Acetone to aid reaction !

[photoman290]

Did you manage to do this test? I really would like to find a way of identifying Meth/Acetone percentages in the distilate. I think if we can find this then a high percentage of the Acetone can be recovered and since it is not actually consumed during the reaction the volume used is academic. We can just use the optimum 25% or whatever is best.

Dave

i have  had a quick look at using chromatography  to  check to pecentages of meth and acetone. checking if you have any meth left can be done using potassium di chromate mixed with battery acid. it changes colour in the presence of methanol.

having also spent years designing and using things that can kill people i also like to know what i am doing before i do it.

[photoman290]

i feel it is important to follow the experimental method  in the paper as closely  as possible otherwise we will get confusing results. ok recovering the acetone at 25 torr might prove a bit difficult, but that doesn't affect the reaction.  once we have established a base line then is the time to experiment with less acetone. being as non of us are trained chemists, as far as i know? it is important if a chemist did come along to present  them with  the same experiment as in the paper.
i know i am struggling with a lack of basic chemistry. if they used 25% acetone there must have been a good reason. if it worked with 10% i am sure that is what they would have used and if they did they would have said.

I cant say I am in agreement with you on this, we know it works with the amounts they used, they have written the paper. However for me it is impracticable to use these amounts without the ability to recover the Acetone in a guaranteed re-usable state. We know why and how it works and using as little as 1 litre in a 180 litre batch had positive results based on our usual 2 stage no titration method. My next batch will have more adjustments which will either further improve my previous results or not.

agreed we know it works according to the paper. but what the paper doesn't say is if it will work as well will smaller quantities of acetone. how much meth is taken up by the GL may well vary using different percentages of acetone. what i mean by this is we may be assuming the relation in linear. it may be or it may not be. unless we test using the same ratio we wont know. i don't see why it shouldn't be linear but i can't say that for certain until it is tested. not  wanting to  waste  acetone because it might not all be recovered is not a very scientific approach in my humble opinion. there  might be a magic percentage but all we know is 25% seems to be the maximun.

[photoman290]

i feel it is important to follow the experimental method  in the paper as closely  as possible otherwise we will get confusing results. ok recovering the acetone at 25 torr might prove a bit difficult, but that doesn't affect the reaction.  once we have established a base line then is the time to experiment with less acetone. being as non of us are trained chemists, as far as i know? it is important if a chemist did come along to present  them with  the same experiment as in the paper.
i know i am struggling with a lack of basic chemistry. if they used 25% acetone there must have been a good reason. if it worked with 10% i am sure that is what they would have used and if they did they would have said.

I cant say I am in agreement with you on this, we know it works with the amounts they used, they have written the paper. However for me it is impracticable to use these amounts without the ability to recover the Acetone in a guaranteed re-usable state. We know why and how it works and using as little as 1 litre in a 180 litre batch had positive results based on our usual 2 stage no titration method. My next batch will have more adjustments which will either further improve my previous results or not.

agreed we know it works according to the paper. but what the paper doesn't say is if it will work as well will smaller quantities of acetone. how much meth is taken up by the GL may well vary using different percentages of acetone. what i mean by this is we may be assuming the relation in linear. it may be or it may not be. unless we test using the same ratio we wont know. i don't see why it shouldn't be linear but i can't say that for certain until it is tested. not  wanting to  waste  acetone because it might not all be recovered is not a very scientific approach in my humble opinion. there  might be a magic percentage but all we know is 25% seems to be the maximun.

I am not nor ever will be a scientist so doubt I will ever take a scientific approach, time to go underground I think.

dont do that!! my comments are not directed to anyone in particular. just trying to establish some scientific method to the process. your experiments are what got us here in the first place. please carry on reporting your results.

[Tony]

Acetone is definitely miscible with NaOH Glyc, and it rapidly sets solid (50:50 ratio) without any separation.  This is in the absence of Methanol, however.

[1958steveflying]

Acetone is definitely miscible with NaOH Glyc, and it rapidly sets solid (50:50 ratio) without any separation.  This is in the absence of Methanol, however.

That was an interesting finding of your's Tony I will try a sample of KoH glyc and Acetone.

[thewormman]

Acetone is definitely miscible with NaOH Glyc, and it rapidly sets solid (50:50 ratio) without any separation.  This is in the absence of Methanol, however.

Do they separate when heated and liquid again?

[Tony]

Acetone is definitely miscible with NaOH Glyc, and it rapidly sets solid (50:50 ratio) without any separation.  This is in the absence of Methanol, however.

Do they separate when heated and liquid again?

Not tried this though I need to in order to get the solid lump out of Nathanrobos nice centrifuge glassware 

[Dickjotec]

I have just finished the bubbling of the bio I made on Saturday. It has had 24 hours bubbling.
On the surface is a thick sheet of thick foam, it looks like HPME. I have never had this before could just be coincidence or could be the acetone? Will take a pic and test it later. If it is HPME I wonder how much more is in the tank?
Dick

[Tony]

Hi Dick I almost always get it, it depends how long I bubble for.  24 hours is usually not enough for it to form, but if bubbled longer (36 hours) it will almost always appear.   I assumed it was soaps and its presence was an indication that all the Methanol was successfully removed. I give it a good stir into the surface liquid and it sinks to the bottom.

If it is soaps, then maybe Acetone has somehow reduced the Methanol content in some way?

If it's HMPEs then that raises a bunch of other questions!

[1958steveflying]

I have just finished the bubbling of the bio I made on Saturday. It has had 24 hours bubbling.
On the surface is a thick sheet of thick foam, it looks like HPME. I have never had this before could just be coincidence or could be the acetone? Will take a pic and test it later. If it is HPME I wonder how much more is in the tank?
Dick

I had that once when my bubble stone was really low in the tank, I made the assumption it was stirring up the soaps that were trying to settle,

[Carrington]

The sample I did last at the weekend has been left to settle and now has a layer if crust on the top, this sample was
25%meth
25% acetone
75% required ASM using a base of 3.5
 
Mixed twice but Glyc left in between mixing
1st mix 1.5-2 mins
2nd mix 2mins
Temp 25c

Will see if I can test it

Paul

[Dickjotec]

I have just finished the bubbling of the bio I made on Saturday. It has had 24 hours bubbling.
On the surface is a thick sheet of thick foam, it looks like HPME. I have never had this before could just be coincidence or could be the acetone? Will take a pic and test it later. If it is HPME I wonder how much more is in the tank?
Dick

I had that once when my bubble stone was really low in the tank, I made the assumption it was stirring up the soaps that were trying to settle,

You could be right. I used a new bubbler as the normal one fell off the pump into the bio! The new one is longer.

[Dickjotec]

It looks like the foam is HMPE

Foam

I have heated a sample to 50C and it is clear. A mix with 50/50 water is now splitting, it is in a hot45C room.


Hot sample on left initial water mix on right.
Have taken a sample from the bottom of the tank and the bio is cloudy but has no evidence of 'cotton wool'. It is settling and showing clear bio above HMPE.

Perhaps the acetone stops HMPEs coalescing?
Dick

[1958steveflying]

It looks like the foam is HMPE

Foam

I have heated a sample to 50C and it is clear. A mix with 50/50 water is now splitting, it is in a hot45C room.


Hot sample on left initial water mix on right.
Have taken a sample from the bottom of the tank and the bio is cloudy but has no evidence of 'cotton wool'. It is settling and showing clear bio above HMPE.

Perhaps the acetone stops HMPEs coalescing?
Dick

I have done a 50/50 test on my settled batch and have a heavy white line in between water and Bio. I have fuged a fair amount of HMPE/wax out already so yet to work out what this is, I am going to have to try some acid neutralisation samples maybe.

[Dickjotec]

BTW the glyc from the batch on Saturday has now set. I will do a 50/50 tomorrow and see what the interface is like.
Dick