just above freezing?
Question 3- Can I tell what strength of Nitric I have by watching it closely and slowly raising the temperature on solution untill it boils? If using the following method (your temperature Post) can I tell what strength of Nitric I have when the solution boils?
(USING YOUR TEMPERATURE POSTING BELOW)
If solution boils at 116 degree C. I take off heat and put in storage container, after it cools of course. That would be (50% HN03, that would be fine with me).
If solution boils at 103 degree C. (contains ony 20% Nitric) is it best to bring solution to boil or just let it steam untill solution concentrates to where it doesn't boil untill solution reaches 116 degree C.? I would want to do this without having to set up a condenser. If I rememeber your post correctly I reach Azeotropic Conditions at 68% anyway?
YOUR POST A WHILE BACK

(100% H2O) boils @100 degC density 1.00.
20% HNO3 density 1.115- boiling point 103 degC.
30% HNO3 density1.180 boiling point 107 degC.
50% HNO3 density 1.310 boiling point 116 degC.
70% HNO3 density 1.413 boiling point 121.5 degC.

I will let you know what has happened when I return.
Thanks, Oneal

 

[Oneal58]

Hi Butcher, just got back in. Nothing to report, some salts forming but just a little in the bottom. Temp. still around 96 degrees F. It needs to drop another 20-25 degrees or so before I decant. That bucket and blanket I put on the container sure slows things down as far as cooling. Salts seem to be on track right now. Checked the weather report, warming up a little tonight, low around 20 degrees. I am thinking I will just let the solution sit outside tonight instead of sitting it in the freezer. Giving solution plenty of time to react. It's already 22 outside, by the time I decant the temp should be around 20 degrees F. or close. I will just get up early and decant solution before it warms up any at all. I will let you know tomorrow how things turned out.
I feel sure I rushed things last night, didn't give things time to react as you said. I cooled the solution down as quickly as I could last night. That north wind was howling bringing this cold front in. It was blowing directly on the pots of solution taking the heat away probably as quickly as it's ever been done. I thought it was a good idea and I was doing good! I didn't even consider reaction time as you said. I should have just left everything outside all night, out of the wind under a tarp or bucket. It got down to 18 degrees F. last night and didn't get above 20 degrees untill around 9 or so this morning. The weather was almost the perfect ice box for me but I didn't realize it. I turned the freezer down as low as it would go when I put the solution in the freezer. And then just as soon as the solution hit -5 C. I jerked the pots out of there and went straight and decanted.
Oh well, you live and learn. I honestly didn't even consider reaction time at all. I just thought the temps were important to watch and that would get the job done. I think and hope I know better now? On this particular recipe, the slower the better and I didn't realize that until you told me last night.
Thanks Butcher, one day I will get there.
Oneal

 

[butcher]

Oneal,
Lets look at the homemade nitric acid, using potassium nitrate (KNO3), sulfuric acid H2SO4 and water H2O.

2KNO3 + H2SO4 --> 2HNO3 + K2SO4
(Not figuring the water)
KNO3 101g/mole (2moles 202g)
H2SO4 98g/mole
HNO3 63g/mole (2 mole 126g)
K2SO4 174g/mole
Mole’s not that little thing eating turnips in your garden,
(Molecular weight from periodical table)


This produced nitric acid HNO3 and potassium sulfate K2SO4

Both of these are soluble in water, the nitric acid is diluted by the water., but in this reaction it also helps us to get the sulfate salts out of the nitric acid we made, temperature and solubility of these salts is also used.

Solubility of the potassium sulfate salts K2SO4,
7.4g/100ml H2O @ 0deg C,
And
24g/100ml@100degC

If you did not have, as much water in the reaction above your byproduct with concentrated sulfuric acid can be potassium bisulfate KHSO4 that is a lot more soluble in water, 36g/100mlH2O@OdegC, and 122g/100mlH20@100degC, this is one of the reasons we make the nitric with more water.

The strength of the nitric can be judged by its reaction on copper.
Measuring the density of nitric acid is the best way to tell what percentage the nitric acid is.

With water density 1g/ml@20degC, boiling point 100 deg C
Nitric acid at 20 degrees centigrade
0% (water) density 1.ooog/ml, boiling point 100deg C
20% HNO3 density 1.115g/ml, boiling point 103 deg C
30% HNO3 density 1.180g/ml, boiling point 107 deg C
50% HNO3 density 1.310g/ml, boiling point 116 deg C
70% HNO3 density 1.413g/ml,, boiling point 121 deg C
90% HNO3 density 1.482g/ml, boiling point 102 deg C
98% HNO3 density 1,503g/ml, boiling point 86 deg C

(Density concentrated sulfuric acid approx 1.83g/ml)

Remember if concentrating the nitric we do not want to boil it or get it up to its boiling point for that concentration, we just want to vaporize off the water, so we heat below the boiling point for the concentration we have (evaporation of water will happen way below the boiling point of water. so with this knowledge we can heat below 100 deg centigrade and concentrate our nitric acid.

Here is a solubility table.

http://en.wikipedia.org/wiki/Solubility_table

I Hope this helps
Butcher