Bench still for Proofing

[George A]

Hi there. My name is George and I have a start up alcohol company. We are blending GNS with our own mixture of spices, but I don't really have the expertise to set up a bench still for proofing. I also might need help choosing equipment such as pumps, hoses, flow meters, etc. I am located in Los Angeles.

Does anyone know of a person or company that could tell me exactly what I need and exactly what I need to do to make sure I'm right on with the TTB. I already know that Anton Paar makes the best equipment, but as you all know, the equipment wont work directly on the product because of the sugar in it.

Any advice would be greatly appreciated. Thank you.

[Gwydion Stone]

What are you making? Why would you need a still for proofing?

Regarding TTB compliance, you should start by reading the full Beverage Alcohol Manual for distilled spirits, and if you don't have a DSP yet, download and read the DSP permit packet.

[will]

George,

Anton-Paar also sells another gizmo that works with the alcohol meter thing to tell you the % alcohol of a liqueur. it doubles the price.

The procedure is mentioned in 30.31 et seq of the Gauging Manual

In 30.31©(1) they're prescribing a procedure similar to 30.32© which basically says that if you distill a sample of known quantity and temperature in a lab still until the kettle side contains nothing but a small bubbly mass (the sugar), then all the alcohol is in the distillate from the sample. Now, if you add pure water to the distillate until the volume and temperature are the same as what you started with, then you have replaced the sugar with water, and now the proof of the distillate can be measured in the normal manner. Restoring the distillate temperature to the original temperature is important because you can't know the actual volume accurately at any other temperature, so a water bath is generally required for this test as well as a simple bench still. Once you get accustomed to doing these "burnoffs" you'll use them for anything that contains stuff other than common alcohol. The burnoff method is also valid for quantities of sugar less than 6g/L.

Compliance with all laws and regulations is required, and those that are alcohol specific are HERE.

Good luck,

Will

[porter]

It's good to see another individual starting in the alcohol business, and best wishes to succeed.

However, this is another glaring example of why there should be a distinction in both licensing and labeling between 'blenders' and those who are actually distilling a product. Again, nothing wrong with what 'George A' is starting out his business as, it's just that his business doesn't really qualify as a distillery in any practical sense, other than by old-testament governmental standards.

Products which end with over 51% NGS not from the company's own distillery need to be labeled something to the effect of a mixed or blended product. There seems to be a big stink over the large firms stretching what sugars they use to ferment with, where's the voices on this blending issue?

Sorry for the thread snagging........but it is relevent.

[Kristian]

I use this for "obscuration" or proofing for tax my liqueurs. http://www.pelletlab.com/distillation_equipment, fill it with 250mL, distill it to almost nothing and then add water til its back to 250mL. Then read temp, hydrometer, weight, etc. for your tax records.

[daveflintstone]

Sorry for the thread snagging........but it is relevent.

no it's not

And there is already a distinction in TTB licensing between rectifiers and distillers, it's on the license and the bond requirements.

Anyway, I have a similar lab still to what Kristian linked to, and it does the job.

[Carlos]

George:

Regarding the benchtop still for proofing, you need to look at the AOAC method, which has listed all the materials you need. (AOAC Official Methods of Analysis 920.47, 942.06, 945.07,

982.10, 983.12 (17th Ed.); ASBC Official Method Beer-4; 27CFR part 30), but basically you need a glass distillation equipment as follows:

Boiling flask with 35/20 joint

Vigreaux distilling column with 35/20 joints, 50cm long and 2.2cm od

Connectig adapter with 35/20 joints

Liebig condenser with 35/20 female joint on top and straight 7mm od tube as outlet (H20 jacket lenght ca 38cm)

Conderser outlet connector tube

Pinch-type clamps

volumetric flasks

You will obviously need a heat source (electric heater) for the distillation.

Now, depending on the method you use for the density measurement, you might need to have to size the flasks differently (if you are going to use hydrometers you need bigger volume than the Anton Paar DMA or the pycnometer). Also, depending on your equipment availability and method chosen you will need either a 20°C water bath or a scale sensitive to ±0.1mg

Please feel free to contact me if you need more info

Carlos

[George A]

I use this for "obscuration" or proofing for tax my liqueurs. http://www.pelletlab.com/distillation_equipment, fill it with 250mL, distill it to almost nothing and then add water til its back to 250mL. Then read temp, hydrometer, weight, etc. for your tax records.

Thank you Kristian. This info is helpful. Have a great day!

[George A]

George:

Regarding the benchtop still for proofing, you need to look at the AOAC method, which has listed all the materials you need. (AOAC Official Methods of Analysis 920.47, 942.06, 945.07,

982.10, 983.12 (17th Ed.); ASBC Official Method Beer-4; 27CFR part 30), but basically you need a glass distillation equipment as follows:

Boiling flask with 35/20 joint

Vigreaux distilling column with 35/20 joints, 50cm long and 2.2cm od

Connectig adapter with 35/20 joints

Liebig condenser with 35/20 female joint on top and straight 7mm od tube as outlet (H20 jacket lenght ca 38cm)

Conderser outlet connector tube

Pinch-type clamps

volumetric flasks

You will obviously need a heat source (electric heater) for the distillation.

Now, depending on the method you use for the density measurement, you might need to have to size the flasks differently (if you are going to use hydrometers you need bigger volume than the Anton Paar DMA or the pycnometer). Also, depending on your equipment availability and method chosen you will need either a 20°C water bath or a scale sensitive to ±0.1mg

Please feel free to contact me if you need more info

Carlos

Carlos, Thank you for such detailed and relevant information. If you don't mind, I might like to speak with you on the phone regarding set up. I do plan on getting the Anton Paar DMA. I appreciate the help.

Regards,

George

[Gwydion Stone]

... there is already a distinction in TTB licensing between rectifiers and distillers, it's on the license and the bond requirements.

But it's not on the label, and that's pretty much all the consumer gets to see. As we know there are examples of folks calling themselves distillers when they're only rectifiers or blenders, and language is easily used to manipulate the consumer's impression of the product.

... this is another glaring example of why there should be a distinction in both licensing and labeling between 'blenders' and those who are actually distilling a product. ... his business doesn't really qualify as a distillery...

To his credit, he never called it a distillery, so it's not a glaring example of that at all. And as you said: "nothing wrong with what 'George A' is starting out his business as", so I'd have to say that I agree with daveflintstone on this one. It's not relevant to this particular thread.

[will]

Our little stills came from United Glass Technologies

We got a whole bunch of stuff, but the 89501-005 is pretty close to what we use. Everyone should have one of these.

Good luck,

Will

[ryankf]

On 4/18/2011 at 9:36 AM, Carlos said:

"...20°C water bath..."

Hi Carlos, any tips on where to source some of this lab equipment, especially the water bath.

Cheers,

Ryan

[Silk City Distillers]

Lab equipment and glassware?

Depends what you want to pay.

If you are feeling like the CFO of a billion dollar global pharmaceutical company, go to Fisher Scientific and pay $700 for a water bath.

If paying $700 for a water bath seems insulting to you, check the lab surplus companies who sell on eBay, and you can probably get the same one, used, for 1/4 of the price.

[Silk City Distillers]

For example, nice smaller Cole Parmer water bath, perfectly suitable - $655

https://www.coleparmer.com/i/economical-poly-bath-5-5-liters-110v-60-hz/3906410

Looks like the same one, brand new, surplus on ebay - $79.00 + Shipping.

http://www.ebay.com/itm/Cole-Parmer-39064-10-115V-5-5L-Cap-Utility-Water-Bath-/232206538959?epid=2136105879&hash=item36109698cf:g:ZDsAAOSwq1JZJaTd

Bet if you offered this guy $60 for it ($100 shipped) - he'd take it.

Saved you $500.  I take payment in beer.

[ryankf]

Thanks Silk City, hadn't considered looking on the used market. I'll check it out. Ultimately would be nice to have a reliable manageably priced vendor to work with.

[Silk City Distillers]

That's a killer deal actually, so if you aren't going to buy it, I'm going to buy it to have a spare.

[ryankf]

It is a great deal. My next question is if it's min. temp setting is ambient temp how does one get a sample to 20C?

[Silk City Distillers]

Turn down the air conditioning in your lab?

You can fill the bath with cool water and slightly cool the sample to start.  However, you are correct, the longer you wait the greater the chance the sample temp starts increasing.

Refrigerated baths are very very expensive and you generally wouldn't go to all that trouble here.

 

[ryankf]

Makes me wonder what most "small" distillers who don't have full labs do with products that contain over 600mg/100ml solids. Send to outside labs? But then how does one reproduce...or hit a COLA approved proof. Just trying to wrap my head around this before I venture down a path to a liqueur or schnapps, etc.

[George A]

Hi Ryan,

I posted the original thread on this topic.  You can reach out to me with any and all questions re: getting started in the alcohol biz.  george@evolspirits.com

[JustAndy]

22 hours ago, Silk City Distillers said:

For example, nice smaller Cole Parmer water bath, perfectly suitable - $655

https://www.coleparmer.com/i/economical-poly-bath-5-5-liters-110v-60-hz/3906410

Looks like the same one, brand new, surplus on ebay - $79.00 + Shipping.

http://www.ebay.com/itm/Cole-Parmer-39064-10-115V-5-5L-Cap-Utility-Water-Bath-/232206538959?epid=2136105879&hash=item36109698cf:g:ZDsAAOSwq1JZJaTd

Bet if you offered this guy $60 for it ($100 shipped) - he'd take it.

Saved you $500.  I take payment in beer.

I would think the Max Temp of 90C would prevent you from distilling a proofing sample to completion?  We also use the pellet labs still for proofing tests (https://www.pelletlab.com/distillation_equipment) 

[Silk City Distillers]

No no, talking about adjusting sample temperatures for measurement.  Not using the bath as a Bain Marie for distillation.

If it's any help, I've found that it's easier to just distill in an erlenmeyer on a hot plate.  I've got a ton of heated stir plates for yeast propagation that work just fine.

 

[Silk City Distillers]

That and if I tried to use of spherical boiling flask, I'd just end up rolling it off my table or spilling it at the least.

[JustAndy]

Ah I see, my mistake, I've never needed to heat up a sample (only cool down) so it didn't occur to me. When I was originally looking for a proofing still I wasn't able to find a condenser that was the right shape and connection to use with an erlenmeyer flask without a bunch of adapters which made the pellet lab setup cheaper for me. 

[Pachasius]

On 29-8-2017 at 7:55 PM, Silk City Distillers said:

Turn down the air conditioning in your lab?

You can fill the bath with cool water and slightly cool the sample to start.  However, you are correct, the longer you wait the greater the chance the sample temp starts increasing.

Refrigerated baths are very very expensive and you generally wouldn't go to all that trouble here.

 

Wouldn't it also be an option to put all your samples on, lets say, 30 degrees Celsius to measure a volume prior to distillation. And also do the topping up with H20 after distillation at 30 degrees Celsius?