Methanol testing, recovered methanol, purity, and process?

[julianf]

My spirit hydrometer has just turned up. 

Its calibrated to ethanol at 20c.

The 'virgin' meth i just tested came out at 99% at around 15c ish (outside temp). 

I have confidence that the sample tested was close to pure (ie 99.99%), so i would assume that the 1% deviation is due to equipment, calibration, temperature etc.


I then tested a sample of reclaimed, and that read 96% on the scale.  Under my assumption that the previous 1% deviation is due to equipment calibration, rather than an impure reference sample, this would give a purity on the reclaimed to be between 96% and 97%.  Ie probably 3% water.


Im now wondering which stage of the 2stage process to use the reclaimed in.

In S1, there are loads of other 'unknowns' anyhow.  Also the reclaimed will never be the total amount on S1 (due to the reclaimed total from the last batch never being as large as the S1 dose) - however, at present i have a load of reclaimed, and very little virgin.


When do you use your reclaimed?

[Tony]

I've used reclaimed that was 96% before.  Made the methoxide up with virgin meth, put that in and let it process a bit, then added the reclaimed working on the assumption that the glyc created in the initial part of the reaction would help with the water.

[Tony]

If you want to check the graduations are the expected distance apart on your hydrometer, a 100ml measuring cylinder is good for this.  Put in 100ml Meth, pop in the hydrometer, add 1ml of water - should float up by 1%.

My ethanol hydrometer (which goes up to 99%) sinks entirely when put into virgin Meth, though it bobs up if 1ml water is added.  So if I'm testing reclaimed and I see it sink, then I'm happy it's good to re-use without worry.

[julianf]

Interestingly (for me) ive just fount the correction chart for my hydrometer.

As mentioned, its calibrated at 20c.  I was testing at more like 15c.  The chart states that, at 85%+, at 15c, 1% should be added to the read out.  Which, specific density errors between ethanol and methanol aside, would tie in with the 99% reading that i got from my 'virgin' sample.

I would therefore be happy to assume my recovered to be 97%, however, when im feeling keen, i will do as you say, and test by adding water to a 100% sample.

[Jamesrl]

I get a regular 98% reading on my Spirit Hydrometer for reclaimed methanol.

I use the reclaimed in stage 1, ASM first, reclaimed and top up with virgin to required volume.

I prefer to use virgin for stage 2.

I once used reclaimed methanol for stage 2 that was distilled off of stage 1, I was very short of methanol at the time and it worked a treat. 

[nigelb]

I then tested a sample of reclaimed, and that read 96% on the scale.  Under my assumption that the previous 1% deviation is due to equipment calibration, rather than an impure reference sample, this would give a purity on the reclaimed to be between 96% and 97%.  ie probably 3% water.

That would probably be right for your reclaimed Julianf....so long as you've generated it yourself.

A word of warning though for people who buy reclaimed methanol is any impurity could be anything and should not be assumed as being water. Reclaimed methanol is recovered from all sorts of chemical processes.

[thewormman]

Take the water out? If its just water in it use a molecular sieve

Explanation of them here

http://www.bio.umass.edu/microscopy/mol_sieves.htm

Have got the molecular seive just got to buy the hydrometer and try it when I get a chance

[Tony]

Recovered meth is often polluted with FAME , I'm guessing that won't do a molecular sieve much good?

[thewormman]

Recovered meth is often polluted with FAME , I'm guessing that won't do a molecular sieve much good?

Don't know will find out  Was going to wash after use in IPA they are made of ceramic I believe

Need to get a hydrometer could you recommend a source? Seen them on eBay but could I get one locally from a wine making suppliers or something? What size am I looking for?
Anyone got a link?

Ta very much 

[julianf]

1 x Stevenson Reeves Spirit Hydrometer / Alkohometer 0-100% (alchometer) = £4.29
1 x Glass Trial Jar (glass trial jar) = £5.75
------------------------------------------------------
Sub-Total: £10.04
Shipping: £2.00
Total: £12.04

 http://www.balliihoo.co.uk


The trial jar is cheaper than getting one off ebay, however, its base is small, so its not that stable.
If that's a problem for you, there's one on ebay that i was otherwise going to buy - i can look up the item number for you later.

[nigelb]

You have a pm..........message me back and I may have a solution to your problems.....

[nigelb]

Just so that Nathan can read this......y hv..........mssg m bck nd my hv   sltn t yr prblms

[kamaangir]

Nige you spelt "Your" worng its UR as opposed to YR

[thewormman]

1 x Stevenson Reeves Spirit Hydrometer / Alkohometer 0-100% (alchometer) = £4.29
1 x Glass Trial Jar (glass trial jar) = £5.75
------------------------------------------------------
Sub-Total: £10.04
Shipping: £2.00
Total: £12.04

 http://www.balliihoo.co.uk


The trial jar is cheaper than getting one off ebay, however, its base is small, so its not that stable.
If that's a problem for you, there's one on ebay that i was otherwise going to buy - i can look up the item number for you later.

Thanks for that 

[nigelb]

Nige you spelt "Your" worng its UR as opposed to YR

just goes to show how old I am....I'm just not down with the kidz