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Jun 08, 2022 View:

Distillery Analysis

Hello all.

A very neglected thing in the new arm of the distilling industry is analysis. Lately, I'm trying to make my focus developing a pragmatic best bang for the buck distillery laboratory. I'm hoping to learn what people are currently practicing and what they would like to take on next, even if they're only growing from a hydrometer and pH meter upwards.

Lots of people are buying big ticket u-tube densitometers before they buy other tools like automatic titrators, but is that a good idea? One of my projects is trying to add pycnometry to my analysis tool set as a stepping stone before a u-tube densitometer. It is no walk in the park, but I'm getting there.

The big tool that is looking like the foundation for any distillery lab is Arroyo's birectifier lab still. It can tell us incredible things about spirits and allow us to intimately compare them. As far as time goes, when manually operated it can take 2.5 hours to operate and then perhaps 20 minutes to assess the output. Is that too long for many people's busy schedules? We are hoping with automation to dramatically slash the active time it takes to operate so it can run twice a day unattended. My consulting work is showing that it can significantly shorten product development time and expense for products like gin, paying for itself quite quickly. The birectifier also allows a priceless education in the inner workings of role models and competitors.

Is anyone currently using automatic titration? I'm looking at buying a model that is about $3500 from Hanna Instruments. I want to investigate the concept of Δ acidity for working with ferments that have large buffers. This is an idea first brought to my attention by Michel de Miniac in a French paper I translated. The Δ, as opposed to the pH, can imply how many acids beyond the norm of your yeast were created by bacteria. This can either be used to tell when clean spirits go dirty or perhaps when intentionally dirty products like heavy rums become a run away train. Within anyone's current experiences, would that tool pay for itself quickly? or are the learning curves of integrating the equipment another large barrier?

Is there any interest in other titrations such as for fusel oil or esters and has anyone priced them out? It is surprising me that ester obsessed people are not investing in counting esters or perhaps I'm just not aware of it. Some analysis such as ester contents seem like it can be woven into marketing.

Has anyone tried the exhaustive test which is a low cost rudimentary alternative to titration that works in a variety of scenarios? The Germans developed a variety of organoleptic techniques that seem really useful before shelling out the money for chemical analysis equipment.

Is anyone interested in botanical assay? I have the lost Seagram procedures that I haven't done much with. They cost about $3000-$4000 to fully implement (half of that is an analytical balance). The tools required can also help perform a bunch of other tasks such as measuring barrel solid obscuration by the TTB evaporation method. Seagram used two specialty pieces of lab glass and I may start producing one of them (a modern day optimized Clevenger apparatus).

Some gins are getting really successful. I'm suspecting the cost to accurately standardize botanical charges has to becoming viable for many. What are the biggest micros performing?

I would love to start some discussion here, but if anyone want to discuss very specific things privately, feel free to DM me.


Reply:

I don't know where people are with exploring chromatography based analysis, but I just wrote a fun post about birectifier assisted chromatography.

In the fall, I attended a conference in Jamaica where pretty much all the distilleries used chromatography (and ran 3 shifts around the clock!), but all wished they did more with organoleptic analysis and possibly olfactometry. A lot of the compounds producers are missing are derived from carotene and very hard to look at. These turn out to be the highest value components in a spirit, be it rum or bourbon. The birectifier becomes the cheapest way to evaluate them and the smartest way to contextualize them and tie them to decision making during production.

This post was in response to three different university labs requesting birectifier samples. They wanted to look at what was in fraction 5 and possibly name the compounds that Arroyo called "rum oil". They keep insisting on 100 ml samples, but I had to explain that traditional birectifier samples are already concentrated 10x! If I sent one to further concentrate for chromatography, it would already be a better than average starting point. We'd also have more context than usual because we know the band of volatility we are looking at and we can repeat the birectifier work on the cheap.

I'm making slow progress, but the birectifier is attracting some of the world's great labs and hopefully will be a part of research papers that will be especially useful to craft distillers.


Reply:

love your enthusiasm, perfectionist attitude and approach, but I have to ask, what's the real goal ?  Beyond that, why do you think any small distiller even cares ?

the products we make either taste good, or they don't. For clear spirits they are as clear as ones equipment can make them, and for aged spirits the flavor profiles at distillation will change so dramatically during maturation that they make the initial information gained from your exhaustive process, vitually meaningless. 

The fact that on day one, a specific batch of bourbon had 1/10,000 of congener ax1, vs 3/10,000 is almost nothing but noise, considering that one will not even know what the product will actually taste like for 5 years. Even then the blender will just attempt to hit a representative sample by blending a certain amount of different products with their nose.

it seems like your incredible attention to detail would be better (and more profitably) served in something like the medical field, vs determining minutia about something so  banal as alcohol. In fact one could assume by the lack of responses to your OP, that this field of endeavor may be very limited. 

prost/Roger 


Reply:

Hi Roger,

There clearly isn't much interest here, but interest/sales are coming from the Caribbean and the largest new players. There is also interest from university programs and a few PhD projects. There definitely isn't much of a profit motive.

Some of these congeners have extremely low thresholds of perception, so very small quantities are surprisingly very meaningful. Best bets are emerging on how to maximize them just through practical operation and nothing exotic. It is kind of like trying to cook the same dish as a chef with modest ingredients. You make something edible while they take the same ingredients, seem to understand a few more variables, and manage to create something far more appealing with no more effort than you. Ingenuity.

During maturation, we know what is changing. During distillation we know what is going where and what is being formed. Garbage in, garbage out. Fermentation is the climax of production. The U.S. and other countries conducted decades of public research for entrepreneurs to build sound private enterprises upon. It blows my mind that it is so easily dismissed. The birectifier project aims to give one affordable and practical tool to use to compete against deep pocketed multi-nationals with million dollar labs. To have no tools but a pH pen is kind of crazy especially when people are investing millions.

You can lead a horse to water, but you can't make it drink. Hopefully it should at least be comforting to know tools and ideas are readily available. Good luck.


Reply:

 

My commentary is not meant to be negative, it is just one distillers look at your offerings to if nothing more, allow you some insight into your future endeavors. 

prost/Roger 

 

 


Reply:On 7/18/2018 at 8:10 PM, bostonapothecary said:
Reply:

boston apothecary,

 

I have a question, but not about beverage ethanol distilling.    What instruments would a person use to check a sample of denatured ethanol for percentages of heptane and ethanol?  I know that I can spend thousands on equipment to do this or send it to a lab, but is there any way that I can do it inexpensively in house?

 

thank you.


Reply:On 1/6/2019 at 7:31 AM, Silk City Distillers said:
Reply:16 hours ago, Southernhighlander said:
Reply:

I thought the cannabis extractors didn't care about heptane in their denatured alcohol, since in the rotovap or vac still it distills with the ethanol and doesn't remain in the product.  It forms a difficult azeotrope, that's why it's used for denatured alcohol.

Seems like heptane denatured ethanol is becoming the defacto standard for tax-free ethanol in that market.

https://ultrapure-usa.com/marijuana-solvent-extraction-botanasolv/

https://710spirits.com/tell-me-more/

 


Reply:

Oh wow, I would have thought heptane was from the fuel ethanol world and not the cannabis world. Doesn't it have properties that can help dry ethanol?


Reply:

I wrote a post on what to consider when making cuts. A lot of the ideas are based on using the birectifier as an analysis tool to ensure you are distilling at the peak potential of your ferment. This was brought on by a new distiller's questions and by a unique case study where we looked at a tails fraction and found a startling quantity of high value congeners that were just not making it into the hearts. Not many realize that what is high value is less volatile than fusel oil. Something I'm consistently seeing in new American spirits is that they are too light on ethyl acetate. Simple analysis, especially of role models, may help hone in on ideal amounts.


Reply:7 hours ago, Silk City Distillers said:
Reply:

I know temperature is an unreliable thing to measure, but could you reflux it and try to measure the temp of the azeotrope to make sure it is in spec? Or are you concerned with measuring what is left behind in the oil?

I thought the tax thing would not be that big a deal because you'd be able to reuse the solvent over and over?


Reply:

Yeah, I'd also assume you could infer the concentration by measuring the temperature at boiling point at a specific pressure.  It might be easier to do this under vacuum.  Measure the boiling point of a laboratory tested sample - and compare subsequent samples to this boiling point.  The BP is not likely to be a simple linear function though, so you wouldn't necessarily be able to easily determine the concentration, unless you had a table to compare against.

That said, you could just get some 200 proof ethanol, some heptane, mix them in known ratios, and test the boiling point of each at a specific pressure.  Then, plot out a graph of the boiling point vs concentration.

However, this is pretty crude, assumes only a binary azeotrope, adding water to the mixture complicates this immensely.  So old solvent that has absorbed water, will likely read as having a higher percentage of heptane than it actually does.

 


Reply:22 minutes ago, Silk City Distillers said:
Reply:4 hours ago, bostonapothecary said:
Reply:4 hours ago, Silk City Distillers said:
Reply:

Recently, I used the birectifier to look at the tails fraction of a full bodied rum. The results were very cool and quite insightful. Fusel oil was shown blocking a significant portion of high value congeners from entering the spirit. If fusel oil could be reduced, more HVC's could be captured and spirit quality improved. The birectifier made examining and making sense of it fairly easy. We generated great actionable insights with the minimum of hard science.


Reply:

Recently, I started exploring titration for acids and ester determinations and wrote a primer. Is anyone here currently using titration in their analysis work that is willing to offer some tips?

I'd love an automatic titrator, but working affordably so the work can be duplicated by others is important.

My goals are to accurately measure titratable esters in a spirit and then subtract the ethyl acetate isolated in the first three birectifier fractions to create a ratio of low value to high value esters. Arroyo worked with a similar ratio in Studies on Rum. I'd also like to be able to create numbers that can bring more of the historic data tables to life. Tracking the development of ethyl acetate is important to understanding maturation.

Titratable acidity is key to working with ferments that feature large buffers and significant noble volatile acid production.

I'll hopefully add these basic titration results to my birectifier role model case studies.

Any tips, tools, suppliers, or calculators you like?