Testing for impurities?

junkyard dawg · Post by **junkyard dawg** » Tue Feb 21, 2006 8:11 am

So, If a fella wanted to take a sample of hootch to a lab for testing, what would he ask for. I want to know what exactly it is in this bottle...how much ethanol, methanol, esters, aldehydes, pixie dust, and metal salts etc. Anyone ever had their hootch tested like this? I know of a lab I can take it to for GC/MS. I don't really know what to ask for or how to ask for it...

Rocky_Creek · Post by **Rocky_Creek** » Tue Feb 21, 2006 8:31 am

I would think that a comprehensive test would cost you more than a liquor store. Just my thought.

Bujapat · Post by **Bujapat** » Tue Feb 21, 2006 9:07 am

Hello. I found a few months ago an article about "French Cognac Chimic Analysis" at :

http://udppc.asso.fr/bup/844/08440881.pdf

Sorry, it is in french, but on the last page is it a frame with the components that are officially analysed in french Cognac. Maybe it may help you... I rewrote the list of components from the frame. Here they are (in french, sorry, no time to translate) :

Éthanal + acétal
Acétate d’éthyle (piqué)
Butyrate d’éthyle (putride)
Butanol-1
Butanol-2
Hexanol
TDN (hydrocarbure)
Lactate d’éthyle
Alcool allylique
Isobutanal

The Chemist · Post by **The Chemist** » Tue Feb 21, 2006 9:49 am

A one-off sample is going to cost a lot more that you probably want to pay. If this is a commercial lab, not a buddy that works in one, that is. If you've got a buddy in a lab with GC/MS, he could give you an idea of the approximate amounts of all the major components pretty easily. If it's a commercial lab, they will have to develop a method to quantitatively analyse the sample. There is also some sample preparation needed. The article Bujapat linked has a good list for GC/MS, it's the one right before the last one. For metel salts, you would need a lab with atomic absorption spectroscopy.

Post by **golden pond** » Tue Feb 21, 2006 9:51 am

I've always been curious myself to know just how pure my product is compared to store bought. I'd guess the distilleries have a way of checking their own.

canadianmoonshiner · Post by **canadianmoonshiner** » Wed Feb 22, 2006 12:15 am

golden pond wrote:I've always been curious myself to know just how pure my product is compared to store bought. I'd guess the distilleries have a way of checking their own.

I'll bet anything they send out samples to a lab. If you got caught by the IRS (or equivalent gov't agency) I'm sure they'd be more than happy to test it for you.

Post by **golden pond** » Wed Feb 22, 2006 4:59 am

The Chemist wrote:A one-off sample is going to cost a lot more that you probably want to pay. If this is a commercial lab, not a buddy that works in one, that is. If you've got a buddy in a lab with GC/MS, he could give you an idea of the approximate amounts of all the major components pretty easily. If it's a commercial lab, they will have to develop a method to quantitatively analyse the sample. There is also some sample preparation needed. The article Bujapat linked has a good list for GC/MS, it's the one right before the last one. For metel salts, you would need a lab with atomic absorption spectroscopy.

Chemist, can you enlighten us some more in lay-men's terms, I can't read French

I have two customers that have their own in-house labs, I may run it by them one of these days. Yep Canadianmoonshinner, I'd say your'er right also.

stoker · Post by **stoker** » Wed Feb 22, 2006 5:34 am

golden pond wrote: I have two customers that have their own in-house labs,

i don't think a house lab has GC/MS

chemist, where did you read anything about metal salts? are there even any present in distillede spirit ( next to a few coppersalts?)

Post by **golden pond** » Wed Feb 22, 2006 5:43 am

stoker wrote:
golden pond wrote: I have two customers that have their own in-house labs,
i don't think a house lab has GC/MS

Stoker, I think you misunderstood, in-house means they have their own lab and chemist, they don't have send samples off to an independent lab. By the way, what is GC/MS??

The Chemist · Post by **The Chemist** » Wed Feb 22, 2006 6:31 am

GC/MS is gas chromatography (which seperates the components of a mixture) using a mass spectrometer (which identifies specific compounds based on the mass of the ions produced when the compound is blasted to pieces by an ion beam) as a detector. It's a very powerful (and expensive) tool. The trouble with analyzing alcoholic beverages is the multitude of compounds at very low levels in a very "difficult" matrix. To get a signal for the compounds of interest, you must concentrate them, and remove a lot of the ethanol. I extract with dichloromethane. To get quantitative result, you have to make a standard curve of the response of the instrument to known concentrations of the compounds you want to measure. This is the "bulk" of the work, and what would cost the most, in time and therefore money, in a commercial lab. As I said, though, if you just want a general idea of the amounts, GC/MS will give you that quickly and pretty cheaply.

Junkyard asked about metal salts. That's quick and easy with AA, but as you mention, stoker, it's not really of much concern in a distillate. Barrel aging will add some salts, but testing for salts is usually done just to be sure there is no contamination in an industrial setting. Home guys probably have nothing to worry about.

stoker · Post by **stoker** » Wed Feb 22, 2006 9:50 am

golden pond wrote:
stoker wrote:
golden pond wrote: I have two customers that have their own in-house labs,
i don't think a house lab has GC/MS
Stoker, I think you misunderstood, in-house means they have their own lab and chemist, they don't have send samples off to an independent lab. By the way, what is GC/MS??

Code: Select all

                         ~communication error~

Bujapat · Post by **Bujapat** » Wed Feb 22, 2006 9:50 am

I don't have large knowledge in chemistry, but like The Chemist wrote, the Cognac analysis consist in two operations:
1- micro distillation to get 72%ABV alcohol
2- gaz chromatography

The result is in the chart in mg/liter exponent-1 for the components listed in my precedent post.

canadianmoonshiner · Post by **canadianmoonshiner** » Thu Feb 23, 2006 12:08 am

The Chemist wrote:GC/MS is gas chromatography (which seperates the components of a mixture) using a mass spectrometer (which identifies specific compounds based on the mass of the ions produced when the compound is blasted to pieces by an ion beam) as a detector. It's a very powerful (and expensive) tool. The trouble with analyzing alcoholic beverages is the multitude of compounds at very low levels in a very "difficult" matrix. To get a signal for the compounds of interest, you must concentrate them, and remove a lot of the ethanol. I extract with dichloromethane. To get quantitative result, you have to make a standard curve of the response of the instrument to known concentrations of the compounds you want to measure. This is the "bulk" of the work, and what would cost the most, in time and therefore money, in a commercial lab. As I said, though, if you just want a general idea of the amounts, GC/MS will give you that quickly and pretty cheaply.

Junkyard asked about metal salts. That's quick and easy with AA, but as you mention, stoker, it's not really of much concern in a distillate. Barrel aging will add some salts, but testing for salts is usually done just to be sure there is no contamination in an industrial setting. Home guys probably have nothing to worry about.

So to find out what is in your hooch, you need a list of suspects, and known samples of what you are looking for. Just like a single fingerprint is useless without a match. I've read & believe that our senses can detect volatile compounds much better than analytical means, so if you can't smell it, it's not there. If you can smell it, it is there but you can't be sure how much, in terms of ppm (or ppb).

Ricky · Post by **Ricky** » Thu Feb 23, 2006 3:28 am

Golden Pond, in response to your curiosity you would probably rather not know what is in commercial hooch. i was in the company of a chemist who works for a major university and the same subject came up. granted we were all a little under the influence , but i do remember that there were things in jim beam that made me squirm at the mention of them. i hope to get a sample to him one day to satisfy my on curiosity myself. but only if he can sneek it in the back door. like chemist had said, i bet the fee would be more than enough to settle my curiosity. if i ever get around to this i will be sure to post the results, good or bad.
Happy Drinking,
Ricky

Post by **golden pond** » Thu Feb 23, 2006 5:24 am

Yep Ricky, I've heard them tales before also. Someone else on the forums had some of their granddad's tested and it also was much more pure than commercial. My liquor has no after taste what so ever and knock on wood I've not had or anyone else that drinks it has had a hang over from it yet. I take great pains in keeping everything clean, mash barrel washed out before each use, I ferment in open air but have my mash barrel covered with a fine SS screen, still is washed out before use and all collecting containers and test equipment is washed also. I quit collecting at about 75 proof, although I run singles down to about 40 for the next run. When I'm done with all my runs, I then double run and double run to no lower than 150 proof, the rest hits the ground. My liquor is always filtered atleast 3 times. Corn and sugar is cheap so why cut corners.

The Chemist · Post by **The Chemist** » Thu Feb 23, 2006 6:10 am

canadianmoonshiner wrote:
So to find out what is in your hooch, you need a list of suspects, and known samples of what you are looking for. Just like a single fingerprint is useless without a match. I've read & believe that our senses can detect volatile compounds much better than analytical means, so if you can't smell it, it's not there. If you can smell it, it is there but you can't be sure how much, in terms of ppm (or ppb).

Mass spectrometry, by it's nature, will give you the "list of suspects". But, yes, to get quantitative results, you have to have the known samples. In an aged Bourbon, this can run into the several hundreds. And it's true that many of these compounds have only been detected after serious concentration--like concentrating 20 liters (~5 gal) down to half a milliliter. I'm generally only concerned with about twenty compounds, the major ones being: Acetaldehyde, Ethyl Acetate, Methanol, Ethyl Formate, iso-butyl alcohol, iso-butyl acetate, iso-amyl alcohol, iso-amyl acetate, phenethyl alcohol, phenethyl acetate, acetic acid, furfural, the ethyl esters of capric, caproic, and caprylic acids, vanillin, syringaldehyde, and a few others that I shouldn't talk about

. There are other "custom" features that I look for in particular distillates/types--like ethyl laurate in Scotch etc. And, yes, most of these things will kill you if you drink them, but they are in such low concentrations in booze, it's okay. Like we always say, the alcohol will get you first!!