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roeintgen
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[*] posted on 29-9-2021 at 00:47
Glassware cleaning routine


I'm really somewhat paranoid when it comes to cleaning glassware that I'm leaving some impurities there and it's gonna mess up my reaction or something.

My routine is: if it's water soluble and non toxic that can be discarded it's poured down the drain, the flask rinsed with water, then ethanol and dried.

If it's water soluble and hazardous, I try to neutralize it or otherwise store it in waste container, washings also store in waste container and then rinse with ethanol/acetone and then burn the solvents, dry glassware with heat gun.

If it's organics, then distill the solvent if possible, if not then try to neutralize it that it could be poured down the drain, if not then store it in waste container. Ethanol/acetone washes are either burned or stored along with the waste.

How do you deal with dirty glass with potentially dangerous solvents/byproducts &what do you think about this writeup?
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teodor
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[*] posted on 30-9-2021 at 04:00


For me, waste processing and cleaning are different procedures.

Waste processing is much more dependent on the waste nature. Some organic compounds I use to kill ants in my backyard, many of them being quite toxic or carcinogenic for humans are bio-degradable (there is no smell after 1-2 days). For heavy metals, I have nice pots when I collect them as residue.

As for cleaning, my best friends (in the order from most used ones to rarely used ones) are:
- tap water
- distilled water. I have a bottle for rinse and I return the water to this bottle. So, it can be used many many times.
- Sodium phosphate solution + pumice
- diluted HCl
- ethanol
- acetone
- cold 10% NaOH
- cold chromic acid
- hot 10% NaOH

As a last resort, I use the dirty flasks for doing some aggressive reactions, like H2SO4 distillation etc.
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TheMrbunGee
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[*] posted on 30-9-2021 at 04:34


Heavy metal salts I put in a large open container, mostly as solutions and let the solvents dry off naturally. Usually I do not mix different metal salts, but If I have tiny quantities, they all go to non recoverable waste, with what I have no plan jet (I have a 5l container with about 150g of solid unknown chemical mixture, that I would not touch pour down the drain or look at for too long). for large amounts of salts I collect them and then recover as much as I can, discard the rest (<1g quantities might go into environment sometimes but I rarely do super toxic chemistry).

for uncleanable organic mess from glassware I use hydroxide/peroxide mix as strong as necessary or sometimes acid/peroxide.

Then again I never worried about invisible impurities, I see how d.water sticks to glassware, and if it sticks, its clean enough for me.




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[*] posted on 11-10-2021 at 21:43


I got a pair of condensers (an Allihn and a Dimroth) but I got them when I went dumpster diving. The glass is completely intact, no usage crud or anything visible, just storage grime. The Allihn condensor was filled small boiling chips (it took a lot agitation to get them out) while the Dimroth had nothing but small amounts of grime.

So far I washed them soap and water, as well as a solution of sodium carbonate in order to neutralize any acids. After the wash the tube is quite clean, but I need to run some water through the cooling jacket/spirals to clean those out as well.

I have no idea what the previous owner used them for. I want to clean them as completely as possible in case the previous owner didn't clean it correctly before tossing it out. I found them amid all sorts of other neat chemistry equipment. But I only kept the condensers.

Quote:
As for cleaning, my best friends (in the order from most used ones to rarely used ones) are:
- tap water
- distilled water. I have a bottle for rinse and I return the water to this bottle. So, it can be used many many times.
- Sodium phosphate solution + pumice
- diluted HCl
- ethanol
- acetone
- cold 10% NaOH
- cold chromic acid
- hot 10% NaOH


I don't have any phosphates or dichromates, what would those neutralize?

I plan on using the condensers to make nitric acid and refluxing nickel nitrate. The Allihn for the reflux, the Dimroth for the nitric acid.
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Herr Haber
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[*] posted on 12-10-2021 at 10:01


Tap water
Distilled water
Isopropanol (cheaper than ethanol here)
Acetone

I use salt or sand as a mechanical abrasive.
It is quite unusual if I have to go beyond those.
I have used H2SO4 in the high 150, low 200°c. Never was brave enough to add H2O2




The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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teodor
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[*] posted on 12-10-2021 at 10:33


Quote: Originally posted by ManyInterests  

I don't have any phosphates or dichromates, what would those neutralize?

I plan on using the condensers to make nitric acid and refluxing nickel nitrate. The Allihn for the reflux, the Dimroth for the nitric acid.


Sodium phosphate works similar to soap or washing powder, it is a general detergent that was a component probably of any washing powder in the past but then it was prohibited as everything else (it cause the growth of duckweed or something like that in rivers). It is much easier to wash out than household washing powder though.
A chromic acid solution is a universal all-hands cleaner for chemical glassware, but dichromates were prohibited (as everything else) so it is not used in many labs anymore, but some people say piranha is equally good for cold washing. It destroys almost any organic and probably even carbon (very hard places could be just carefully heated) and dissolves many insoluble salts but its usage requires some basic chemical experience of working with concentrated sulfuric acid not to mention heating this acid during the preparation. If you have no any holes accidentally made with concentrated sulfuric acid yet probably you should not try to start this way.

Making nitric acid is a good cleaning routine also. Depending on the concentration you can get different degrees of spotlessness. Just reject the first 20ml of distillate (return it to the source flask). The general rule is: if some deposit on walls is not destroyed/dissolved by the liquid which you distill it is not relevant and could stay there.

[Edited on 12-10-2021 by teodor]
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[*] posted on 12-10-2021 at 17:58


that's good to know that nitric acid is a good cleaner. I will follow your recommendation and return the first 20ml to the original container.

One other question though, and I know it's going to sound a little weird but... a friend of mine had a 2 necked 1000ml boiling flask that I thought would be better for distillations (allowing me to add the nitrates and sulfuric acid through the other neck and just plugging it without to remove or install the joints afterward).

But he was using it for a bong. So I had to clean it extensively before hand. I soaked it with 500ml of 99% Isopropyl alcohol and filled in the rest with water. I left it for 24 hours and then scrubbed the interior as much as I could until all internal stains were gone (those flexible necked brushes are a godsend), after which I scrubbed it with dishsoap and water until it looked like new. Then I soaked for another 24 hours in 95% ethanol alcohol (700ml) and filled it to the joints with distilled water. I had a stir bar in for an hour as well.

The thing is spotless now and should be clear of any THC. But I am wondering... I will need to return it to my friend after I am done with it. Since I will be using it for making nitric acid, will I need to do any special cleaning for it afterward, or will washing it out with a sodium carbonate solution be sufficient?
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[*] posted on 13-10-2021 at 02:53


ManyInterests, I don't recommend adding components to the distilling flask during the process of making the nitric acid.
My first experience with making nitric acid was unsuccessful and I would prefer to make something else if I could return to that day.
Could you please share more details about the experiments you plan to do with the acid because your questions puzzled me a bit?
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[*] posted on 13-10-2021 at 10:28


My apologies. I want to make small quantities of energetic material. Specifically NHN (Nickel-Hydrazine Nitrate), picric acid, ammonium picrate (if possible) DDNP (from picric acid), ETN, and RDX.

So I will need both fuming nitric acid and 65-70% nitric acid for these.

I made a picture of my setup so far (it needs a little improving).

Basically before I put the joints. I will put the quantity of KNO3 into the flask before putting the joint and condenser (and greasing all joints with sulfuric acid). Just when I am about to start distillation I will power the quantity required of sulfuric acid through the funnel you see and then close that with the joint plug I placed on the mantel. I will not add any further material once the distillation begins.

You mentioned to put the first 20ml back into the flask when distilling, this is what I plan on doing. At least during my first distillation.

Does nitric acid distillation produce any bucking or movement of the glassware? The setup as you see it is quite steady but I don't want anything tipping over. for very obvious reasons.

My dimroth condenser cannot have any joints added, so it needs to drip directly into a container. I have several beakers that will work just nicely.

Setup.jpg - 1.8MB
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[*] posted on 13-10-2021 at 12:53


ManyInterests, you don't need to return 20 ml to the flask during the distillation. Just keep it separately, so you can use it for the second run for the fuming acid. Also, your setup is not safe enough for distilling the fuming acid. Try to use the vacuum type of receiver for that. Also clamps could be damaged, so provide some additional fix for the condenser (piece of wire?). Also, make sure the thermometer adapter doesn't contain a silicon/rubber part.
For cleaning the flask after the acid.
Put a little water or (better) sodium (bi)carbonate solution, close it and allow to stand to absorb nitric oxides. Then fill the flask with water to the top to displace all fumes. Be careful at this step. Then wash 5 times or attach a piece of hose to a tap, turn the flask upside down and put hose through one neck allowing water fountain to wash the internal surface.
You don't need any neutralization. Nitric acid is liquid so it just evaporates. If the glass is dry there is no acid.
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[*] posted on 13-10-2021 at 13:26


The joint at the top allows for a thermometer to be inserted, which I have and will use (as I cannot the mantle's own thermometer) It does appear to have a seal on the top. But I have seen that exact type used by people distilling nitric acid (fuming and otherwise) by NileRed, and other chemistry YouTubers. Links below:

https://youtu.be/QmCdrDLyNXQ

For NileRed While we don't see the absolute top. I don't know of any other joint that would allow for an insertion of a thermometer in any other way.

https://youtu.be/-vuLjbXh5Qc

For the Canadian Chemist. He uses the same kind of joint. I assume he has smaller glass funnels than I do, because I was not able to fit my funnel through the top joint that I have.


Quote:
Put a little water or (better) sodium (bi)carbonate solution, close it and allow to stand to absorb nitric oxides. Then fill the flask with water to the top to displace all fumes. Be careful at this step. Then wash 5 times or attach a piece of hose to a tap, turn the flask upside down and put hose through one neck allowing water fountain to wash the internal surface.
You don't need any neutralization. Nitric acid is liquid so it just evaporates. If the glass is dry there is no acid.


That's good! Because that's how I also cleaned my glass after sulfuric acid purification. Also my glassware after making nitrocellulose (mixing KNO3 with sulfuric acid to make a nitrating mixture). I always have plenty of sodium carbonate because of how cheap and easy it is to make.

Joint1.jpg - 1.6MBJoint2.jpg - 1.7MB
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Herr Haber
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[*] posted on 13-10-2021 at 13:58


Just add the chilled acid after your nitrate, put everything in place, clamp the condenser aswell than all you have to do is adjust the temperature and add Al foil to prevent heat loss and protect from light. Using this funnel makes it unnecessarily complicated. Put a stopper instead and make sure it doesnt leak.

Your condenser is less than ideal for the task. Actually, it's probably the worst one. Get an adaptor to let the acid in a flask immersed in ice / salt. Your lungs will thank you.
Do this outside or at least on the ledge of the window because I'm pretty sure you'd gas yourself with that setup no matter how experienced your are.
Making nitric acid takes a lot of time even with a good setup. Making *quality* nitric acid takes even longer.
The one thing that is certain is that the bong condenser will be absolutely clean.

That said, to clean that part I would first fill it with vegetable oil and an abrasive such as sand. Then I'd do the same with ethanol / isopropanol.
If it's not clean after that, hot nitric acid will definitely do the trick.





The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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[*] posted on 13-10-2021 at 14:52


I have another Allihn condenser (bulb condenser) that I can fit another adapter to. If that is your recommendation I will do so. This is because I have no adapter for the other condenser.

And yes, of course I will be doing it outside. I setup my balcony for such things and make sure that all my neighbors are not at home or asleep so as not to cause any alarm. Safety is my number one concern.

Thank you.

[Edited on 13-10-2021 by ManyInterests]
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[*] posted on 14-10-2021 at 05:11


An Alhin condenser would be a much better choice. Not "the best" but sill way better than the current one.
I recommend an adaptor anyway. Look for Deschem on eBay it's a really good and cheap source. What you'll spend there you'll save it by getting more acid.




The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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[*] posted on 14-10-2021 at 15:07


Thanks, but I think I have all the adapters I need. They fit in quite neatly and with clamps they are rocksteady (I will of course grease them with sulfuric acid before clamping them.

I need to also mention here that I will be buying a respirator. I am nitrating a bit of nitrocellulose right now using 98% purified H2SO4... and I need to say this, while the fumes from the drain opener acid were tolerable, the ones from the pure acid were unbelievable!

I had to leave my apartment ( did the nitration on my balcony, but the way the wind was blowing it blew the fumes directly into my place) for a while to let my apartment ventillate because it was unbearable. I feel like it might have done something to me, but it'll be better.

I need a respirator! Even if I make my nitric acid in the balcony and close the door (I have the power switch in side so I can switch it off as needed without opening the door) and never need to go outside to see if it done. I don't think I can do any nitration without being exposed to some gasses. I need to have that thing on me at all times. I will do them all on my balcony, but I need to keep my apartment door closed to prevent any gasses from coming in.
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[*] posted on 15-10-2021 at 02:21


Quote: Originally posted by Herr Haber  
An Alhin condenser would be a much better choice. Not "the best" but still way better than the current one.


And what is "the best" in your opinion? I personally used Dimroth condenser for many distillations (including WFNA) and didn't see why it could be not "the best". It would be interesting to know what I missed.

Also, as a receiver, it is convenient to use 2 necks flask.

I wouldn't use sand in any cleaning routing personally, I think it can scratch glass and I don't like scratched glassware, but this is a matter of preference.

[Edited on 15-10-2021 by teodor]
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[*] posted on 15-10-2021 at 22:07


Quote:
And what is "the best" in your opinion? I personally used Dimroth condenser for many distillations (including WFNA) and didn't see why it could be not "the best". It would be interesting to know what I missed.


Yeah, I don't know what 'the best' would be. Every chemistry YouTuber who made Fuming HNO3 or 68% HNO3 had far more basic setups than that. Just a simple liebig condenser with cold water flowing through for cooling. From the flask to the Alhin consenser I have the thermometer attachment joint, and on the other end I will have a vacuum joint. The vacuum part is optional, but even without the pump attached it makes a very firm seal with the receiving flask.

The only thing I need to do is raise the mantle on a platform, because the receiving flask will not fit.
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[*] posted on 16-10-2021 at 01:34


I just have the impression that the Dimroth condenser is more effective than Liebig. I had some issues only with diethyl ether distillation, for anything else it works pretty well. The completeness of condensation in Dimroth is more visible than in Liebig - you can see where is the end of the condensation area inside the condenser - some part of the spiral will be covered by drops and after that it is clear, so you see how complete the condensation is. With diethyl ether you see the drops covered the full length of the spiral - that's a signal that some ether escapes condensation.

[Edited on 16-10-2021 by teodor]
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Herr Haber
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[*] posted on 18-10-2021 at 06:48


A Graham maybe but a Dimroth ? I'd use a Liebig for the task at hand.



The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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[*] posted on 12-11-2021 at 01:55


Dimroths are far superior compared to liebigs. If you want a good combo, use dimroths as condensers and put a graham after it as a cooler unit. Better yet, use two coolant reservoirs, normal one for dimroth and a cryo-coolant (either salt-ice or CaCl2 solution) for graham.

I used this kind if setup when I dehydrated reactions under vacuum. The water goes freely through any single stage condenser setup, no matter how cold coolant you use. I first used a dimroth as a condenser with snow-ice water(winter time), then a graham as a cooler unit with separate, but same composition coolant to bring the condensate as cold as possible. The 3-neck receiver flask was also immersed in a bucket of ice water. Finally, the vacuum outlet was put on top of a liebig condenser, with the graham circuit, so any residual vapors would face as much resistance as possible, and finally the pump had a -30C CaCl2 solution coldfinger. I managed to keep the oil clear over multiple hours of distillation.
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[*] posted on 12-11-2021 at 21:53


That doesn't look like a Dimroth in that picture.
It looks like a coil and tube condenser, which has both the outer jacket of a Liebig and the inner coil of a coil condenser.

These are very efficient, and expensive, condensers, and they have a very high internal surface area to volume ratio.

This one is unusual in that the coolant is entirely fed through the inner coil and then goes through the outer jacket.
Most coil and tube types I've seen are built with an internal nozzle which directs some of the coolant through the coil while the rest runs through the jacket.

Why can't you put joints on it?
Does that drip extension on the end foul the joints?

Some coil and tube condensers are designed specifically to be used vertically with the output going right into a flask.

Not sure why this is but I've got an old one with an integral drip tip that can only be used vertically because otherwise it would trap lots of distillate in the condenser.

Mine has an internal drip tip that would be tough to remove cleanly, but that external tip on yours could be cut or ground off some day if you've got a Dremel tool. A little work with wet sanding paper will smooth it out.

EDIT: Maybe I missed it and somebody already mentioned this, but in addition to an adaptor between the condenser and collection flask you can add a hose (not rubber, some more inert plastic) on the vacuum take-off for the adaptor and run it into a gas trap to absorb those toxic gasses. Or a scrubber.

There shouldn't be any smell getting out during the distillation, except possibly a very slight one.

Learning to set up your apparatus for proper safety is vital.
Get those vapors under control before they blow into your neighbor's apartment and the emergency services get called.

[Edited on 13-11-2021 by [SWIM]

[Edited on 13-11-2021 by SWIM]

[Edited on 13-11-2021 by SWIM]




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[*] posted on 15-11-2021 at 04:10


I use Dimroth horizontally, it is very efficient for distillation at atmospheric pressure. Yes, it can keep a few milliliters (~2 ml) of distillate when it is used horizontally but I don't see it as a big problem because usually, I use it for larger volumes than my Liebig (and my Liebig also holds some distillate when used horizontally).
I am interested to know how do you measure the efficiency when you say that Dimroth is not efficient.
I suspect it could be only the case when the volume of vapors / stream speed is very fast, which is rarely the case with my heat sources.

[Edited on 15-11-2021 by teodor]

[Edited on 15-11-2021 by teodor]
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[*] posted on 17-11-2021 at 13:46


Maybe it's just in my head because I was tought Dimroths are for reflux and never questioned beyond that ;)
I may have used the Allihn a couple of times when it was closer than a Liebig but dont tell anyone!

To be honest, I think the question of efficiency is related to what you are going to do with your condenser. The big volume of coolant inside a Liebig suits my needs most of the time. I get vapors when I dont cool enough.
On my to-do list are a couple of Soxhlet extractions. My gut just tells me I'll want something with a bigger volume for vapours than a Liebig.

But right now... I have to find something to do with what Santa sent. A beautiful Davies !




The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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