Not seen this with titrated acid wash before.

[Julian]

Ah, I see regarding the calc, but don't see how it can be a one size fits all.

Having been scared of overdosing when I first started, my thoughts were turning to overdosing the acid in the first place because subsequent washes will take out any excess.  Which got me thinking, if we dry the bio thoroughly and there was excess acid what will happen to it?

I hope I'm not confusing things with my terminology ... by slurry I mean the dark brown stuff which seems to be holding onto bio thus making a sort of slurry.  I don't have much acetone, so would methanol do instead?  My thinking was that it was miscible with both water and bio, so should wash both away from the brown solid.  Any residual methanol would evaporate quickly.

[Carrington]

I'm wondering if by using acetone we could identify the remaining product as Glyc in some way.
If when mixed with acetone it all dissolves then that will tell me its not Glyc and put my mind at rest.
I'm wondering if maybe the 90/10 test isn't realy clear enough and is mabe leaving some mono's in and then wondering if the acid even at a weak solution is able to disassociate the fatty acid from the glycerine , its still this small residuals that I belive have something to do with hmpe's.

Probable just waffling now

Paul

[Julian]

I can dump a sample into a small quantity of acetone quite easily ... would that be satisfactory?

With  the methanol I was intending to wash it through a filter paper in a funnel.

You mention the 3/27 test not being clear and indicating mono glycerides.  This cropped up a year or so ago.  I asked where that part of the test came from and no one could site a source.  I tracked down what I believe to be the first mention of the test in the form of an email from Jan Warnqvist on the JTF site, and there's no mention of it in there.  I stuck a copy of Jan's mail on the wiki, here ... http://www.biopowered.co.uk/wiki/3/27_test#References

[1958steveflying]

I may be barking up the wrong tree here but as the 3/27 is scaled down from the original 25/225 it may not have sufficient quantities of meth and bio to be accurate.

 ie: maybe a clear 3/27 could have  either a cloudy 25/225 or even dropout !

[Carrington]

I was just wondering if you get any dropout with the acetone which would lead me to think Glyc to start with.
With regards to the test it was only realy ment  to work on the larger quantities as this enabled a better indication of haze (the haze probably monos) . Every partical that contributes to the haze has a full size Glyc molecule so this could amount to some considerable amount

These are just my thought and could amount to nothing.

Sorry Steve beat me to it great minds think alike

[Julian]

Sorry, but I'm struggling with the logic here.  If the ratio is the same the cloudiness will be the same, surly.

What would make cloudiness more obvious would be the size/shape/proportions (however you want to look at it) of the container in which the test was carried out.

So, we can categoricaly state that a cloudy result indicates mono glycerides?

What about a very clear but tinted result?

Jan just states "a clear bright phase".  I would say that doesn't mean cloudy, but it doesn't preclude the result being tinted.

In over a hundred batches I can only say I've had one 3/27 which could be described as both clear and colourless with one other quite close. 

I've done the business with acetone and methanol and will post later when I've uploaded some photos.

[Head Womble]

I've had a look at the stuff I removed from my drying/storage tank (formally known as my settling tank),
there is only one colour change and that looks like around 5l of waxy dropout (HMPE's ?),
nothing that looks like what you have Julian.
Allthough it has been dried, so maybe it stays in suspension once dried.

[Julian]

OK, mixed some of the dryest gunk with acetone and ran it through some filter paper.  These are the results ...




Gunk as it scraped off the J cloth after filtering out bio/water.  It was scraped from the top of the filter where it was the dryest.  It had the consistency of a paste.





Gunk with a few mls. of acetone added ... no real effect immediately.





After mixing, it appeared to form a suspension ... nothing seemed to dissolve.





Filtering arrangement.




What was caught in the filter.




Acetone after filtering.  Not too obvious from the photo, but it didn't appear to be discoloured. The Brown tint is very fine particles which passed through the filter paper (Not lab quality paper.  Just paper from a commercial veg oil filtering system).





I ran methanol through the original Jcloth filter and pretty much the same happened.  I've just been down and checked what ended up in the filter paper after an afternoon of drying and it's like a very fine, still sticky powder binding together.

Don't know if any of that helps?

[Carrington]

Hi Julian

Good job there
Sorry my fault but can you mix the different phase's back again and leave to settle, what I would like to see is the dark pasty stuff settle to the bottom and not dissolve in the bio/acetone mix

Sorry wish I'd had more time in my op to point out what i Was looking for.
I still think its Glyc related from monos.
With regards to the 90/10 test I still think the size of the test solution is relevant to reveal slight amout of monos but this could amount to a reasonable amount of glycerine.

Paul

[Julian]

Hi Julian

Good job there
Sorry my fault but can you mix the different phase's back again and leave to settle, what I would like to see is the dark pasty stuff settle to the bottom and not dissolve in the bio/acetone mix

Sorry wish I'd had more time in my op to point out what i Was looking for.
I still think its Glyc related from monos.
With regards to the 90/10 test I still think the size of the test solution is relevant to reveal slight amout of monos but this could amount to a reasonable amount of glycerine.

Paul

I can scrape or wash with acetone, what's left on the paper back into the beaker, but there's appears to be far less on the filter paper than went into the beaker in the first place.

Would the stuff I washed with methanol still behave as you want?  There's quite a bit of that left.

[Carrington]

I think it would

[Julian]

OK, if there's not enough of the acetone washed stuff, I'll try the methanol washed stuff.

Just so I don't cock up this time ... you want to see the gunk settled out in acetone?

[Carrington]

Yes please
The gunk should settle and the rest should dissolve I'm hoping

[Julian]

There you go ...







The beaker on the left is the remnants from the acetone filtering.  It's rather stuck together, but would separate with agitation.

The right hand one is the gunk washed with methanol.  The photo is a bit misleading as there is a distinctive layer of brown solid at the bottom.  The acetone is slightly more coloured, but don't forget that the very fine particles from the left hand sample were previously washed through the filter paper.

Any the wiser?

[Carrington]

Hi Julian thanks for doing all this.
I still think its Glyc related , just have to get my head round some other stuff andthen look at how we can go about bringing this issue to a definite conclusion

Paul