nbk2000
April 10th, 2002, 07:23 AM
<BODY BGCOLOR="#FFFFCC" TEXT="#000000" ALINK="#33FF33" VLINK="#0099FF" LINK="#FF0000">
This is part of an article on nitric acid production that I'm writing for my PDF. What I need is peer review as to anything that has been left out, and suggestions for things to include.
This is the part dealing with the distillation of nitric. I'm also including the acid/nitrate decanting method, solvent concentration, catalytic conversion of ammonia, and some others.
Articel begins below.
<HR>
<CENTER><H1><FONT FACE="COMIC SANS MS" >NITRIC ACID</FONT></H1></CENTER>
Nitric acid is THE most important single chemical for explosives manufacture. Without it, virtually every high explosive in existance would be either impossible, or extremely expensive, to make.
And because nitric acid is of such great importance, it's either tightly regulated, or extremely expensive, to buy. This is why it is of vital importance that you know how to make it yourself.
<HR>
<H3><FONT FACE="Comic Sans MS">Nitrates</FONT></H3>
Regardless of which method you use, you'll need a supply of nitrate to make nitric acid from. Common chemical fertilizers are the source of the nitrate radical (NO3) needed to make nitric acid.
The nitrates that can be used are listed in order of preference:
<UL TYPE="DISC">(Chemical Name / CAS # / Molecular Weight)
Potassium Nitrate / 7757-79-1 / 101</LI>
Sodium Nitrate / 10124-37-5 / 85</LI>
Calcium Nitrate / 10124-37-5 / 164</LI>
Ammonium Nitrate / 10124-37-5 / 80</LI>
[/list]
It may be possible to use other nitrates, but they're likely to be difficult to obtain, or too expensive for making useful quantities.
Most agricultural grade nitrates come in the form of "prills". These are little BB sized pellets that need to be treated before they can be used.
You'll first dissolve the prills in the minimum amount of boiling water possible. This will remove the coating that some fertilizers have, and save you the hassle of grinding them to powder.
Once the prills are dissolved, filter while hot, and allow to cool while covered. The solution will precipitate out crystals of pure nitrate. The longer it takes to cool down, the larger and purer the crystals.
Filter the crystals and wash with a small amount of cold acetone or 99% isopropyl alcohol to remove the last traces of contaminants.
After letting the crystals dry out, you now put them in an oven to remove the water of crystallization. This is the water that is molecular bound to the nitrate.
To remove it, you place the nitrate is glass or ceramic casserole dish so that it's spread out in a thin layer.
Turn the oven on to 250°F (120°C) and occasionally stir it till it no longer steams and falls apart into a fine powder.
Remove from the heat and immediately place it in pre-heated jar or can to keep it dry.
<H3><FONT FACE="Comic Sans MS">Sulfuric Acid</FONT></H3>
In order to make nitric acid with nitrates, you'll also need sulfuric acid. This is most commonly available as battery acid or drain cleaner.
The battery acid is approximately 30% concentration, and is too weak to be used as is. You'll have to concentrate it by removing the water. The simplest way to do this is to boil it off.
You'll be wanting to use fresh battery acid from the container. Don't use battery acid that's been in a battery if you have any choice as there's bound to be lots of contaminates in it.
Take a glass or ceramic pot, pan, jar, flask, etc, and fill it a quarter ways full of your dilute acid. Have the boiling container sitting in a shallow pan filled with sand to prevent cracking.
Using an electric hot plate or burner, gradually heat the acid till dense white fumes come off.
Do this outdoors as the fumes are HIGHLY DANGEROUS! Stay upwind at all times.
Once the fumes are coming off, turn off the heat and immediately cover the container with a glass lid or plug. Don't use rubber or cork as it will be destroyed.
Once the acid has cooled off, pour it into a dark glass soda bottle which works well. You can also use polyethylene bottles which are safer from breakage.
<H3><FONT FACE="Comic Sans MS">Distillation</FONT></H3>
The most frequently cited method of preparing nitric acid in a laboratory or field enviroment is heating of a nitrate with concentrated sulfuric acid. So we'll start with this method first.
The reaction that takes places between an alkaline nitrate (R = alkali metal ion) and sulfuric acid is as follows.
<H3><CENTER>2RNO<sub>3</sub> + H<sub>2</sub>SO<sub>4</sub> = 2HNO<sub>3</sub> + R<sub>2</sub>SO<sub>4</sub></CENTER></H3>
When you react the alkali nitrate with sulfuric acid, it decomposes in nitric acid and alkali sulphate.
To determine the proper amount of nitrate to use with any given amount of acid, you divide the weight of the acid by 98. Multiply the results by twice the molecular weight of the nitrate that you are using.
For instance, you have 98 grams of sulfuric acid. You also have potassium nitrate. Potassium nitrate has a molecular weight of 101. So, double 101 = 202. Thus, you'd use 202 grams of potassium nitrate with the 98 grams of sulfuric acid.
Though, in actual practice, you'd want to use a slight excess of acid to ensure a complete reaction.
Ideally, when distilling the acid, you'd be using laboratory grade glassware, but even 2 beer bottles could be used in dire circumstances.
To start, place the concentrated sulfuric acid in the container that's going to be heated. Next, add with swirling or stirring with a glass/plastic rod, the dry powdered nitrate. If there's any visible fuming, STOP! Get upwind and wait a few minutes for it to stop. Then continue until all the nitrate is added and well wetted by the acid. There should be no clumps.
If you have lab glass, you already know what to do for a distillation. If you're using a beer bottle still, place the bottle with the nitrate/acid paste in a larger can with a layer of sand on the bottom. Fill the remaining space with more sand the filled, and slide the cut out lid with a hole for the bottles neck over the can. Wire the lid in place.
(The purpose of the sand can is to prevent the glass bottle from shattering from uneven heating.)
Now lay the can on it's side. If you've measured it correctly, then no paste will come out the neck. If any does, catch it in a bowl or such and save it for your next batch.
Now line up the second bottle exactly parrallel to the first one, and seal them together using teflon tape (if possible) or damp cotton cloth (bandages work). The second bottle is the condenser that the nitric acid will be collected in. If using tape, poke a very small hole in the gap between the two bottles to provide pressure relief so the tape doesn't rupture.
Keep this second bottle well cooled. You can do this by wrapping it in a small towel and having a constant stream of cold water from a hose flowing over it. Or wrap it in ice. However you do it, keep it as cold as possible.
Proceed to gently heat the bottle using a gas or charcoal fire. You don't want to overheat the paste which would cause some to carry over into the receiving bottle.
You'll know the reaction is done when no more fumes are seen to be in the bottles.
At this point, remove the heat and allow the assembly to cool down while keeping the receiver cool.
Carefully seperate the two bottles, being careful to wear acid resistant gloves and staying upwind of the assembly.
This is part of an article on nitric acid production that I'm writing for my PDF. What I need is peer review as to anything that has been left out, and suggestions for things to include.
This is the part dealing with the distillation of nitric. I'm also including the acid/nitrate decanting method, solvent concentration, catalytic conversion of ammonia, and some others.
Articel begins below.
<HR>
<CENTER><H1><FONT FACE="COMIC SANS MS" >NITRIC ACID</FONT></H1></CENTER>
Nitric acid is THE most important single chemical for explosives manufacture. Without it, virtually every high explosive in existance would be either impossible, or extremely expensive, to make.
And because nitric acid is of such great importance, it's either tightly regulated, or extremely expensive, to buy. This is why it is of vital importance that you know how to make it yourself.
<HR>
<H3><FONT FACE="Comic Sans MS">Nitrates</FONT></H3>
Regardless of which method you use, you'll need a supply of nitrate to make nitric acid from. Common chemical fertilizers are the source of the nitrate radical (NO3) needed to make nitric acid.
The nitrates that can be used are listed in order of preference:
<UL TYPE="DISC">(Chemical Name / CAS # / Molecular Weight)
Potassium Nitrate / 7757-79-1 / 101</LI>
Sodium Nitrate / 10124-37-5 / 85</LI>
Calcium Nitrate / 10124-37-5 / 164</LI>
Ammonium Nitrate / 10124-37-5 / 80</LI>
[/list]
It may be possible to use other nitrates, but they're likely to be difficult to obtain, or too expensive for making useful quantities.
Most agricultural grade nitrates come in the form of "prills". These are little BB sized pellets that need to be treated before they can be used.
You'll first dissolve the prills in the minimum amount of boiling water possible. This will remove the coating that some fertilizers have, and save you the hassle of grinding them to powder.
Once the prills are dissolved, filter while hot, and allow to cool while covered. The solution will precipitate out crystals of pure nitrate. The longer it takes to cool down, the larger and purer the crystals.
Filter the crystals and wash with a small amount of cold acetone or 99% isopropyl alcohol to remove the last traces of contaminants.
After letting the crystals dry out, you now put them in an oven to remove the water of crystallization. This is the water that is molecular bound to the nitrate.
To remove it, you place the nitrate is glass or ceramic casserole dish so that it's spread out in a thin layer.
Turn the oven on to 250°F (120°C) and occasionally stir it till it no longer steams and falls apart into a fine powder.
Remove from the heat and immediately place it in pre-heated jar or can to keep it dry.
<H3><FONT FACE="Comic Sans MS">Sulfuric Acid</FONT></H3>
In order to make nitric acid with nitrates, you'll also need sulfuric acid. This is most commonly available as battery acid or drain cleaner.
The battery acid is approximately 30% concentration, and is too weak to be used as is. You'll have to concentrate it by removing the water. The simplest way to do this is to boil it off.
You'll be wanting to use fresh battery acid from the container. Don't use battery acid that's been in a battery if you have any choice as there's bound to be lots of contaminates in it.
Take a glass or ceramic pot, pan, jar, flask, etc, and fill it a quarter ways full of your dilute acid. Have the boiling container sitting in a shallow pan filled with sand to prevent cracking.
Using an electric hot plate or burner, gradually heat the acid till dense white fumes come off.
Do this outdoors as the fumes are HIGHLY DANGEROUS! Stay upwind at all times.
Once the fumes are coming off, turn off the heat and immediately cover the container with a glass lid or plug. Don't use rubber or cork as it will be destroyed.
Once the acid has cooled off, pour it into a dark glass soda bottle which works well. You can also use polyethylene bottles which are safer from breakage.
<H3><FONT FACE="Comic Sans MS">Distillation</FONT></H3>
The most frequently cited method of preparing nitric acid in a laboratory or field enviroment is heating of a nitrate with concentrated sulfuric acid. So we'll start with this method first.
The reaction that takes places between an alkaline nitrate (R = alkali metal ion) and sulfuric acid is as follows.
<H3><CENTER>2RNO<sub>3</sub> + H<sub>2</sub>SO<sub>4</sub> = 2HNO<sub>3</sub> + R<sub>2</sub>SO<sub>4</sub></CENTER></H3>
When you react the alkali nitrate with sulfuric acid, it decomposes in nitric acid and alkali sulphate.
To determine the proper amount of nitrate to use with any given amount of acid, you divide the weight of the acid by 98. Multiply the results by twice the molecular weight of the nitrate that you are using.
For instance, you have 98 grams of sulfuric acid. You also have potassium nitrate. Potassium nitrate has a molecular weight of 101. So, double 101 = 202. Thus, you'd use 202 grams of potassium nitrate with the 98 grams of sulfuric acid.
Though, in actual practice, you'd want to use a slight excess of acid to ensure a complete reaction.
Ideally, when distilling the acid, you'd be using laboratory grade glassware, but even 2 beer bottles could be used in dire circumstances.
To start, place the concentrated sulfuric acid in the container that's going to be heated. Next, add with swirling or stirring with a glass/plastic rod, the dry powdered nitrate. If there's any visible fuming, STOP! Get upwind and wait a few minutes for it to stop. Then continue until all the nitrate is added and well wetted by the acid. There should be no clumps.
If you have lab glass, you already know what to do for a distillation. If you're using a beer bottle still, place the bottle with the nitrate/acid paste in a larger can with a layer of sand on the bottom. Fill the remaining space with more sand the filled, and slide the cut out lid with a hole for the bottles neck over the can. Wire the lid in place.
(The purpose of the sand can is to prevent the glass bottle from shattering from uneven heating.)
Now lay the can on it's side. If you've measured it correctly, then no paste will come out the neck. If any does, catch it in a bowl or such and save it for your next batch.
Now line up the second bottle exactly parrallel to the first one, and seal them together using teflon tape (if possible) or damp cotton cloth (bandages work). The second bottle is the condenser that the nitric acid will be collected in. If using tape, poke a very small hole in the gap between the two bottles to provide pressure relief so the tape doesn't rupture.
Keep this second bottle well cooled. You can do this by wrapping it in a small towel and having a constant stream of cold water from a hose flowing over it. Or wrap it in ice. However you do it, keep it as cold as possible.
Proceed to gently heat the bottle using a gas or charcoal fire. You don't want to overheat the paste which would cause some to carry over into the receiving bottle.
You'll know the reaction is done when no more fumes are seen to be in the bottles.
At this point, remove the heat and allow the assembly to cool down while keeping the receiver cool.
Carefully seperate the two bottles, being careful to wear acid resistant gloves and staying upwind of the assembly.