Sugar in Liqueurs

[Dismal]

I'm looking for the tradeoffs between the various forms of sugar in liqueur production.  Sucrose vs. dextrose vs. invert vs high-fructose corn syrup vs ...

Does one or the other

   - Contribute to clarity more/less?  

   - Crystalize?

   - Interact with botanical extracts to form haze or particulate or condensate?

I'm developing liqueurs and using white sugar and making my own syrup for development.  I'm getting snot, sediment and haze.  I filter extracts down to 2 micron.  I'm being systematic exploring combinations of sugar concentration, ABV and botanicals concentration but I'm not seeing correlations to haze and snot.  In some cases the snot forms fast, in others it takes weeks/months.  

I'm adding a picture for reference.  This has been agitated a bit.  When not agitated the snot look more like clouds or strands than the blobs in this picture.  

All input appreciated.  

IMG_8018.HEIC

[Foreshot]

I filter down to .5 microns and still get that stuff though it takes way longer. It's possibly terpenes (essential oils) or esters (fatty acids). Michael at TCW has haze filters that might help. You could chill filter but that can be expensive and you will loose flavor. To test if it is terpenes/esters put it in the freezer. It will coagulate in a few hours. I don't believe the issue is sugar related but that part I don't have as much experience.

[SCLabGuy]

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.

[Thatch]

Our Chocolate Vodka is as clear as the original Vodka.  We've never had a problem.   Our dosage is only 3% Simple Syrup plus the flavoring.  We use a bar grade product.

 

[Foreshot]

https://beerandbrewing.com/dictionary/ycg6ddyEMu/

Good read there on colloidal haze. No idea if that's your problem but it could be a contributing factor.

 

[glisade]

I've had that same floc-like formation in some liqueurs. The floc forms from sub-micron particles that attract each other over time and form the larger floc blobs. My solution has been to filter, then fine and rack the liqueur then filter again. It doesn't come back after that and now the most I get is some slight wispy sediment on the bottom of the bottle. 

[Dismal]

This is good information.  Thanks all. 

I'm also looking into terpenes/esters for their contribution.  I've isolated one of my botanicals as the culprit of a haze I've been chasing.  The botanicals haze immediately whereas what I'm discussing here develops in weeks/months.  

I'm focussed on sugar's contribution.  Here's an article discussing the phenomena: https://www.eatortoss.com/single-post/2019/03/17/the-case-of-the-uninvited-wisp-in-the-honey-liqueur 

Here's a peer-reviewed paper that goes deep: https://www.semanticscholar.org/paper/Sugarcane-cells-as-origin-of-acid-beverage-floc-in-Lima-Tessmer/0d9e9261e888c16df5e5575507efbc47ed80c758

I found sugar products that are designed to address this:

https://www.dominospecialtyingredients.com/b2b-product-sku/lcmt-invert-syrup

https://www.sugars.com/products-sugar-and-sweetener/bottlers-sugar/

https://unitedsugars.com/wp-content/uploads/2020/07/cordial-sugar-7-15-20.pdf

 

I haven't yet found a supplier of such a product that has a minimum order quantity that's less than a tanker truck but I'm still looking.  In the mean time one of the producers is sending me a pail of their product to test.  I'll report the results.  

[Foreshot]

I've never heard of Acid Beverage Flocculation before. Thanks, that's something new to add to the list of troubleshooting items. And thanks for the links, those are great reads.

Quote

the chemical composition of sugar may contain numerous compounds that promote the formation of acid beverage flocs (ABF)

Quote

identification of compounds, such as p-hydroxybenzaldehyde, vanillin, triacontanoic acid, hexadecanoic acid, octadecanoic acid and n-octacosanoic acid, in the ABF composition. These compounds are widely found in vegetable tissues, confirming that the ABF are formed by tiny particles of plant cells of sugar cane

So if maybe if you do a sanitary filtration (.5m or less) after adding sugar/right before bottling would reduce/eliminate the ABF?

[Foreshot]

Some more research:

https://www.researchgate.net/publication/236879657_A_review_on_acid_beverage_floc

Interesting side note here:

Quote

Chill haze is caused by the interaction of proteins and polyphenols. The beer manufacturing industry uses silica to stabilize the product, and the interaction of silicates with proteins is certainly relevant to ABF formation in soft drinks.

https://internationalsugarjournal.com/acid-beverage-floc-abf/  I can only read the abstract but the following nugget is interesting:

Quote

It should be noted that it is not associated with other haze forming processes in sugared solutions, such as the alcoholic precipitation of polysaccharides, the precipitation of SiO2, and biological activity.

unsworks.unsw.edu.au/fapi/datastream/unsworks:34859/SOURCE01 Page 17 (PDF page 34) gives a long discussion on what makes up ABF. There's references to particularities in alcoholic beverages.

Quote

Dextran and amylopectin were both found to stabilize any flocs formed rather than contribute directly to ABF formation. Future studies are recommended with other types of high molecular weight polysaccharides to determine whether this finding is consistent with all types of polysaccharides or only of certain polysaccharide types.

 

[Dismal]

The Silica bit is interesting.  I read that it's used sparingly in beer because it inhibits the head for the same reason that it inhibits floc.  

 

Next I'm running an experiment using Baker's sugar (per SCLabGuy) and borosilicate glass, 1 micron filter (per Foreshot).  I'll report results.  

[Foreshot]

More geekery: The micro/nano particles of plant remnants in sugar are colloids. https://en.wikipedia.org/wiki/Colloid

Colloids are groups of molecules bound together vs individual molecules. Think of it this way: A small amount of sugar in water will dissolve completely in water. Those remnant particles from the sugar that are not dissolved are colloids. They are extremely small particles: 1 micron or less. Due to their light weight they can be suspended in the liquid for a time. There are multiple forces that dictate how long the colloidal materials are able to be suspended. The wiki article is kinda crazy with the science. Colloids are like dust, on their own you don't really see them. Once they come together (aggregate) then you can.

 

Video of large particles flocculating in space:

 

[Dismal]

I'm not done yet but wanted to update progress.  First let me add that my botanical bill has a few unusual botanicals in it so all past experience may not be applicable here.  

I extracted each botanical individually and added sugar to each.  One botanical, Star Anise clouded up immediately.  The rest stayed clear.  I experimented with Anise and Fennel as substitutes.  Each remained clear with added sugar but Fennel was a better match for my recipe.   

As mentioned,  I was not able to get the Baker's Sugar nut I was able to get a good sized sample of low color, metals and turbidity liquid sugar from Indiana Sugars which is ideal. I ran a batch using the Indiana Syrup and Flocculation occurred quickly even after running it through a haze filter. 

For filtering I followed up on Foreshot's suggestion of using the Borosilicate cartridge filter.  I spoke with TCW and they were very helpful.  My development batch size is small (1 liter) so the TWC filter is not appropriate yet.  To test the approach I used vacuum filtering with paper disk filters.  Here are links to the parts I use:

• Borosilicate Glass Microfiber Filter Paper, 1.1 Micron
• Buchner funnel
• Pump
• Flask

 

The paper filter is an imperfect fit to the Buchner so being super careful to make sure your seal is as good as possible is important.  The results were impressive, much clearer.  But I still got flocculation after a while, even with the high quality syrup.

Lastly I chill filtered the final product.  I put the product in the freezer for hours and ran it through the Buchner in my refrigerator.  So far this seems to be the key.  Absolutely clear.  Time will tell if flocculation occurs.  

My b=botanical concentration was too high in the experiments above so those experiments are worst case scenarios.  I have a batch in process now at what I beleive will be the final botanical concentration, using ordinary crystal sugar and using chill filtering with the borosilicate filter paper.  Fingers crossed and i will report back when I have results.  

[Dismal]

I found some very interesting technical resources that are relevant here. 

Pharmaceutical compounding syrups technology is very relevant.  I found this great presentation that discusses how to preserve a syrup via water/alcohol vs sugar concentrations (starts on page 64) and general syrup technical goodness:  https://www.philadelphia.edu.jo/academics/rmansour/uploads/Pharmaceutics/Solutions.pptx

Great free Sugar Technology textbook: https://onlinelibrary.wiley.com/doi/book/10.1002/9781444314748

I found the exercises in Appendix B particularly helpful.  

Table starting on page 31: https://www.ams.usda.gov/sites/default/files/media/TechnicalProceduresManual[1].pdf

Cool calculator: https://www.vinolab.hr/calculator/gravity-density-sugar-conversions-en19

[Dismal]

I've completed all my experimentation and so i will post one last message here with my final findings.  

In the end what works for me is haze filtering the final product with glass fiber filter.  For my experimentation I used a vacuum filter with a Buchner funnel and these filter papers: https://www.ahlstrom-munksjo.com/products/medical-life-sciences-and-laboratory/laboratory-papers-and-test-filters/micro-glass-micro-quartz-filters/

They're available on Amazon: https://www.amazon.com/gp/product/B006H8XGNC/ref=ppx_yo_dt_b_search_asin_title?ie=UTF8&psc=1

The flocculation occurs because the floc material is polar and the molecules find each other in the liquid and attach +/- and form chains.  Hence the ribbon-like floc.  The glass fibers in the paper are charged/polarized and attract the polar floc molecules especially well.  Thanks to the folks at TCW for setting me in the right direction finally.  

In production I will use my cartridge filter and this cartridge: https://www.tcwequipment.com/products/graver-gfc-haze-pre-filters?taxon_id=69

I also experimented with different sugars.  I looked at Sucrose (ordinary white granular sugar), Belgian Candi Sugar (an adjunct used in certain beers.  can be from beets, corn, invert) and dextrose.  As a simple syrup the Dextrose was crystal clear and less viscus than the others so I was optimistic.  In the end I found no difference between them in my products.  I use a combination of distilled and macerated extractions and so the coloring of the macerated extracts overpowers any clarity that the dextrose produced.  Your mileage may vary here and I can see where Dextrose will be useful in certain recipes.  I found that using 25% more dextrose by weight produces comparable sweetness to sucrose.  

I've produces a few recipes that have shown floc resistance over months using this approach.  

In the final analysis haze filtration with a glass fiber filter is the key.  A good quality /purity of your sugar will help but is distant second.  

I hope this helps anyone dealing with this issue.  Little is written about this that I could find.  

[LuckyGuy]

anyone have any links to distillation equipment for use in sugared spirits?   I"m having trouble with the roto evaporator, and maybe it's because the instructions are translated from Chinese and completely unhelpful.

I just need to get the TTB distillation 96ml from a 100ml sample....and my heavily sugared and altered coffee liqueur is proving to be a real challenge......

I'd take any easier road, even if it came with some extra cost at this point.  Last two recommendations I got from folks are dead links to businesses that no longer sell distillation kits.

[meerkat]

Rotavaps often come with vacuum pumps, so if you are pulling a vacuum you must make sure that your cooling water temperature is low enough to condense the alcohol that is evaporated. Generally with rotavaps it is the solids that are left behind that you want, but in this case it is the evaporated alcohol that is the important bit. Turn the vacuum pump off if you can.

High solids can also cause problems when working strictly to the TTB method.  See my earlier post at

 

 

[Dismal]

More to add for future reference ...

Fining (per glisade above) makes a huge difference.  In my case I tested Kieselsol/Chitosan, Bentonite, Spakalloid and Albumin.  I tested these on multiple recipes (Amaro, herbal liqueur similar to Chartreuse and Vermouth).  In my experiments Kieselsol/Chitosan was always performed best.  Best clarity, lowest impact on aroma and taste, most compact bed, fastest results and easiest filtering.  Albumen is a good second choice.  Bentonite performed well but did not achieve the clarity that Kieselsol/Chitosan did and was hard on the filter due to low bed compaction and lower precipitation. 

As far as sugar goes white sugar can be made to work, but a low-color syrup such as Indiana Sugar's low-color distiller's syrup produces the clearest, lowest floc product by far: https://www.sugars.com/product-catalog/all-products/distillery-grade-invert-sugar-syrup