Evaporation versus boiling

Gold Refining Forum

Help Support Gold Refining Forum:

This site may earn a commission from merchant affiliate links, including eBay, Amazon, and others.
I use distillation for much of my work (not all), I also capture the red fumes as much as possible when dissolving metals in nitric acid, the nice thing as garage chemist stated is the temperature can be raised to boiling (I keep mine forming small bubbles not large bumping bubbles), and as long as you carefully watch for foam over or carry over, the metals stay in the heated reaction vessel (color of condensed liquids are also a clue you are getting carry-over), the fumes if condensed in very little water and H202 for NOx gas into the receiver bottle the acid can be reused as dilute HNO3, this saves me from wasting my acid, and from dumping NOx gases into the atmosphere that the EPA has tried so hard to eliminate (which creates acid rains), I am no tree hugger but I do care for our earth and the air we breath, even the HCl or aqua regia can be distilled (bubbled into water to make a weak solution, which can be reused with heating its action on metals and heat concentrating solution, it works well.

The small amount of gold added to aqua regia to use up excess nitric is nice when you do not want to evaporate just a little heat and let it react, very little fumes are released (normal amount for gold being dissolved), it is quick and easy, and you get your gold back.

What works for me also, is to calculate how much acid I need, calculating just under this amount needed to dissolve the gold, and measure my solutions,
(I can even use the 4 HCl : 1 HNO3 ratio if wanted, although normally just add HCL then adding in small additions), add a small portion of solution to metals with heating, add more as needed, the goal is to leave a small amount of metal un-dissolved with strong heat, and plenty reaction time (this portion of saturated solution is decanted from remaining metal), (the small amount of metal left is then dissolved, usually with just covered in HCl and the drops of nitric added as needed, and with heating (heat is an important part as more metal is reacted with acid with heat, and these hot solutions hold more metal salts, even if I over shoot on this last bit of metal I am dissolving, and use a bit more acid than necessary it is simpler to remove any excess nitric if I made a mistake.

I agree 100% with garage chemist, but I also think if we tell someone to distill their solution then we can explain that the solution can boil, actually when I distill I normally do not want large bubbles popping and splashing, but just want my temperature where lots of little tiny bubbles form (less carryover), also when distilling (or even evaporating in dish with watch glass) as the solutions concentration changes, from gases leaving the system, the temperature (or boiling point changes as this progresses), and if you are not closely monitoring the POT, so then keeping the temperature lower when using either of these methods is best, as you may get a boil over when you turn your back.

Solutions will vapor of gases way below the boiling point of that solution so a lower temperature does no harm, it just takes more time.

I do have a brand new distilling glass lab set still in the box and never got it wet, but I do use my home made distilling rigs, the sand bath and pickle jar has distilled many gallons of solution, so I just keep using it, I also have a coffee pot Pyrex, it looks similar to a flask (wider mouth) with a handle, I made a Teflon cork and use a hose and distill with it sitting on an electric hotplate in a casserole dish (no sand used).

That store bought distilling rig is just too pretty to use.
 
It may also be a good idea to discuss some precautions if we do use distilling; I will note a few here.

As with any process in glass, the temperature of the glass should not be changed quickly, this can thermally shock the glass and crack or break it, also glass ware should be chosen for the heating method you are using, sand baths or oil baths can be used (I prefer sand bath as nitric concentrate and oil scares me), a sand bath is just a pot of sand surrounding the jar, to heat it indirectly and evenly (the pickle jar or canning jars were made to boil in water, and in a sand bath protected from direct heat and heated evenly these jars perform well as long as temperature is not changed fast).

Glass ware should be chosen to be able to withstand temperature and the pressures involved.

Tubing and fittings for distilling rigs bought, or homemade should be able to withstand the hot acids you are distilling, rubber is not a good choice for nitric acid nitric eats rubber. Teflon holds up well.

Also chemical resistant tubing can be used.


When distilling the hot glass vessel can build pressure, this is not a problem as long as this pressure has a place to escape.

On cooling a boiling vessel can go into a vacuum, when distilling this vacuum can suck cold liquids back into the hot glass breaking the glass and spilling hot acid everywhere, open the distilling rig to atmospheric air before lowering or turning off heat.

Tubing and fittings for distilling rigs, store bought, or homemade should be able to withstand the hot acids you are distilling, rubber is not a good choice for nitric acid.
Nitric eats rubber. Teflon holds up well.

Also chemical resistant tubing can be used, I use a clear tubing (looks like PEX to me a type of HDPE, I really do not know for sure the type of tubing as I got it from the dumpster, but it holds up to chemicals and hot acids well), chemical resistance charts can help you select materials resistant to acids.


When distilling the hot glass vessel can build pressure, this is not a problem as long as this pressure has a place to escape.

On cooling a boiling vessel can go into a vacuum, when distilling this vacuum can suck cold liquids back into the hot glass breaking the glass and spilling hot acid everywhere, open the distilling rig to atmospheric air before lowering or turning off heat.


Here are a few links that will have some useful lab safety.


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

http://www.radford.edu/fpc/Safety/ChemHyg/chp3.htm

http://web.princeton.edu/sites/ehs/labsafetymanual/sec7i.htm#glassware

http://wolfweb.unr.edu/~jacques/safety/glass_safety.html

http://www.ehs.indiana.edu/LabSafety/LCSP%20Part%2007%20-%203.0%20Standard%20Operating%20Procedures.pdf

http://www.des.umd.edu/ls/labguide/one.htm

Want more?


http://www.google.com/search?q=lab+safety++distilling&btnG=Search&hl=en&gbv=2
 
Can &/or should you boil ? --- Yes – you can & at times you should (such as the case of “boiling” tungsten points to leach out the silver)

And I don’t think Harold is fed up with the word boil being used – when used in the right context.

It’s when boiling is suggested – when in fact the desired process goal is to evaporate – that Harold is fed up with - & rightfully so IMO

Another words – Harold is fed up with people being told to boil a solution - as the evaporation process – when doing so is the cause of lost values.

When the desired process goal is to evaporate – the words – “But Do Not Boil” – should be included - IMO

Kurt
 
Years ago, I graduated from Penn State University. I took the Nuclear Energy Technician course which included a lot of classes on thermodynamics and heat transfer. We were taught there are no less than seven types of boiling from the point where small bubbles start to form on the container to all out boiling where the steam bubble are huge and blow the liquid all over the place. I can see where Harold has problems when people use the term boiling when they should be saying evaporation and vice versa.
 
kurt said:
Can &/or should you boil ? --- Yes – you can & at times you should (such as the case of “boiling” tungsten points to leach out the silver)

And I don’t think Harold is fed up with the word boil being used – when used in the right context.

Correct. I used heavy boiling in many of my operations-----some where had I not, the process wouldn't have worked. An example would be the processing of polishing wastes, where the preliminary wash with HCl required heavy boiling in order to keep the solids in suspension. Even then, without care, I occasionally experienced areas that failed to suspend, resulting in superheated areas that lead to fractured vessels when they were stirred.

There's more than a few examples of boiling being desirable. Evaporation just happens to not be one of them. The repeated *boiling down* that I see yields no end to problems, and it's clear to me that those who continue to use the terminology are perpetuating the problem. It's as if my words fall on deaf ears.

Don't boil when evaporating, unless you have provisions for preventing the resulting spatters, or to capture the traces of values that are propelled from bursting small bubbles at the surface. Each of those circumstances lead to losses, and they're dead easy to prevent by simply keeping the solution below a boil. What the hell is so hard about that?

Harold
 
1. Evaporation.
2. Boiling.
3. Distillation.

These are all different terms, with different meanings.

They have different purposes, plus different safety measures are necessary.

It's a very bad thing, for both financial and health reasons, to recklessly interchange them.

Thanks to Harold for continually pointing this out, and being adamant about it!
 

Latest posts

Back
Top