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rkbassin

Well-known member
Joined
Feb 3, 2011
Messages
52
HELLO IM BOILING MY MIXTURE DOWN AND ITS FORMING SOME KIND OF SLUDGE OR ALMOST LIKE A CLEAR FLAKE CRYSTALS AT THE BOTTOM WHAT IS IT AND IS THAT NORMAL THANKS
 
1st: Stop screaming at us.

2nd: if you are boiling your solution and you are seeing crystals you have most likely lost some of your material your are trying to recover.

3rd: Do some more searching on your process on the forum because you definetly don't know what you are doing.
 
Actual boiling is too high a temperature, I do not know the boiling point of aqua regia loaded with metals and it will change with concentration, but this temperature is too high, bubbles exploding at the surface of the liquid will carry off not only the gasses in that bubble but also acids and metals.

(The chlorine gasses can carry gold)

When eliminating the nitric from aqua regia you want a slow evaporation process (I AM SCREAMING AT YOU NOT BOILING), yes many times you have read to boil but that was a false term to describe the process, slow heat evaporation would be a better term to use, a steam bath (pot of boiling water with beaker suspended over steam bath would prevent loss as that will not let your aqua regia boil and would maintain the slow evaporation temperature needed,
Keep your solution under the boiling point steam gases escaping is good, boiling bubbles is bad.
The steam bath is not necessary if you keep the temperature low enough.

The boiling point of pure acids can change with concentration for example nitric acid:
20% HNO3 boiling point 103 deg C,
30% HNO3 boiling point 107 deg C,
50 % HNO3 boiling point 116 deg C,
70% HNO3 boiling point 121 deg C, (azeotropic point of nitric acid and water)

The boiling point of Hydrochloric acid (HCl):
10% HCl boiling point 103 deg C,
20% HCl boiling point 110 deg C,
38% HCl boiling point 48 deg C,

Water boiling point 100 deg C.
Mixtures of these acids and metals can drastically change these boiling points of pure acids or water.


When you first start evaporation more water will evaporate off than acid gases as the acid concentrates (to azeotrope) then more NOx gas will vapor off these are NO, NO2 and other forms of nitrogen gas from the nitrate in solution,

This part is important when the nitric acid in solution concentrates to an azeotropic mix you will see small bubbles even at the same evaporation temperature, I lower the temperature of solution at this point, because the nitic will now be concentrated and it will FOAM OVER if temperature is too high as nitric is trying to come out almost all at once as NOx gases, these foam over carry many of your values.

After most of nitric has gases off then HCL will vapor off.

Note these gasses are not pure separation but portions of each in the mixture, just more of one gas than the others as each have a differing boiling point.

The water and acids can vapor out of solutions without reaching their boiling point temperature.

When you concentrate the aqua regia you do not want to form salts, add some hydrochloric acid before that point.

If you are using poormans aqua regia you may form salts from other byproducts than when using purer acids,
If using HCl/sodium hypochorite it will also form salts easily (NaCl, table salt and sodium chlorate), both easily dissolved in water.

When you add an acid to a metal you make a salt of that metal, these salts can be soluble in the acidic solution or in water, or even insoluble in them, depending on the acid and the metal involved.

Salts if white can be several different things, NaCl table salt is water soluble, AgCl silver chloride is not water soluble even in hot water, PbCl lead chloride is not water soluble in cold water but is soluble in boiling hot water.
 
YES BARREN RELMS I DONT KNOW WHAT IM DOING THATS WHY IM HERE TRYING TO LEARN IS THAT LOUD ENOUGH FOR YOU
 
now butcher your a great help and i didnt really boil it bad choice of words i let it evaporate like you said and what im getting some kind of salt like your saying its a clear salt but when i mix the solution it desolves again i started by adding sulfuric like hoke says then i oiled it no evaporated it twice with adding hcl at the end of evaporation so is this correct so far now ive added 4 times the water and let it sit over nite ive got some sludge and crystal flakes in the bottom anybody care to help please thank you oh and sorry for the yelling just didnt know im a greenhorn
 
I have heard enough yelling (all CAPS), as well as the arguing about it.

Keep it civil gentlemen.
 
rkbassin said:
YES BARREN RELMS I DONT KNOW WHAT IM DOING THATS WHY IM HERE TRYING TO LEARN IS THAT LOUD ENOUGH FOR YOU

I din't get smart with you. I was giving you a point blank answer to what you needed to possibly do. So please calm your attitude and take the chip off your shoulder.
 
mr barrenrealms me and you could but heads forever im trying to learn something and your making it hard to do no matter have a blessed day and maybe we can compare notes one day thanks for the help
 
rkbassin said:
mr barrenrealms me and you could but heads forever im trying to learn something and your making it hard to do no matter have a blessed day and maybe we can compare notes one day thanks for the help

You can ask anyone on the forum, I am here to help you as much as you need it unless there is an attitude with it. If I took you wrong I am sorry. So if you need help just ask but you have to be willing to accpet criticism. It comes with the territory.
 
rkbassin said:
mr barrenrealms me and you could but heads forever im trying to learn something and your making it hard to do
Barren Realms can be your best friend and asset on this forum,you may want to consider letting him help you when he tries to.He is on the forum almost 24 hours a day helping others,and he is very knowledgable of what you are going through.You have been on the forum for 3 weeks now and have gotten upset on several occasions now.You are allowed to get frusterated even pissed off,but do not post it on the forum.Too many members,myself included,have found themselves on the wrong end of an upset moderator,I do not want that for you.If you find yourself getting upset over something, just take a breath and maybe a little break and come back to it.
For the time being,until you cut your teeth,try to be a little more understanding.I think you can do well,if you stay here and relax.Ok?
 
rkbassin said:
mr barrenrealms me and you could but heads forever im trying to learn something and your making it hard to do no matter have a blessed day and maybe we can compare notes one day thanks for the help

Try to start using . , ? !
If you dont use them why bother with space between words?
maybeitcanbeeasierforyoutotypelikethis - as it is the same like reading your thousand words one sentence. Please understand that this is international place with people from all over world. It is very hard to comprehend one homogeneous block of text even for english speakers not to mention people from other countries.

Your questions will be readable and understandable. They may get answered faster.
 
rkbassin said:
my bad sorry folks just getting frustrated and needing help
I was asked to consider editing/deleting my post so as not to open any old wounds, & I certainly don't want that to happen.
So there you go - you're free & clear!
good luck
 
Thanks butcher...many points in ur explanations...
Just known now...chlorine gas can carry the gold..


butcher said:
Actual boiling is too high a temperature, I do not know the boiling point of aqua regia loaded with metals and it will change with concentration, but this temperature is too high, bubbles exploding at the surface of the liquid will carry off not only the gasses in that bubble but also acids and metals.

(The chlorine gasses can carry gold)

When eliminating the nitric from aqua regia you want a slow evaporation process (I AM SCREAMING AT YOU NOT BOILING), yes many times you have read to boil but that was a false term to describe the process, slow heat evaporation would be a better term to use, a steam bath (pot of boiling water with beaker suspended over steam bath would prevent loss as that will not let your aqua regia boil and would maintain the slow evaporation temperature needed,
Keep your solution under the boiling point steam gases escaping is good, boiling bubbles is bad.
The steam bath is not necessary if you keep the temperature low enough.

The boiling point of pure acids can change with concentration for example nitric acid:
20% HNO3 boiling point 103 deg C,
30% HNO3 boiling point 107 deg C,
50 % HNO3 boiling point 116 deg C,
70% HNO3 boiling point 121 deg C, (azeotropic point of nitric acid and water)

The boiling point of Hydrochloric acid (HCl):
10% HCl boiling point 103 deg C,
20% HCl boiling point 110 deg C,
38% HCl boiling point 48 deg C,

Water boiling point 100 deg C.
Mixtures of these acids and metals can drastically change these boiling points of pure acids or water.


When you first start evaporation more water will evaporate off than acid gases as the acid concentrates (to azeotrope) then more NOx gas will vapor off these are NO, NO2 and other forms of nitrogen gas from the nitrate in solution,

This part is important when the nitric acid in solution concentrates to an azeotropic mix you will see small bubbles even at the same evaporation temperature, I lower the temperature of solution at this point, because the nitic will now be concentrated and it will FOAM OVER if temperature is too high as nitric is trying to come out almost all at once as NOx gases, these foam over carry many of your values.

After most of nitric has gases off then HCL will vapor off.

Note these gasses are not pure separation but portions of each in the mixture, just more of one gas than the others as each have a differing boiling point.

The water and acids can vapor out of solutions without reaching their boiling point temperature.

When you concentrate the aqua regia you do not want to form salts, add some hydrochloric acid before that point.

If you are using poormans aqua regia you may form salts from other byproducts than when using purer acids,
If using HCl/sodium hypochorite it will also form salts easily (NaCl, table salt and sodium chlorate), both easily dissolved in water.

When you add an acid to a metal you make a salt of that metal, these salts can be soluble in the acidic solution or in water, or even insoluble in them, depending on the acid and the metal involved.

Salts if white can be several different things, NaCl table salt is water soluble, AgCl silver chloride is not water soluble even in hot water, PbCl lead chloride is not water soluble in cold water but is soluble in boiling hot water.
 

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