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  1. bostonapothecary

    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.
  2. bostonapothecary

    Damson plums

    I suspect that the future of fruit eau-de-vie's and premium fruit liqueurs is extremely bright, but very narrow and exclusive. They are increasingly only going to work for farms with agro tourism programs that can sell pretty much their entire batch capturing the full retail mark up. I bet the opportunities for a lot of regular distillers will just be consulting and equipment lending for the much smaller true farmer-distillers.
  3. bostonapothecary

    Birectifier for gin development

    The birectifier, which I've resurrected, was the renowned laboratory analysis still of Rafael Arroyo. He died young and the design was lost for the last 60 years so it was never applied to gin production. My pet project within my other birectifier work is successfully applying it to gin development. I also have the lost Seagram botanical assay protocols for precisely standardizing a botanical charge which are quite pragmatic and I think are from the 1930's. I am hoping to fuse the two ideas. The birectifier is typically operated with a charge scaled to 100 ml of absolute alcohol and 8 fractions of 25 ml are collected every 15 minutes. So this is slow incredibly high reflux micro distillation. When collected carefully and faithfully, comparisons can be made, fraction to fraction, across multiple distillations. What is special is how very different all the fractions are from each other. This was well understood with typical spirits from fermented products, but what would happen with gin? Gin surprisingly ended up with well differentiated fractions that we can learn a lot from. A role model gin was carefully analyzed here (there is lots of other great stuff in the post beyond my quote here). A lot of this complements and adds weight to Odin's teachings, but can be used to refine things and create in depth first hand experience. The process can be used to follow along with role models and organoleptically evaluate the quality and consistency of botanicals before graduating to the Seagram protocols. It is easy to create an actionable path to making a new production fit the shape and outline of role model. Incredibly, all the auxiliary botanicals seem to get pushed into fraction 5 which tell us a lot. For starters, we can test funky botancial choices for their potential with the birectifier by where their aroma ends up. If it is in fraction 5, it is on the money. The birectifier is like a scalpel meets magnifying glass so we are cutting away noise and magnifying things. This helps investigate complexity achieved by a botanical formulation. The tool may help elaborate and refine choices so that each batch progressively improves. Eventually, the distilling decisions will be paint by numbers and we'll be able to shift our involvement to the quality of the botanicals themselves and our create linkage concepts. I'm going to keep diving into this and hopefully I can produce some really useful protocols for people.
  4. bostonapothecary

    Condensation Inside Spirit Bottles

    I've been told this is because of insufficient rinsing of bottles and they should be rinsed with a portion of what they are being bottled with. I've never seen a chemical description of what is happening, like what exactly is condensing.
  5. bostonapothecary

    Bostonapothecary signing in

    It has an air cooled dephlegmator and vapor goes through the part that looks like a claisen. The bi in birectifier is because it is a rectifier in a rectifier. The earliest version of it is from at least 1907 where the internal rectifier was just straight. The vapor goes up the outside, is condensed in the air cooled dephlegmator, down into the internal rectifier and then out. Eventually a vapor trap was added to the dephlegmator and a return tube connecting the second rectifier back to the first which prevents pressure from building up and allows everything to come to an equilibria. It was first used for beverage work by Dr. Karl Micko and eight fraction analysis is/was referred to as Micko distillation. When Dr. Luckow got a hold of it, all the proportions were optimized for a 100 ml of absolute alcohol scaling system. Luckow and Wustenfeld developed all the companion techniques like the exhaustive test which is an alternative to complicated titrations. Things were mostly developed when the still reached Arroyo, but he was the first to systematically apply the tool to yeast selection, fermentation optimization, and maturation. Everything was shaken up by WWII, the post war economy, and then the untimely death of Arroyo in 1949. The last reported use of the tool was in Trinidad in 1953 as part of a PhD thesis. My first edition copy of Studies on Rum own by a Seagram employee had a single page "photostat" in it of a 1945 International Sugar Journal article on the birectifier that wasn't in anyone's bibliography. Who know if Seagram guys ever used one. Arroyo did correspond with Paul Kolachov who is acknowledged at the end of Studies on Rum. We almost didn't think the thing would work just by looking at the drawing, but it generates a wild amount of reflux. By a quarter way through the 5th fraction, you've exhausted all 100 ml of absolute alcohol. No off the shelf glass parts can do that. The only micro distilling units that can are "spinning band" still and they cost pretty startling money. A friend is a micro distilling expert and he optimized all the fittings so the thermometer ports are threaded and the condensor joint is a ball style to reduce stress and opportunity for breakage.
  6. bostonapothecary

    Slow Distillation and Maturation

    Instead of slow distillation, for the last few years I've been advocating for something I call guided traditional practices. It is something I see in the fine wine industry and something that is part of many spirits category's history such as Bourbon. Bourbon went from practical distillers who weren't formally trained and knew little science but often produced excellent products to scientific concerns that relentlessly pursued efficiency to bland commodity ends and then back upwards to guided traditional practices with Maker's Mark and Wild Turkey when they got their own production (tequila is in the violent throws of this). If you read through the oral histories of the California wine producers that won at the Judgment of Paris, you'll understand that fine wine was born in the lab. All the winners like Mike Grgich and Warren Winierski were the lab guys from their previous wineries. They were not exactly scientists and were sitting in on night classes at UC Davis, but they weren't matriculated students studying to produce wine by the silo. Right now near no small producer operates a full on distillery lab and my big pursuit is creating a pragmatic one and sharing it. The absolute foundation of the lab is turning out to be Rafael Arroyo's birectifier lab still. The beauty of the birectifier is how much can be done with only organoleptic technique. It really respects slow ambitions, but you can stack chemical analysis on top as you get more sophisticated. Fine wine makers do tons of lab work, but its simple and pragmatic. They aren't all in on GCMS, it just doesn't help. One of the things the new distilling industry needs to confront is that "fermentation is the climax in the manufacture of rum". This is an Arroyo quote from Circular 106 which applies well to any spirit category. Distillers need to get over the fetish of the still and learn that they are really fermentation chemists. This impacts labeling to some degree. I don't want to see anything labelled pot distilled if it didn't have a fermentation worthy of slow and steady pot distillation. I also don't want to have to see spirits like rum have to live up to the Bourbon template. A lot of the labeling ideas proposed don't make any sense and a lot of them become irrelevant if there is a public intellectual behind the helm like most cult fine wineries. Publicly explain yourself, and if the juice is good, you can do mostly whatever you want. One thing not often acknowledged is how terrible many of the practical distillers were and that many often couldn't ferment to dryness. The IRS actually became the lead consultant educating producers because it was easier to keep the books when you guaranteed everyone fermented to dryness. Grain in matched ethanol out. The revenuer didn't have to become a detective with a flashlight wondering whether a ferment was botched or if ethanol was stolen. There is very little traditional knowledge on building spirits to age until Arroyo comes around. Arroyo ultimately attributed his success in tackling it to the birectifier. Eight fraction Micko distillation makes readily apparent the factors that contribute to maturation time. Slowly by analyzing spirits over time you can build trajectories. I don't think anyone's career is long enough to build intuition for these maturation trajectories without sitting down and doing frequent analysis and deconstruction of role models. The more role models you deconstruct, the faster you can build mastery. Our next step with the birectifier is automating it so a distiller can run it twice a day. This makes it practical to pre-screen your ferment with micro distillation and then grade it A,B,C,D which will correspond to the distillation proof it deserves and the cutting regimen. Cognac was known for micro distillation pre-screening before large producers switched to inline spectroscopy. The A,B,C,D pre-screened framework means a distiller could start taking risks and slowing down ferments to gain quality. Faults would be caught (fraction 6,7,8 of the birectifier) and distillation changed to accommodate it. One big benefit of an analysis framework is adding confidence in delegating tasks and there will also be more confidence in tackling new products like a rum producer taking on an apple brandy. A lot more could be said, but the foundation of slowness or guided traditional practices is practical analysis.
  7. bostonapothecary

    Bostonapothecary signing in

    The surprising and very cool thing about Arroyo is how all his advice travels far beyond rum. The birectifier deconstructions are turning up rum oil-like terpene fractions left and right (fraction 5). Initially, I was stressing about finding them in rum to validate his work, but then they were turning up gloriously in pear eau-de-vie and even Overholt rye! My last deconstruction of Fortaleza tequila was the most fascinating relative to Arroyo's advice. He went to great lengths to figure out how to create ferments that could be distilled at low proofs, both to capture more terpene fraction and to create less aroma breakage later on. Well, tequila seems to do it relatively effortlessly relative to rum. My big wild theory, which started in my sensory sketches post, is that sensory properties of the terpene fraction allow a spirit to contain more of other categories like fusel oil and still remain harmonious on a sensory level. Some substrates unlock their terpene fraction easier than others as may be the case with agave or rye relative to molasses. (Pictured in the center left flask is the terpene emulsion from fraction 5 of Fortaleza tequila.] To create whiskies that maximize their potential, we may, just like Arroyo, have to become terpene fraction obsessed. For the rum distiller, this may be achieved by yeast selection while for the rye distiller, it may be in the grain selection. No one really knows, but now with the birectifier, we have the tool to look. I aim to take some different grains scaled for potential alcohol and distill them unfermented with the same amount of absolute alcohol added to see if a terpene fraction appears without the need for fermentation. A similar idea appeared in the Distillers Workbook exercise #9, but now it needs re-explored with the birectifier. I'm just about done reading Adam Leith Gollner's The Fruit Hunters where he described the world and culture surrounding rare fruit, most of which do not make it to the market. What I suspect is that with the new more lax distiller's laws, ideas from Arroyo can be translated to fruit eau-de-vies and a lot more heirloom fruits kept viable with the fine alcohol market. Pursuit of the terpene fraction by producers and consumers will drive a lot of interest. The birectifer for analysis will allow a lot of precision production on the very small scale.
  8. bostonapothecary

    Bostonapothecary signing in

    Haha, I'm simply a nerd that abuses my library card. I was able to get so many first time digitized inter library loan papers because a connected bar regular wrote a letter to the PBL on my behalf. Typically they slow you down or if something is too challenging, they give up. The PBL has been really amazing. Many of the papers were in library basements or offsite storage. Public librarians must have put many hours into retrieving each individual first time digitized paper. Studies On Rum came from a Harvard friend who filled out some kind of hardship form to get it out of the reading room. Most copies are reading room only because they are all crumbling to dust. I recently acquired a weird special first edition on better paper with an amazing binding. I have Kervegant's book and that will be scanned next. The birectifier engineer's drawing was found in a rare German text. In the particular text, it was Glass companies are finicky or have really long lead times. The first one made was a little bit incorrect so I found a local guy to modify it who turned out to be amazing and liked the project enough to sign on as manufacturer. They can now be made with a realistic lead time. I have no chemistry background besides youtube and reading Peter Atkins. The significance of the birectifier is that you can get so much out of it organoleptically before you stack titration and other chemical analysis methods on top. It is a tool that at the minimum allows distillers to get so much done by just smell, taste and feel. Tests like the exhaustive test allow you to weight congeners organoleptically without titration. Sometimes adding the titration, with modern high productivity equipment, may cost thousands (often more than the birectifier itself!). All this recent work brings powerful tools affordably, and without being a full fledged chemist.
  9. Hi there, Many of you may know me from the bostonapothecary blog which I've written for the last 10 years about explorations in beverage technology. The blog hosts many significant writings on distillation such as the recovered papers of Rafael Arroyo [2], my many translations of French and German papers on rum production, and a near complete bibliography of journal articles published on gin production. For whiskey, I published a data table from a 1968 document that has the detailed production parameters of 42 American whiskey distillers producing 112 different whiskey mashes (85 Bourbons, 10 rye mashes, and 17 corn mashes). I wrote a series of articles called the distillers workbook to, on the lab scale, teach hard to reach concepts in physics and chemistry. The workbook became the foundation of the cocktail centric hotel bar distillation scene flourishing in the UK. I've advised a lot of people and designed a few products on the market, but there are giant practical holes in my knowledge. I would not even feel comfortable running a distillery until I learned a few more analysis techniques and more about yeast work. I can answer lots of obscure questions by pointing people to the literature, but you have to take a lot of it with a grain of something, because I haven't lived it all yet. My latest project is the revival of Rafael Arroyo's beloved laboratory still, the birectifier, and it is proving truly magical. I guess I'm a vendor. The blog lately has numerous deconstructions of role model spirits [1,2,3,4,5,6,7,]. Arroyo attributed much of his research success to this device. It is sort of like a scalpel meets stethoscope for spirits. Small samples, such as 250 ml of 40% ABV spirit, are very slowly super fractionated into multiple (typically 8), uniform fractions for the sake of counting congeners and making comparisons. Coupled with a few sub-analysis techniques, it allows the progressive development and reverse engineering of spirits. Arroyo used this for yeast selection, fermentation optimization, still tuning, and even for decisions regarding aging. I've recently been applying it to gin analysis with amazing success. I've recently recovered Arroyo's own writings about the still and its operation. I've also translated all of the German companion organoleptic tests and have slowly been bringing them back to life. The birectifier solves a lot of problems for a lot of people and I'd be happy to answer any questions about it. They are available and we have a continuously shrinking lead time. I look forward to participating in the forum. -Stephen
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