Poor man's nitric vs nitric cost _poormansnitric_

[eaglekeeper]

I have not tried it so don't take this for sure.
How about mixing the Sulfuric and water and then adding the Calcium Nitrate under heavy stirring?
Would that be a possibility?

It's always worth a try. Maybe I'll try a small batch tomorrow, my nitric bottle needs topped off anyway.

 

[Yggdrasil]

It's always worth a try. Maybe I'll try a small batch tomorrow, my nitric bottle needs topped off anyway.

Let us know how it works.

 

[shadybear]

So if you dissolve calcium nitrate into distilled water
Then add sulfuric acid the calcium will drop out.
How long does it take to settle so the nitric solution can be siphoned off

 

[icejj]

Can anyone comment on the percentage/strength level of the nitric after performing lazersteve's cold nitric method and what was the nitrate percentage of the fertilizer that was used to get that percentage of nitric? I've seen some say 35-40%, and 50% for lazersteve's cold recipe, so I'm trying to figure out how much water that would be needed to dilute the resulting nitric to use it on gold filled material... I'm also realizing that the nitrate percentage of the fertilizer used would make a big difference...? The nitrate percentage of the different types of fertilizers that I've been looking at purchasing have ranged from 10%-30%, so I'm trying to make sure that I'm doing everything correctly.

 

[Shark]

Buried on the forum are several posts giving exact numbers. Some may go back over 10 years. I have played with making it almost that long myself.

 

[lazersteve]

Can anyone comment on the percentage/strength level of the nitric after performing lazersteve's cold nitric method and what was the nitrate percentage of the fertilizer that was used to get that percentage of nitric? I've seen some say 35-40%, and 50% for lazersteve's cold recipe, so I'm trying to figure out how much water that would be needed to dilute the resulting nitric to use it on gold filled material... I'm also realizing that the nitrate percentage of the fertilizer used would make a big difference...? The nitrate percentage of the different types of fertilizers that I've been looking at purchasing have ranged from 10%-30%, so I'm trying to make sure that I'm doing everything correctly.

My typical cold recipe using pure sodium nitrate is 40-45% if your starting reagents are dry (96% H2SO4 and free flowing nitrate prills). Exact weights (no volume measurements) for liquids and solids. Full 24 freezer (-5C minimum) cycle.

As for how much nitrate is required I rely on the very simple mole calculation to determine that. Sodium Nitrate has 1 mole of nitrate per 85g of clean, dry, pure, salt. Therefore 1 mole of sodium nitrate (85g) dissolves 0.375 mole ( 23.8g ) of copper assuming 100% conversion and zero losses when making your nitric.

From wiki:
For example, copper reacts with dilute nitric acid at ambient temperatures with a 3:8 stoichiometry:

3 Cu + 8 HNO3 → 3 Cu(NO3)2 + 2 NO + 4 H2O

The easiest method for determining the exact concentration is a simple density test using a 10ml plastic syringe and a scale accurate to 0.01g. There are plenty of charts online that convert nitric acid density to concentration. This method is within +/-5% of the correct percentage assuming you followed the cold nitric acid recipe to a T. I have outlined this density test procedure elsewhere (in my posts on copper nitrate) on the forum.

Steve

 

[icejj]

My typical cold recipe using pure sodium nitrate is 40-45% if your starting reagents are dry (96% H2SO4 and free flowing nitrate prills). Exact weights (no volume measurements) for liquids and solids. Full 24 freezer (-5C minimum) cycle.

As for how much nitrate is required I rely on the very simple mole calculation to determine that. Sodium Nitrate has 1 mole of nitrate per 85g of clean, dry, pure, salt. Therefore 1 mole of sodium nitrate (85g) dissolves 0.375 mole ( 23.8g ) of copper assuming 100% conversion and zero losses when making your nitric.

From wiki:
For example, copper reacts with dilute nitric acid at ambient temperatures with a 3:8 stoichiometry:

3 Cu + 8 HNO3 → 3 Cu(NO3)2 + 2 NO + 4 H2O

The easiest method for determining the exact concentration is a simple density test using a 10ml plastic syringe and a scale accurate to 0.01g. There are plenty of charts online that convert nitric acid density to concentration. This method is within +/-5% of the correct percentage assuming you followed the cold nitric acid recipe to a T. I have outlined this density test procedure elsewhere (in my posts on copper nitrate) on the forum.

Steve

Thanks for the info. I'm going to read more into it based on the information provided.

 

[NanoCat]

This is a really good YouTube of how to make clean Nitric Acid

 

[icejj]

This is a really good YouTube of how to make clean Nitric Acid

Thank you for this.

 

[James Ball]

Calcium will make a better poormans nitric, where the sulfate can be removed, than it does used as poormans AR.

If you make nitric with calcium nitrate, the gypsum left over will settle very compactly given time, such that the nitric can be siphoned off, (even poured at times) although the container maybe be destroyed trying to remove the salts afterwards. It will also produce a better volume per pound than sodium nitrate.

With either sodium, potassium or calcium, some extra nitric can be salvaged from the salts using a vacuum funnel and allowing time for it to work slowly. To much vacuum and it will self boil potentially ruining your nitric.

Making nitric early on was a good way to practice some chemistry when I didn’t have material to work with. I wish I had more real chemistry schooling before trying to refine, it would have been a big asset in understanding what was going on with the processes as I tried them.

I am wondering if one was to use an empty distilled water container (plastic) for the Ca(NO3)2 + H2SO4 reaction yielding HNO3 and CaSO4 then one could throw away the plastic container with gypsum. I think the plastic will stand up to the acids. Unless I hear some negatives (someone may have tried this already) I will give this a shot.

 

[James Ball]

I am wondering if one was to use an empty distilled water container (plastic) for the Ca(NO3)2 + H2SO4 reaction yielding HNO3 and CaSO4 then one could throw away the plastic container with gypsum. I think the plastic will stand up to the acids. Unless I hear some negatives (someone may have tried this already) I will give this a shot

Calcium nitrate is significantly more expensive than sodium nitrate. I think I will go with NaNO3 for now.......

 

[Shark]

Adding the sulfuric will generate heat. Quite a bit at times and may be enough to cause the plastic to fail.

 

[James Ball]

Can anyone comment on the percentage/strength level of the nitric after performing lazersteve's cold nitric method and what was the nitrate percentage of the fertilizer that was used to get that percentage of nitric? I've seen some say 35-40%, and 50% for lazersteve's cold recipe, so I'm trying to figure out how much water that would be needed to dilute the resulting nitric to use it on gold filled material... I'm also realizing that the nitrate percentage of the fertilizer used would make a big difference...? The nitrate percentage of the different types of fertilizers that I've been looking at purchasing have ranged from 10%-30%, so I'm trying to make sure that I'm doing everything correctly.

I am always skeptical when a procedure goes above expectations. I tried the cold procedure to make HNO3. I used Spectracide Stump Remover which is reported to be 100% KNO3. I used the entire bottle. I made a ton of K2SO4 as expected and my total volume was less than predicted but my density was 1.38 g/mL which is about 65% at 70 F. Too good to be true??? It reacts with copper but is yellow and somewhat cloudy (pottasium sulfate?). My plan is to make more using Duda NaNO3 from Amazon and use all of this to digest some sterling silver.

 

[kurtak]

Duda NaNO3 from Amazon and use all of this to digest some sterling silver.

Home made nitric (nitrate salt + sulfuric) is not a good choice for silver

That is because most - if not all - nitrate salts have at least a trace of chloride in them (even if the label "claims" it is 100%) which results in a trace of HCl in the nitric which then results in the formation of at least some AgCl when processing the silver

This has been discussed (& pointed out) here on the forum before when discussing home made nitric

So if you are going to use it for silver it should first be distilled after the "cold" making of it

Kurt

 

[4metals]

Let me start by saying I have never had to make nitric for refining, I did successfully make nitric acid just to see how effective it is because so many members here tried it or have no other cost effective choice. But, as Kurt pointed out for Silver work the chloride is an issue. I distilled it and ended up with a stronger product and it was chloride free. But, in addition to needing a distillation apparatus, it was also a royal pain in the a**!

But I was thinking, and I remember posting years back about how assayers of old used a trick to remove chlorides from water for use in the assay process. They added a small amount of AgNO₃ to the water which dropped the Silver as Silver Chloride and consumed the chloride in the process. I have a client who does this on a relatively large scale to dechlorinate his tap water to use in his silver cells and it works well. Once a year he empties about 2" of Silver Chloride out of the 55 gallon drums he uses to convert back to Silver metal. He makes about one drum of chlorine free water a week.

I was thinking, if one wanted to use home made nitric for Silver cells, and avoid the complicated step of distillation, adding a small amount of Silver metal powder to the homemade nitric should accomplish the same thing. You will quickly see the highly visible Silver Chloride form and settle, and if you are using this nitric for a Silver cell, a little Silver won't be any trouble. Worth a try with a small sample of your homemade nitric acid because it could save you some serious expense, especially when refining a metal worth $22 an ounce vs. a metal worth $2000 an ounce.

I wouldn't do this on ice cold nitric just out of the freezer, but in a slightly warmed solution, and well mixed with a stirrer to get the finely divided Silver metal up and moving in the solution. It should not take a lot of Silver metal because the chlorine content is probably quite low but seeing how quickly Silver nitrate will convert over to the highly visible Silver Chloride, it has a built in indicator to tell you when it's done.

Worth a try, and if anyone does try it, please report back your results.

 

[Darkthirty]

Let me start by saying I have never had to make nitric for refining, I did successfully make nitric acid just to see how effective it is because so many members here tried it or have no other cost effective choice. But, as Kurt pointed out for Silver work the chloride is an issue. I distilled it and ended up with a stronger product and it was chloride free. But, in addition to needing a distillation apparatus, it was also a royal pain in the a**!

But I was thinking, and I remember posting years back about how assayers of old used a trick to remove chlorides from water for use in the assay process. They added a small amount of AgNO₃ to the water which dropped the Silver as Silver Chloride and consumed the chloride in the process. I have a client who does this on a relatively large scale to dechlorinate his tap water to use in his silver cells and it works well. Once a year he empties about 2" of Silver Chloride out of the 55 gallon drums he uses to convert back to Silver metal. He makes about one drum of chlorine free water a week.

I was thinking, if one wanted to use home made nitric for Silver cells, and avoid the complicated step of distillation, adding a small amount of Silver metal powder to the homemade nitric should accomplish the same thing. You will quickly see the highly visible Silver Chloride form and settle, and if you are using this nitric for a Silver cell, a little Silver won't be any trouble. Worth a try with a small sample of your homemade nitric acid because it could save you some serious expense, especially when refining a metal worth $22 an ounce vs. a metal worth $2000 an ounce.

I wouldn't do this on ice cold nitric just out of the freezer, but in a slightly warmed solution, and well mixed with a stirrer to get the finely divided Silver metal up and moving in the solution. It should not take a lot of Silver metal because the chlorine content is probably quite low but seeing how quickly Silver nitrate will convert over to the highly visible Silver Chloride, it has a built in indicator to tell you when it's done.

Worth a try, and if anyone does try it, please report back your results.

I've used ascorbic acid (vitamin C) to remove chlorine from drinking water for years. Not sure of how efficient it is, or if it would cause contamination for refining.

 

[James Ball]

Home made nitric (nitrate salt + sulfuric) is not a good choice for silver

That is because most - if not all - nitrate salts have at least a trace of chloride in them (even if the label "claims" it is 100%) which results in a trace of HCl in the nitric which then results in the formation of at least some AgCl when processing the silver

This has been discussed (& pointed out) here on the forum before when discussing home made nitric

So if you are going to use it for silver it should first be distilled after the "cold" making of it

Kurt

Thank you Kurt. I had not read about the problems of using homemade nitric acid in silver refining. AgCl formation is a definate problem. I will search for it on the forum and read the discussion. I will do some more reading and then I may respond with some ideas, but these ideas have likely been adressed already.

 

[James Ball]

Let me start by saying I have never had to make nitric for refining, I did successfully make nitric acid just to see how effective it is because so many members here tried it or have no other cost effective choice. But, as Kurt pointed out for Silver work the chloride is an issue. I distilled it and ended up with a stronger product and it was chloride free. But, in addition to needing a distillation apparatus, it was also a royal pain in the a**!

But I was thinking, and I remember posting years back about how assayers of old used a trick to remove chlorides from water for use in the assay process. They added a small amount of AgNO₃ to the water which dropped the Silver as Silver Chloride and consumed the chloride in the process. I have a client who does this on a relatively large scale to dechlorinate his tap water to use in his silver cells and it works well. Once a year he empties about 2" of Silver Chloride out of the 55 gallon drums he uses to convert back to Silver metal. He makes about one drum of chlorine free water a week.

I was thinking, if one wanted to use home made nitric for Silver cells, and avoid the complicated step of distillation, adding a small amount of Silver metal powder to the homemade nitric should accomplish the same thing. You will quickly see the highly visible Silver Chloride form and settle, and if you are using this nitric for a Silver cell, a little Silver won't be any trouble. Worth a try with a small sample of your homemade nitric acid because it could save you some serious expense, especially when refining a metal worth $22 an ounce vs. a metal worth $2000 an ounce.

I wouldn't do this on ice cold nitric just out of the freezer, but in a slightly warmed solution, and well mixed with a stirrer to get the finely divided Silver metal up and moving in the solution. It should not take a lot of Silver metal because the chlorine content is probably quite low but seeing how quickly Silver nitrate will convert over to the highly visible Silver Chloride, it has a built in indicator to tell you when it's done.

Worth a try, and if anyone does try it, please report back your results.

I like your idea. Typically I would filter out the AgNO3 after dissolution in nitric acid. Any AgCl would be filtered out prior to copper cementation. I could save my filters and attempt to recover Ag from AgCl using NaOH and a poly aldehyde like sugar or glucose (reminds me of Tollen's reagent in organic chemistry). I suspect this has been discussed and will look for it on the forum.

 

[billgold]

As far as I have been able to find out with a fairly short search, none of the nitrate stump removers/decomposers are very close to being pure. They seem to contain up to about 5% of non-nitrate impurities - and the composition can vary a bit from manufacturer batch to batch.

But given the lack of purity of some of the other bulk chemicals we use, they may not be an issue.

 

[James Ball]

Thank you Kurt. I had not read about the problems of using homemade nitric acid in silver refining. AgCl formation is a definate problem. I will search for it on the forum and read the discussion. I will do some more reading and then I may respond with some ideas, but these ideas have likely been adressed already.

I have searched the forum for any discussuon on the use of homemade nitric acid in silver refining. I would appreciate any links to this discussion

I am always skeptical when a procedure goes above expectations. I tried the cold procedure to make HNO3. I used Spectracide Stump Remover which is reported to be 100% KNO3. I used the entire bottle. I made a ton of K2SO4 as expected and my total volume was less than predicted but my density was 1.38 g/mL which is about 65% at 70 F. Too good to be true??? It reacts with copper but is yellow and somewhat cloudy (pottasium sulfate?). My plan is to make more using Duda NaNO3 from Amazon and use all of this to digest some sterling silver.

I filtered this solution through a scintered glass funnel after letting any ppt settle over a few days. This solution had a density of 1.34 at 70 F or about 55% nitric acid. I had a fair amount of sulfate that ppt. My nitiric acid from Duda Diesel NaNO3 worked real well too. I am going to have to try refining a kg of sterling silver and see how the filtration goes, If AgCl or Ag2SO4 is a problem It could show up in the filtration. I will keep the forum posted on my results.