Acetone to aid reaction !

[photoman290]

if you move down here i will be your apprentice. high wages clean working conditions and a day off to lie on the beach went the weather is fine,ohh and plenty of tea and biccys.

[Dickjotec]

I don't think the salt would remain in the meth/acetone , it would just settle to the bottom , I thing sodium sulphate would probable do the same job as this is another drying salt. For sodium sulphate I create about 100kg's a day just haven't got round to trying to dry it yet to see how good it is at water absorption. Is there a situation's vacant on this site I could do with a apprentice ( low wages harsh conditions grumpy boss )

If only you were closer!
Dick

[Tony]

Is there a situation's vacant on this site I could do with a apprentice ( low wages harsh conditions grumpy boss )

When I was younger such a thing would have been more fun than work for me

[Tony]

Anyway what seemed to come up a lot was to use Epsom salts. The salts absorb water but not Acetone or Methanol, so you heat the salts to dry them first, then gradually add it to the Methanol, as it sucks up the water it forms into clumps so you keep adding it till it stops clumping, and stays as grains. It then drops down to the bottom of the jar and you just filter it out. Heat it to 150 degrees C to dry it then use it again.

The more scientific way is to use a Molecular sieve, basically crystals that are used in labs to dry these types of liquids. Good explanation here: http://www.bio.umass.edu/microscopy/mol_sieves.htm

This is what I reckon we can use to dry our distillate to be able to work out volume of Methanol to Acetone

That's very interesting.

With Acetone distillation at a much lower temp than water it would naturally favour distillate with only trace water - but as we know with Methanol it can easily lose purity with water present.  This could solve that part of the Acetone cosolvent method.

[Tony]

Was quite strange to read actually, these things being discussed on an open forum 

Personally I think people should be entirely free to do whatever they like to themselves, so long as it doesn't harm others.

[Head Womble]

Is there a situation's vacant on this site I could do with a apprentice ( low wages harsh conditions grumpy boss )

When I was younger such a thing would have been more fun than work for me

If you were any younger you'd still be one of those little swimming things.

[Jamesrl]

Is there a situation's vacant on this site I could do with a apprentice ( low wages harsh conditions grumpy boss )

When I was younger such a thing would have been more fun than work for me

If you were any younger you'd still be one of those little swimming things.

And kids should be seen but not heard, in anyway what's he doing down from the chimley.

[Tony]

Is there a situation's vacant on this site I could do with a apprentice ( low wages harsh conditions grumpy boss )

When I was younger such a thing would have been more fun than work for me

If you were any younger you'd still be one of those little swimming things.

And kids should be seen but not heard, in anyway what's he doing down from the chimley.

Just fetching your teeth back grandpa, looks like they got carried up there on a sudden gust of hot air 

[thewormman]

not sure we want to be adding a possibly corrosive salt solution to our bio. i know  molecular sieve no 3 is ok but not sure about epsom salts. does the water matter that much? apart from academically. we know the reaction works with less than 25% acetone so as long as we get most of the acetone back i cant see removing the water being too big a deal.

The salts don't dissolve into the acetone/meth but I was just saying what I read the molecular sieve is much better. The amount or removal of water is important because if you don't know the quantity in the distlate you cannot work out the volumes of acetone/methanol and therefore you can't work out what you are putting back into the next reaction

[Dickjotec]

Reading the molecular sieves info it occurs to me that it is for small amounts of water and solvent so while it will dry a sample for testing it would not be suitable for the amounts of liquid we would be using. The drying under vacuum of the used sieves would also be problematical.
Perhaps just testing a sample to establish the various proportions of constituents would be sufficient? Very accurate volume and weight measurements will be required.
Dick

[Tony]

My bubblier was always in the very bottom, I'd have to pull it out of the settled soap/gly each time I did a new batch,
and then let it rest on top.
I've only ever seen honeycomb looking stuff form on top, and this was if I'd made a really soapy batch.

My bubbler is also resting on the last batches drop out and I never get a head like that in the picture. I did in the very early days of bio brewing but not for years now.

Just to add to this part of the debate, I've done an overdose batch (bone dry oil and excess catalyst) and got a single stage sparkling clear pass on the 5/45.  Went on to do WBD up to 90C.  Bubbled from 1/3 up from bottom of the settle drum this time, but still got a creamy/foamy top.  So I don't think it is necessarily stirring up soaps from the bottom that causes it.

[Head Womble]

Tony, I seem to remember having a conversation with you about this foam on top,
didn't we decide it was due to not demething completely.

[1958steveflying]

My bubblier was always in the very bottom, I'd have to pull it out of the settled soap/gly each time I did a new batch,
and then let it rest on top.
I've only ever seen honeycomb looking stuff form on top, and this was if I'd made a really soapy batch.

My bubbler is also resting on the last batches drop out and I never get a head like that in the picture. I did in the very early days of bio brewing but not for years now.

Just to add to this part of the debate, I've done an overdose batch (bone dry oil and excess catalyst) and got a single stage sparkling clear pass on the 5/45.  Went on to do WBD up to 90C.  Bubbled from 1/3 up from bottom of the settle drum this time, but still got a creamy/foamy top.  So I don't think it is necessarily stirring up soaps from the bottom that causes it.

 Was Acetone added to this batch ?

[Tony]

Tony, I seem to remember having a conversation with you about this foam on top,
didn't we decide it was due to not demething completely.

It seems (though it's hard to tell) that there is a correlation between the amount of Methanol remaining and the time taken for this foam to appear when bubbling.  So if I have a really well WBD'd batch it can appear in less than 24h, but otherwise it can take a couple of days of bubbling.

My feeling was that the foam appearing indicated that very little Methanol remained in the batch, so I bubble until I see it these days.

I suppose I should see if the foam is soluble in Methanol.  I anticipate that it will be, certainly from conversations here it appears to be one and the same with the HMPE (or whatever it is) cream that forms at the bottom of batches.  Usually I stir the foam into the surface and it sinks (to become "HMPE"s?)

Certainly from my reprocess batch the creamy stuff gives a 3/27 pass - soluble in Methanol - so if the foam is the same it will also be soluble in Methanol - which ties in with my speculation that it doesn't start to appear until the Methanol has been driven out.

My bubblier was always in the very bottom, I'd have to pull it out of the settled soap/gly each time I did a new batch,
and then let it rest on top.
I've only ever seen honeycomb looking stuff form on top, and this was if I'd made a really soapy batch.

My bubbler is also resting on the last batches drop out and I never get a head like that in the picture. I did in the very early days of bio brewing but not for years now.

Just to add to this part of the debate, I've done an overdose batch (bone dry oil and excess catalyst) and got a single stage sparkling clear pass on the 5/45.  Went on to do WBD up to 90C.  Bubbled from 1/3 up from bottom of the settle drum this time, but still got a creamy/foamy top.  So I don't think it is necessarily stirring up soaps from the bottom that causes it.

 Was Acetone added to this batch ?

No acetone in that one, no.

[Julian]

I haven't been following this frothing issue word for word, so sorry if I've missed anything and the following is complete drivel.  But if it only occurs when bubbling, could the issue be moist air, the same problem as I suspect I had when trying to dry oil and distill Methanol?