vodka lab analysis results : I'm pissed

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manu de hanoi
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vodka lab analysis results : I'm pissed

Post by manu de hanoi » Sun Apr 13, 2008 6:34 pm

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 ?

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Post by rad14701 » Sun Apr 13, 2008 7:10 pm

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...

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Post by pintoshine » Sun Apr 13, 2008 7:34 pm

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?

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Post by Dnderhead » Sun Apr 13, 2008 7:55 pm

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

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Post by manu de hanoi » Sun Apr 13, 2008 9:10 pm

pintoshine wrote: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 ?

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Post by Dnderhead » Sun Apr 13, 2008 10:21 pm

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

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Post by Husker » Mon Apr 14, 2008 4:05 am

Dnderhead wrote: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.

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Post by Tater » Mon Apr 14, 2008 5:05 am

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 use a pot still.Sometimes with a thumper

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Post by new_moonshiner » Mon Apr 14, 2008 6:05 am

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.. :D

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Post by pintoshine » Mon Apr 14, 2008 10:30 am

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

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Post by Uncle Remus » Mon Apr 14, 2008 11:06 am

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.
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Post by manu de hanoi » Mon Apr 14, 2008 11:11 am

tater wrote: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 ....

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Post by Dnderhead » Mon Apr 14, 2008 11:48 am

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

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Post by BW Redneck » Mon Apr 14, 2008 11:55 am

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.
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Post by Zman » Mon Apr 14, 2008 2:23 pm

Manu, which laboratory did you send your sample to?

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Post by manu de hanoi » Mon Apr 14, 2008 4:26 pm

Zman wrote:Manu, which laboratory did you send your sample to?
Ministry of Health, Hanoi, Vietnam

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Post by wineo » Mon Apr 14, 2008 7:16 pm

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.

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Post by Centimeter » Mon Apr 14, 2008 9:34 pm

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!

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Re:

Post by manu de hanoi » Thu Apr 17, 2008 7:05 am

Centimeter wrote: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 !

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Re: vodka lab analysis results : I'm pissed

Post by Harry » Thu Apr 17, 2008 11:27 am

manu de hanoi wrote: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.
Slainte!
regards Harry

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Re: vodka lab analysis results : I'm pissed

Post by muckanic » Thu Apr 17, 2008 8:17 pm

manu de hanoi wrote: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.

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Re: vodka lab analysis results : I'm pissed

Post by schnell » Sun May 11, 2008 11:47 am

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 )

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Re:

Post by The Chemist » Mon May 12, 2008 7:11 am

Uncle Remus wrote: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.
Purposeful motion, for one so insane...

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Re: vodka lab analysis results : I'm pissed

Post by schnell » Wed May 14, 2008 2:20 pm

was it a molasses based wash?

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

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Re: vodka lab analysis results : I'm pissed

Post by manu de hanoi » Wed May 14, 2008 10:21 pm

schnell wrote: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

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Re: vodka lab analysis results : I'm pissed

Post by wineo » Thu May 15, 2008 7:40 am

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.

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Re: vodka lab analysis results : I'm pissed

Post by muckanic » Thu May 15, 2008 6:04 pm

schnell wrote: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.

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Re: vodka lab analysis results : I'm pissed

Post by manu de hanoi » Thu May 15, 2008 7:11 pm

wineo wrote: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.

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Re: vodka lab analysis results : I'm pissed

Post by wineo » Thu May 15, 2008 8:32 pm

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.

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Re: vodka lab analysis results : I'm pissed

Post by manu de hanoi » Fri May 16, 2008 2:10 am

wineo wrote: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 ?

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