New Nocino maker in search of help with proofing and obscuration

[michaelbgardner]

Hi all:

New to the forum although I registered a year ago. I am a small maple producer in northeast Ohio, with a ample source of eastern black walnuts on my farm and in the surrounding community. I was introduced to Nocino by the caterer of my son's wedding held at my farm in 2020. Seemed to be a divine match to produce a farm-based nocino finished with maple syrup instead of refined sugar simple syrup.

I found a recipe, obtained my Basic Permit and formula approved by TTB and my Ohio A3A liquor permit. I bought three 10-Gallon stainless milk cans and harvested green black walnuts in July of 2022. For some silly economic i thought it made sense to macerate the walnuts with grain alcohol (190 proof) instead of vodka and dilute the grain alcohol in half with the condensate from the evaporator.  For every bottle of grain alcohol i added one bottle of the condensate. I believed I would end up at ~47.5% ABV and then by adding maple syrup to finish it, I would end up at about 40% ABV.

My recipe (per liter) called for 1 lemon (peel without pith)l 23 walnuts; 1 clove; 1 allspice berry; 1 vanilla pod and 1 cinnamon stick. I bought a pel-a-matic to automatic peeler to peel all the lemons.  

All was moving along well until about this time last year November 2022. I bought an alcohol hygrometer to measure the ABV before adding the maple syrup.  Each batch i measured several times and observed an ABV range of between 20 - 24% It would appear I over shot my mark for dilution.  I tried playing around with 50 ml sample and adding everclear to boost the ABV and then maple syrup to get a finished product, but ended up down the rabbit hole of proofing and obscuration.  I removed the lemon peel from all of the batches as it seemed much too strong.  My mom died last December and its been sitting every since. With the walnuts and all the other ingredients.

I'm really at a loss for how to salvage the whole operation. I'm trying to understand how much obscuration if any, might affect the mixture as it stands now without having added the maple syrup? I don't believe any of the ingredients have added dissolved solids to the mixture notwithstanding the fact that it is black. If so, I can see myself adjusting the existing ABV back to my target of 47.5% or even 40% my final target ABV for the nocino by buying and adding more grain alcohol. And try finishing it with maple syrup to taste and then try the proofing and obscuration process.

My other question is how much obscuration to expect by adding 375 ml of 66.7% Brix maple syrup into 1 Liter of the mixture. adjusted to 47.5% or 40% ABV. I don't have any sense whether its 1- 5% or 20% 30% or more. Just so I could get some sense of where the ABV my lie using my hygrometer.

By way of background i have about $1250 of grain alcohol invested in this already.  I inclined to throw a little more at this to give it a go,

I can't quite fathom how I messed up in adding 1 bottle of condensate for each bottle of grain alcohol in the mixture and ended up at less than 1/2 of the expected ABV of the mixture.  I'm pretty sure I didn't misread the hygrometer. I had my son, a medical student with me taking some of the readings. 

Thanks for listening to my tale of woe. Any advice would be appreciated.

 

 

[meerkat]

The unexpectedly low ABV after dilution with the condensate is difficult to explain. The low dissolved solids – which Google estimates as about 2.5% - would cause a decrease of 0.5 – 1% in the ABV, depending on the mass of walnuts in the spirit.  A more likely culprit would be moisture extracted from the walnuts if they were freshly harvested and not dried yet. But I don’t think that even this would fully explain the drop in ABV.  Do you have any of the original grain spirit left to confirm that it really was 190 proof to start with?

If you were to add 375 ml of 66.7 Bx maple syrup to 1 liter of 40% ABV it would decrease the true ABV to about 29% but if you tried to measure it with a hydrometer the apparent ABV would be less than zero because of the extreme obscuration.

Measuring ABV and Bx at the same time requires special attention.  The official TTB method requires you to distill off all the alcohol and most of the water and then measure the ABV of the distillate.  The TTB has produced a good set of videos on this.  Part 3 is what you need to watch.

A quicker method is to measure the density and the refractive index of the spirit. This allows you to compensate for the obscuration of both the density and the refractive index.  I have written up a description of how this works here.  It is something like specifying your location by giving the longitude and the latitude and knowing that the lines cross at only one place.

You can purchase instruments that perform both the measurements (density and RI) and interpret the results automatically for around $40-50k I think. However, you can get good results with the Anton Paar entry level set of EasyDens plus SmartRef together with my AlcoDens LQ software all for less than $1k.  The EasyDens and SmartRef keep their costs low by excluding some of the computational power and the display, and then relying on your smart phone to provide it.  This combination would certainly be good enough for your diagnostic work and for product development.

[jocko]

Fast & easy: wait until the end, then send a 50ml sample to someplace like White Labs and get the true ABV at the end.  What matters is taste & mouthfeel, not ABV.  Nocino ABVs are all over the map. 

You cannot measure ABV of an obscured spirit unless you do to TTB distillation test, or have an expensive tabletop machine like an Anton-Paar designed to do such things. 

[FIVE x 5 Consulting]

On 11/13/2023 at 6:34 AM, jocko said:

You cannot measure ABV of an obscured spirit unless you do to TTB distillation test, or have an expensive tabletop machine like an Anton-Paar designed to do such things. 

While this used to be true, earlier this year meerkat added functionality to AlcoDens LQ that allows you to do the tabletop-type calculation yourself. You just need a density reading (e.g. from a hydrometer) and a refractometer reading (e.g. from a brix refractometer). I think this is really cool and kind of a big deal that we can do this analysis for a few hundred bucks - those benchtop instruments cost $30k+ and they were previously your only option.

[jocko]

I would love to find out more about this.  I see the link now in Meerkat's post. This could be a game changer if it works on any beverage.  @meerkat, will this method as implemented in AlcoDens LQ meet TTB's standards?  What is your estimated accuracy?

[FIVE x 5 Consulting]

@jocko TTB standards require bench distillation above 6g/L dissolved solids, full stop. Even the expensive benchtops from Anton Paar and Rudolph Research are not TTB approved for proofing of obscured spirits.

With that said, you can potentially get a variance from TTB Scientific Services Division to allow you to use an alternative method instead of bench distillation. Such a variance could apply to GC/MS, AlcoDens LQ method, a benchtop or any other method that you can demonstrate is sufficiently accurate.

Accuracy of meerkat's calculator is utterly dependent on your instrument quality and lab skills. If you use a $9 hydrometer and a $14 refractometer, you're going to get a reading but it's probably off by 2-3% ABV.  I personally like the EasyDens/SmartRef combo that meerkat mentioned ($399 / $279 respectively) which can reliably get you within 0.5% ABV or maybe a bit better in ideal conditions.  If you want to achieve 0.1-0.2% ABV +/- levels of accuracy, then you need the precision offered by a benchtop density meter with temp control + benchtop refractometer with temp control (not temp compensation).  This is what the expensive benchtop instrument combos from AP/RR offer.

[Golden Beaver Distillery]

As the others stated, you will need a desktop or Meerkat's setup. Finally, you will need to do TTB bench top test, regardless.

I can tell you how we manage spirits with syrups/honey and proofing.

1) In your case macerate your walnuts. Drain off distillate and filter for particle.

2) Macerate your botanicals and drain and filter again.

3) Using the Hootchware app. Calculate proof using the weight function.

4) Weigh your syrup/honey in the portion you want to add.

5) Subtract that weight from the water weight to add that Hootchware calculates.

6) Add your syrup and blend well (we do it over night in a spirit mixing tank).

7) Start titrating the remaining water weight.

8 )  We start testing at 75% of added water weight.  

9) Slowly walk down your spirit to desired proof using either a benchtop or Meerkat's system.

10) When you hit your target proof do the TTB method of proofing obscured spirits.

[meerkat]

Regarding Golden Beaver's step 5 - weight for weight syrup or honey will reduce the proof by less than water would.  The difference in proofing effect between the syrup/honey and water varies with the Brix.  As long as you know the Brix of the syrup AlcoDens LQ will calculate for you the exact weight or volume of syrup (or even granular sugar and water) required to achieve a particular target proof.  Regardless of how you do the calculation, step 9 of proofing down slowly is probably a good idea.

Edited November 14, 2023 by meerkat
typo

[et1883]

at the end of the day, thermometer, hydrometer to start, and TTB's dehydration method as shown in their video series to weigh the remaining solids, then do the math to reach 100ml and to reach actual proof.  Unless there is a TTB waiver or approval of alternative method?  EZ link to TTB's how-to vids:  https://www.ttb.gov/distilled-spirits/proofing-tutorial   with part 4 on the right being operative section.   Anyone have a waiver of that dehydration method? 

[TwentySevenBrewing]

There was a great presentation at this past year's ADI that spoke about this, if you have access to the member's ADI videos, check it out. Its title is Proofing: Novel Method for Obscured Spirits. 

 

Chris