SCLabGuy

@dwa336 There is an Anton Paar DMA 4500 M w/ refractometer for sale here: 

Not cheap...!

You could also use a thermowell to ensure only stainless comes into contact with product.

Unless it says specifically that all the materials are compatible with high proof / pure ethanol, it is safe to assume that it is not intended for the use case you are proposing.  I'd wager that you'll taste the plastic, and sooner rather than later, too.

Grain. Includes cereal grains and the seeds of the pseudocereals amaranth, buckwheat, and quinoa.

https://www.ttb.gov/press/press-release-fy-22-5

Seconding: AODD pump (self prime & run dry) and lots of valves....valves everywhere.  

22 hours ago, PeteB said:

I see your proposed regulations won't allow purchased wash. 

Are you sure?  The mash must be produced in the US (one proposed arm of the reg) and it must be distilled all in the same US distillery (another proposed arm).  These two arms would not preclude the use of purchased domestic beer, by my reading.

In a perfect world?  Money is no object?

Copper bus bar throughout areas where you will store or process spirits.  Permanent bonding of stationary tanks, pumps, scales, and tubing.   At intervals, attach clamp-style coiled wires: https://www.grainger.com/product/9WN83  Use these clamps on drums, totes, barrels, and portable pumps, bottle fillers/lines, etc.  What I've just described can easily be thousands of dollars of hardware...

It is common practice.  It can be hard to achieve the flavor density that is typical of a distilled gin, though.

I also know of operators who misused citric with disastrous consequences. Seems like it's usually coming from wine production. It's like I always say. "different things are different." 

Whatever I could scrounge up on Craigslist. I have a Beckman unit I like but quite a few brands make serviceable units. Thermo maybe? I look for a 5A+ compressor on the cooling side. 

I've also cobbled together something workable using a simple compressor-type chiller, pump & sous vide circulator wand in a plastic storage bin. You're heating and cooling and circulating all at once, which works surprisingly well, but isn't particularly energy efficient. Note that lab chillers will also heat and cool simultaneously to maintain temp. 

Good questions, all.  I have sent you a PM.

8 hours ago, Brewstilla said:

Does citric actually remove a layer of copper? Doesn't citric react with and dissolve copper oxide, not the copper itself, leaving the solution a blue color?

I'm sure someone with more chemistry knowledge will chime in here but copper oxide is composed of copper - right?  It stands to reason that you are losing some pure copper to form the copper oxide layer.  So when you blow away that layer, more copper will end up consumed in creating the next oxide layer.

5 hours ago, adamOVD said:

@SlickFloss Why not PBW? I feel like it cleans proteins as well as caustic.

PBW is a caustic.

Yes, you need a water bath to get your sample to a target temp before & after distillation. 

I tried using a cheap heat-only bath, set for a couple degrees above ambient. I had measurable ethanol losses due to evaporation. I replaced the bath with a more expensive lab bath w/ recirculation & heating+cooling. It's set to 60F which also aids in hydrometer proofing. No more evap losses. YMMV.

While the beginning and ending temperatures are not regulated, they do need to be the same before and after, which means you need an accurate thermometer to check your bath. My advice, don't skimp on your gauging tools too much. 

TTB finally made a dedicated webpage for their list of approved density meters.  https://www.ttb.gov/approvalalternatedevices

The Label Modernization Act changes in allowed proofing tolerance did not change the required accuracy of your gauging instruments.  

You can be +/- 0.3% now, but, you must be as precise in your measurement as always.  In other words, you are now allowed a variance, but you must still perform the measurement with a high degree of accuracy and precision.

On 6/30/2022 at 9:37 AM, Charles Brungardt said:

Thank you  @Kindred Spirits

How long does a reference cert last? Can it last 60 months?

Is this an ok thermometer? 

As far as I can tell, the code of federal regulations is silent on the topic of exactly how frequently you have to recheck your instrument calibration.  For the special case of a mass flow meter, it says "every 6 months".  For Density Meters, you are supposed to zero on DI/distilled water every time you use it.

But for Hydrometer & Thermometer, it is more vague: "... must have accurate instruments... for determining proof" and "Proprietors must frequently test their hydrometers and thermometers to ensure their accuracy".

I really dislike wording like that.  How often is "frequently"?  Surely, it depends on how heavily they are used?  I've heard that some TTB agents simply state that you must recertify annually.

The question of "how long does a reference cert last" is therefore unanswerable.  The certificate is just a piece of paper issued by a lab.  It should satisfy a TTB agent for a period of time, but certainly not forever.  It will last until the next instance of "frequently".

My advice?  Since the Reference Thermometer is out of stock, I'd just buy and use the single Reference Thermapen, as it also includes a calibration cert and has an RTD sensor with good accuracy.  Take good care of the instrument and especially the probe, and it will easily last a year.  After a year, buy a new one and use it to calibrate the old.  Now the old is your "workhorse".  This strategy balances cost & compliance to my personal satisfaction, but you have to make your own choice for your business.  You can also hire a lab service to calibrate your existing instrument against their standard, but the cost of that usually exceeds the cost of buying a new one with a new calibration cert included.

I recommend a similar strategy for Hydrometers.  But, due to their cost & fragility, I would suggest buying a calibrated standard (~$200-300) and a workhorse upfront ($50-100).

In a very simple case where you only bottle Vodka & Whiskey and you are a non distilling producer, you will still need to spend around $2k upfront for three pairs of hydrometers (75-95pf, 105-125pf, 185-206pf) and a reference thermometer.  Then, you have an annual rebuy expense of around $1200.  Considering that a used density meter can be had for around $8k, I really recommend thinking about that option, because it's so much faster and easier to use than hydrometer/thermometer.  

CFR citation follows.

§ 19.188 Measuring devices and proofing instruments.

https://www.ecfr.gov/current/title-27/chapter-I/subchapter-A/part-19/subpart-G/subject-group-ECFRe31d95ad7581d87/section-19.188

Here's a video on slow proofing from one of the distilleries (maybe THE distillery) that brought the slow proofing concept to light (brandy makers have been slow proofing for eons).  https://www.youtube.com/watch?v=mFUdKxMN3BU

You have the right idea to cut by weight.  Personally I like to circulate the whiskey in a tote with a small-ish pump (just pump over itself) while a 1/4" ID R/O water supply flows into the tank.  That takes minutes/hours instead of days.  Proponents of slow proofing will tell you that fast cuts lead to cloudy whiskey and/or saponification, and also that the heat increase from cutting causes volatile aromas to be lost to the atmosphere.  I think there's something to the first point and not much to the second point, unless your spirit and/or water are too warm to begin with.

If you have multiple similar barrels, why not proof one down slowly (drip feed maybe?) and the other quickly and see if you can pick a difference in a triangle test.  If you can't, maybe it's not worth the trouble.

My advice...

1) Lawyer up

2) Thoroughly research and understand Alternating Premises and Alternating Proprietorship as it relates to Federal Basic Permits

3) As Foreshot said, make sure it's legal in your state

4) If you still want to do it after steps 1-3, don't.  Partnerships are a nightmare.

6 hours ago, AK2 said:

I am guessing the second picture is some sort of vent to allow pumping into or out of the tank while it is sealed up.  My tanks I need to crack the lid a bit.  I do not have breathers, but now that I see those I may look into them!  The first picture might serve the same purpose, allowing for the air that is sucked in to be filtered.  That being said, it almost looks like a fluid filter.  In any case, these are both just guesses!

I concur.  First one looks like a filter intended to keep particulates out of the tank when emptying the tank.  Second one looks like a breather, serving the same purpose but without filtration.

While open tanks can be problematic for many reasons, due to the heavy mass of ethanol vapor (vs air), I would venture to guess that these fittings do not result in appreciable proof loss in the absence of compounding factors like heat, agitation, etc.

Liquid Ethanol expands and contracts with changes in temperature about 5x more than water does.  Depending on the "weather" inside your facility, you may need a breather just to keep your tanks from cycling between slight vacuum/slight pressure.  Most likely, those fittings were installed for a reason.  Intuition would suggest that you should have a good reason before removing them.

5 minutes ago, whiskeytango said:

Yah not overthinking it. I just swear I remember when we did our original boxes 8+ years ago I was working off a specified minimum size.  Maybe they changed it or maybe Im getting a NABCA requirement mixed up.   IDK lots of alcohol across this old brain between then and now 

You may be thinking of minimum font sizes for mandatory label information.  Those are specified in absolute (millimeter) terms. https://www.ttb.gov/images/pdfs/spirits_bam/chapter2.pdf & https://www.ttb.gov/images/pdfs/spirits_bam/chapter3.pdf

The font size requirement is not absolute, it is relative: "Of adequate size to be easily read".  Don't overthink this.  Although it violates CFR, many small operators do not label or serialize their cases at all.

14 hours ago, whiskeytango said:

Yep I have read that.  Is there nothing about font size and overall size that the overall info panel needs to be?

 

You read it but you didn't read the section that 19.489 references, 19.483, which states: 

(a) Basic requirements. A proprietor must place the marks prescribed by this subpart on cases, encased containers, and packages of spirits and denatured spirits so that they are:

(1) Of adequate size to be easily read;

(2) Of a color in distinct contrast to the color of the background;

(3) Legible; and

(4) Durably affixed.

(b) Use of labels. A proprietor may use labels as the means for applying prescribed marks if the labels meet the requirements of paragraph (a) of this section.

(c) Location. A proprietor must place the prescribed marks on one side of the case or encased container, or on the head of the package.

https://www.law.cornell.edu/cfr/text/27/19.483

Distillery management software packages can take care of this requirement (and many others) for you- highly recommended.

Regular granulated sugar has impurities. Try Baker's sugar. It is the finest 3% of granulated production, sifted off and packaged. The fine grain will dissolve far easier. Only downside is you can't stack the 50lb bags too much, or for too long, or it cakes up.

Reduce the variables - quit using syrup - and start with one of your flavoring ingredients at a time.

I don't know if this is what happened in your case and I hope you don't take this the wrong way but a syrup which got contaminated through improper storage or handling could result in the snot type sediment, IME.

I've never understood using syrups for production. It's an extra step, you're already going to add water to your spirit, why add it to your sugar as well? Plus you've got the potential for more measuring mistakes.

The other thing you probably don't want to hear is that the more natural your flavoring and coloring ingredients, the more you're gonna have these issues. Extracts, essences, and colorants will make it far easier to achieve a consistent quality product.

Thanks for an unsurprisingly well cited post. I looked for supporting CFRs and came up empty so it's great to get them!

On 3/9/2021 at 1:02 PM, JustAndy said:

Breweries are not allowed to add distilled spirit to beer, or even to have bulk spirit on site. 

 

I know of some breweries that have done cryo concentration but I'm unclear if it was approved by ttb. 

Concentrating alcohol is generally considered distillation by TTB and so that was probably not kosher. In the wine world concentration of alcohol is big business but the players that do it are qualified as DSPs

9 hours ago, PeteB said:

I do add extra water the flask after the 250 mL but maybe not as much as you have suggested. I will try with more water and see what happens.

My condenser does not usually become contaminated as long as I switch off heat soon after that cloudy distillate stage.

One time I measured the ABV of a cloudy sample of distillate, then re-distilled it and the distillate was clear and the apparent ABV increased.

Adding on to what meerkat's link says, I would first try increasing your dilution volume - you said you weren't even at 50% (125ml vs 250ml initial sample).  For something with proteins and solids and high viscosity you'd probably want to dilute even further, like 200ml in a 250ml sample. 

On 2/20/2021 at 6:45 PM, PeteB said:

Below are some extracts from TTB requirements.

I make a coffee liqueur which has very much in excess of 600 mg of solids per 100 mL

I distill off 250 mL in a glass lab still, if I boil off any more than about 70% of the original volume I find that my condensate goes cloudy and the apparent ABV readings start dropping. I assume that solids are being evaporated as the boiling point increases, and are condensed into my collection flask so re-obscuring the true ABV.

My understanding is 30.32  (c) says the sample must be distilled until there is only 1 or 2 mL left in the flask, but it does not mention the size of the sample. If the original sample was 250 mL<which is quite common, that 1 mL would be charcoal.

You're gonna want to dilute your original 250mL sample with an extra ~125mL of distilled water before starting, then the instructions will make sense and your glassware (& elbows) wont suffer any more.  If you are still getting cloudy distillate, PM me