vodka lab analysis results : I'm pissed

[manu de hanoi]

got the results from the lab today for my vodka :

acid (acid acetic equivalent ) :6 mg/L
Ester: 220 mg/L Max limit allowed : 200
Ethanol: 38,2 %ABV
Aldehydes: 188 mg/L Max allowed : 50
Methanol :0,03 mg/L Max allowed : 0,1
Propanol:204 mg/L
isobutanol: 481 mg/L
isoamylic: 1154 mg/L
furfurol: 5 mg/L (they say it's too much only "traces" allowed)

Conclusion : Does not pass
The samples were stored in plastic bottles (used for spring water) for 6 days before testing. Any idea of wether this could influence which result ?

For Ester I could remove it by adding NaOH just before distill, for aldehydes it seems I do have heads even though i though I didnt.

Any of you guys ever had your booze analyzed ?

[rad14701]

Some newer spring water bottles are designed to bio-degrade fast and probably even faster when introduced to high ABV ethanol... You may have seen a warning on the bottle stating "Do Not Refill", or something along those lines... Some bottles can break down in as little as just over a month when not filled with water... The absence of water actually triggers the break-down process...

[pintoshine]

Allow me to use your analysis as a medium to stir the pot. I bet you tossed the foreshots and still your methanol was above the tolerance? Hmmmm...

Seriously though. Was this a single run vodka or multiple distillations?

[Dnderhead]

RE read that Pint that was not methanol aldehydes/esters
Theo I'm not a scientist

[manu de hanoi]

Allow me to use your analysis as a medium to stir the pot. I bet you tossed the foreshots and still your methanol was above the tolerance? Hmmmm...

Seriously though. Was this a single run vodka or multiple distillations?

it's a single run vodka on a continuous still. The methanol is ok but not the other heads. Anyone has an idea of what is an acceptable level of furfurol ?

[Dnderhead]

Curiosity Is killing me how do you remove heads with a continues
still? since you have "new" wash all the time?

[Husker]

Curiosity Is killing me how do you remove heads with a continues
still? since you have "new" wash all the time?

Some commercials running continuous stills, take off at a plate below the top "head" plate (they are using "real" bubble plate columns). However, as Manu is seeing, most anything taken off a continuous is contaminated, to a certain level.

I can not drink commercial spirits any more. Get a hell of a head ache after about the level of 2 shots, and if I drink more, the headache just gets worse. My body has just become acclimated to "properly" distilled spirits, and I hope to NEVER have to go back to commercial mass produced swill again.

I can tolerate most commercial vodkas (not rotgut), and most commercial gins, without a headache. However, I think that is just due to they spend a whole lot more effort cleaning things up, thus removing almost all of the offal from the end product.

H.

[Tater]

Manu de hanoi meaning no disrespect what so ever Ive got to say this.Of all my time being on and reading distilling forums you are the first Ive heard of to do what many newbies ask.How do I make likker like the big boys. Looks like ya got it figured out.

[new_moonshiner]

I wonder how those test results compare with off the shelf products.. I bet we would be surprised ...Sure would be nice to have access to a lab..

[pintoshine]

you are correct I mis read the methanol numbers. My apologies.

[Uncle Remus]

I would bet if you took the same spirit you got tested and run it through a reflux or even a pot still for that matter and did a proper head and tails cut it would pass with flying colours.

A couple years ago when Golden Pond was still with us, he showed me an analysis of his corn whiskey. It was double distilled in a big pot still. In every category tested, and I believe there were about 30 different things, his sample below half the acceptable level in all areas. He was pleased as punch with the results.

[manu de hanoi]

Manu de hanoi meaning no disrespect what so ever Ive got to say this.Of all my time being on and reading distilling forums you are the first Ive heard of to do what many newbies ask.How do I make likker like the big boys. Looks like ya got it figured out.

I dont make likker like the big boys, my tower is only 2,5 meters high and this isnt enough to do continuous heads removals. Big boys also do continuous tails removal which i dont. A lot of work ahead ....

[Dnderhead]

If you do not take " heads-tails" off continuously then how is it a continuous still ? from my understanding a continuous still you replace
wash as it is used . in theory never stopping to empty/refill

[BW Redneck]

If I had a continuous still, I would use it to do a primary distillation, then take what I would get get from that and run it through a batch setup. It would probably pass all of the tests possible.

[Zman]

Manu, which laboratory did you send your sample to?

[manu de hanoi]

Manu, which laboratory did you send your sample to?

Ministry of Health, Hanoi, Vietnam

[wineo]

Ive had real good results potstilling mine,and making a large forshot cut of 200mls,and doing cuts on every run.If I do a 2nd run it just gets better.
I havent had it tested,but you can drink a ton of it and have no hangover of any kind the next day.

[Centimeter]

This is a very interesting subject for me! I work in a mass spectrometry lab and it would be oh so easy for me to run some hooch on the gas chromatography mass spec. That'll tell me what's in my whisky down to the femtomole!

Zman, if you're looking for a place to have your distillate tested, definitely try emailing the chemistry department at your local university. Any proper lab will have access to a GCMS.

This hobby just keeps getting better and better!

[manu de hanoi]

This is a very interesting subject for me! I work in a mass spectrometry lab and it would be oh so easy for me to run some hooch on the gas chromatography mass spec. That'll tell me what's in my whisky down to the femtomole!

Zman, if you're looking for a place to have your distillate tested, definitely try emailing the chemistry department at your local university. Any proper lab will have access to a GCMS.

This hobby just keeps getting better and better!

Please send your result and let's see who's got a bigger shlong !
Harry is setting up a distillery , he should have to go through that too !

[Harry]

Harry is setting up a distillery , he should have to go through that too !

Not guilty, Manu. Like I said in my email to you. Strictly amateur & hobbyist. Pro takes all the fun out of it.

But I can give you a few pointers.

1. What you have in your continuous setup is essentially a stripper. In industry it's called the "Analyser". It's column number one (1) of a multi-column rig. You need to take the product from that (as vapour) and run it through a second stage, sometimes even a third stage column, known as the "rectifier". Essentially this stage is a re-distillation stage, steam driven. As has been mentioned already in this thread, you can achieve the same result by taking your "Analyser" output as 'liquid', cut it to 30% a/v with demineralised or distilled water and re-distil in either a pot still or better yet a good reflux column such as we use in the hobby. This is where you do your heads/tails cuts.

2. Furfural: This is mainly due to pyrolysis or 'burning' of proteins and unconverted starches compounds (think 'burnt whiskey'). It is always found in whisk(e)ys, particularly Scotch Malts. A second source of furfurals is from the thermal degradation (charring) of wood in barrel aging. If you go by the regulations for vodka of it being essentially a 'neutral' spirit devoid of all congeners (basically ethanol & water), then barrel aging and pyrolytic congeners are not supposed to be in a vodka at all.
Therefore you need to improve your wash filtering (remove all solids) and improve your starch conversion (if that is your substrate source) so that distilling heat does not create furfurals or other pyrolytics.

I do not have an analysis for vodka (it wouldn't show much of anything anyway), but I can give you an analysis for Scotch Whisky to show what congeners are present in their malts. That may give you an idea of some of the things you may have to look out for and remove from your vodka.

Typical malt distillery analyses
(in grams per 100 litre absolute alcohol)

Component Speyside Islay

Acetaldehyde 5.4 7.0
Ethyl acetate 26.3 33.2
Diacetyl 2.1 2.8
Methanol 4.8 9.0
Propanol 40.3 37.6
Isobutanol 80.1 85.6
o.a. Amyl alcohol 44.2 53.1
Iso-amyl alcohol 138.9 170.8
Total higher alcohols 303.5 347.1
Ethyl acetate 3.7 5.3
Ethyl octanoate 1.8 2.7
Furfural 3.6 4.8
Ethyl decanoate 6.0 8.9
b-Phenethyl alcohol 7.2 8.7
Ethyl myristate 0.9 1.2
Ethyl palmitate 2.8 3.3
Ethyl palmitoleate 1.6 2.1
Phenols 1.0 4.5


Hope this is useful.

[muckanic]

for aldehydes it seems I do have heads even though i though I didnt.

The lab isn't necessarily saying the aldehydes are low boiling. These can come from ingredients (eg, apples), fermentation technique (eg, brewer's yeast + fructose), and ageing (namely, oxidation - also applies to acids). Acetaldehyde could also in principle form an azeotrope with something in the tails, which could bring it into the hearts fraction. Lipids presumably also kick up the fatty acid quotient, eg, through running the grains and/or yeast. This last point obviously isn't so relevant to vodka, although it could be interesting to compare whole grain-based recipes with refined grains with potatoes. One thing that occurs is that alkali treatment possibly does more than just eliminate esters, which is the usual justification. It presumably also forms non-volatile carboxylate salts with any fatty acids, thus reducing the lipid content, a major constituent of essential oils.

[schnell]

One thing that occurs is that alkali treatment possibly does more than just eliminate esters, which is the usual justification. It presumably also forms non-volatile carboxylate salts with any fatty acids, thus reducing the lipid content

indeed it does. and this drags the equilibrium toward further hydrolysis of the esters.

most esters exist in an equilibrium with their carboxylic acids. salting out the acids effectively removes it from the equation, with the resulting equilibrium shift. so not only are there less esters, but there's less capacity to make more of them after the alkali treatment.

i doubt many fatty acids are volatile enough to evaporate without esterification by an alcohol. which a still usually has in abundance. esters that distill into the receiver flask then re-equilibrate by hydrolysis ( ester <=> acid + alcohol )

[The Chemist]

A couple years ago when Golden Pond was still with us, he showed me an analysis of his corn whiskey. It was double distilled in a big pot still. In every category tested, and I believe there were about 30 different things, his sample below half the acceptable level in all areas. He was pleased as punch with the results.

Unless GP was 'cheating on me', I did this analysis. If so, though I don't have the data in front of me at this moment, as I recall, the sample was entirely acceptable in all respects. That means that the things you didn't want were low enough to "pass", and the things you did want fell within and accpetable range.

The gentleman made some fine hooch, God rest him.

[schnell]

was it a molasses based wash?

if i remember correctly the furfural comes from pentosans which are abundant in cane.

[manu de hanoi]

was it a molasses based wash?

if i remember correctly the furfural comes from pentosans which are abundant in cane.

it was a cassava wash

[wineo]

I bet if you throw out the first 750mls that comes off,most of the bad stuff would be gone,and it would pass the test.

[muckanic]

i doubt many fatty acids are volatile enough to evaporate without esterification by an alcohol. which a still usually has in abundance. esters that distill into the receiver flask then re-equilibrate by hydrolysis ( ester <=> acid + alcohol )

As far as I am aware, most esterification is enzyme-catalysed by the yeast. It would take a big heap of reactants and a relatively small amount of water for this to occur in the still. I guess these conditions might exist at the start of the run in the gas phase, but that of course requires volatile acids. Vinegar is clearly volatile in the sub 95C range, so I would imagine some of the lower molecular weight fatty acids also should be. IIRC, one of the justifications for running the lees in brandy making is to rupture the yeast cells and get the fatty acid quotient up.

[manu de hanoi]

I bet if you throw out the first 750mls that comes off,most of the bad stuff would be gone,and it would pass the test.

I tried a second run like that but this still seems to be not enough.
I read that continuous rectification is much more efficient than the traditional one, I modified the continuous still to allow for that, and should redistill with continuous heads & tails removal in the next 3 days.

[wineo]

It would also help if the wash is cleared,and most of the yeast is gone before running it.Yeast in the boiler produces esters,so you would loose some if you cleared it first.

[manu de hanoi]

It would also help if the wash is cleared,and most of the yeast is gone before running it.Yeast in the boiler produces esters,so you would loose some if you cleared it first.

I neutralise before i still, should I go basic ?