# Lab glass



## pinman (Jan 30, 2010)

Given access to lab glass, What types and sizes of glass would one want to have in their hobbyist refining lab? What would be the ideal vessel for the reaction? If affordable What pieces would be required for a closed system? 
Thanks


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## 4metals (Jan 30, 2010)

What do you mean by a closed system. A beaker with a watch glass will direct the fume out of the pour spout where it can be collected in a fume hood. Then there are reactors with heads and condensers to condense your fume and again direct it to a collection point in a hood. Glass is nice but it breaks. 

I remember reading that Harold processed in 4 liter glass beakers and he processed quite a bit of material. 

Today a heavy walled pyrex glass beaker with a watch glass will set you back about $120. You can heat it on a hot plate but you have to be careful. 

I just priced reactors for a client so these prices are current. For a closed reactor a 5 Liter flask with a 4" conical neck will cost you $199, the heating mantle $358, rheostat $163, Glass head with 2 necks $349, condenser varies, I like vigereaux condensers, 24" long $455, clamp for head $277, and plug for 1 neck $19. This size compares in processing volume to a 4 liter beaker, actually it holds a little more, but it is obviously more costly. 

If it were me, I'd put the cash into a good hood and scrubber and go with a 4 liter beaker.


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## Irons (Jan 30, 2010)

4 metals is right. I've been building a closed system over the Winter, and so far, I'm out over $3K. If you don't have any previous experience, hire a pro to set it up for you.


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## pinman (Jan 30, 2010)

When saying closed I was referring to just as you mentioned, condensing and collecting. I only ask because I have gathered quite the collection from a second hand store. I will post pictures tonIght to see if maybe someone could make sense from the collection.


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## 4metals (Jan 30, 2010)

Most of the glassware available second hand is old organic glassware kits. They're fine for the fittings, condensers, reflux columns etc. but in refining you need access to inside the reaction chamber. Imagine digesting some karat and having to clean out the vessel of the insoluble chlorides form the small 29/42 tapered hole most have on top. Even if you're inquarting getting out the insoluble gold after a nitric leach is also a pain. Not to mention getting the scrap in.

The reactor I mentioned has a 4" conical neck, big enough for most to get an arm in to clean up if necessary. They come in 5 liter, 12 liter, 22 liter, 50 liter, 72 liter, 100 liter, and 200 liter. For small capacity the 5 or 12 work well. Over 22 liter I would go with a bigger condenser. Now you're getting into real money.


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## pinman (Jan 31, 2010)

Here is the glass I have collected. My girlfriend and I actually decorated our Christmas tree with some of it this year.


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## 4metals (Jan 31, 2010)

As I assumed, lots of organic glassware. The sep funnels are probably 1 liter, it appears you couldn't get any closer to the ceiling to take that photo. Don't see any condensers or large spherical vessels, Buchner funnels are useful but be careful on the glass fritted funnels, they clog easily and don't clean up well. (cover the frit with filter paper to protect it and don't use gravity filtration as the liquids will seep under the paper) 

Some of the large columns look like resin columns, they could be useful.

What are you looking to process?


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## pinman (Jan 31, 2010)

There are 2 small condensers and 2 what appear to be 1/2gal spherical flasks as well as 2 1cup? Spheres.
I would really like to process karat gold and maybe refine foils on a small scale. Very small. Maybe a few grams to an ounce at a time.


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## pinman (Jan 31, 2010)

Would "pharmed" tubing be suitable for cointaining AP vapors?
It's specs are located here...
http://www.coleparmer.com/techinfo/techinfo.asp?htmlfile=SelectingTubing.htm&ID=700


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## 4metals (Jan 31, 2010)

It's one thing to contain fumes, another to neutralize. Contain them on their way to where? Yes that tubing will withstand exposure to acid fume.


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## pinman (Jan 31, 2010)

My goal/intent is to safely dispose of my wastes. So I was thinking I could condense then neutralize. I have the glass so I am just trying to put it to use.


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## pinman (Jan 31, 2010)

If I'm making this more difficult than it needs to be please tell me.


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## butcher (Jan 31, 2010)

well it sounds a little more complicated than my mason jars, and coffee pots, or my pickle jar distiller, but with all of that glass you can build a nice looking distilling rig all of us hillbillys would envy.

tools for this can be simple, or complicated, the main thing they work, serving the purpose intended, are safe easy to use, and don't loose, or contaminate your values.


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## 4metals (Jan 31, 2010)

Fumes are neutralized by scrubbing the fume in a sulfite solution followed by a caustic solution to take care of both the NO2 and the NO fractions of NOx. The glassware you have could be rigged to run the fume through bubble traps to scrub them but you will be doing quite a bit of setup to attain your goals. Plus you'll need an eductor to suck the fume through the setup. 

Read this forum and try small lots of karat using methods defined on the forum, better yet read Hoke, and try a few small lots. Completely refine to fine gold, small lots will pose little pollution if done outdoors. If you then decide this is something you want to do, then worry about a closed setup to entrain the fumes.

We'll still be here to help you and having done a few small lots you will be much better prepared to improve your processing techniques.


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## pinman (Jan 31, 2010)

I appreciate the help. I have read both hoke and ammen and am rereading hoke now. I plan on using the glass to do my ap refining experiment. I had been collecting karat scrap prior to but began gathering escrap after finding this forum via YouTube. I have been visiting multiple times a day since. I am totally fascinated with refining and want to pursue it as a hobby. I am in debt to all of you that provide this wealth of knowledge noxx thank you so much for making this possible. I have been slowly gathering the tools that I will need from local salvage yards and second hand shops. I even found a small ball mill!! Mind you the motor is burnt, no biggie. All my glass came second hand and my investment so far in this hobby has been minor but I want my first button!


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## 4metals (Jan 31, 2010)

Use Hokes methods, she won't steer you wrong. Get some small refining under your belt with some karat scrap and aqua regia. (inquarting with silver will make it even easier) If you've noticed her methods use the most basic equipment. 

Wait until you've successfully run karat before you jump to processing e-scrap with AP, start to process before you get your head filled with too many ideas from this forum. Keep it simple and you will succeed. 

The most interesting posts on this forum come from those that are processing and commenting on this forum, the hands on experience will steer you through the seemingly endless comments which come from both the experienced and the inexperienced. What you learn from seeing your own materials react is what will help you sort it out.


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## nickvc (Feb 1, 2010)

To heat your solutions try a cheap electric ring and place a piece of steel over the rings to give you indirect heat, they dont last forever but they do the job for a reasonable time.I used these for all the time i refined and if i remember correctly they cost about $50.


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## pinman (Feb 11, 2010)

If I condense and collect the vapor from my ap crockpot could I use it for the next batch?


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## qst42know (Feb 11, 2010)

Once you add the peroxide to Acid/Peroxide there are few if any visible fumes. AP is relatively tame fume wise. Though it will rust and corrode any and all metals in the vicinity. I haven't tried it heated though. Heated AP may take some of your gold into solution. An aquarium air pump is usually enough.

Anyone else heating their AP?


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## butcher (Feb 11, 2010)

used acid peroxide if boiled would first produce mostly water, as the Hcl concentrates to azeotrope then fume of free HCl would vapor off.

copperchloride2 can be reused as is.


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## solar seeker (Aug 2, 2010)

Ok after looking over the glass ware it looks like that Erlenmeyer flask (largest one on the top right first picture) is connected to something air tight that's connected to a rubber tube. I would use this or the large tube bottom left ,which also looks glass and air tight, as the reaction vessel. Then I would take some rubber tubing and connect it to the reaction vessel with glass pipette (tube) on the other end. I would then put the glass tube into either the other large tube on the bottom left of the first picture or into one of the round bottom flasks top left first picture and fill that other container half full with either hydrogen peroxide (30% is better) or water. So the way this works is when the reaction is going it builds pressure which forces the fumes through the tubes into the collection vessel where it reacts with the water or hydrogen peroxide to make more of whatever acid you're processing with which is commonly aqua regia which will make nitric acid. This process only reduces the fumes produced so there will still be dangerous quantities of fumes that still escape.


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## 4metals (Aug 2, 2010)

Be careful performing digestions in an ehrlenmeyer flask. Until you are familiar with the reactions and how violent they can become, using a vessel that tapers off towards the top is an accident waiting to happen. As a reaction rises in the flask, the area it has to expand decreases and it moves upward even faster. Not a situation someone new at this should be in. Use a straight walled flask so you don't accelerate the reactions rise. And always leave a t least 50% of the vessels volume to allow for a rise.


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## Harold_V (Aug 3, 2010)

4metals said:


> Be careful performing digestions in an ehrlenmeyer flask. Until you are familiar with the reactions and how violent they can become, using a vessel that tapers off towards the top is an accident waiting to happen. As a reaction rises in the flask, the area it has to expand decreases and it moves upward even faster. Not a situation someone new at this should be in. Use a straight walled flask so you don't accelerate the reactions rise. And always leave a t least 50% of the vessels volume to allow for a rise.


I heartily endorse your comments, 4metals. I'm at a loss to understand why anyone chooses an Erlenmeyer flask for these operations, and for the precise reason you mentioned, to say nothing of the difficulty in keeping them clean. 

Harold


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