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Oils in Distillate After Vapor Infusion With Fresh Citrus


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We're experimenting with gin and would really love to put citruses in the basket.

We cut up some citruses in half, placed them all in the basket for vapor infusion, used about 90 proof to run a distillation, diluted the hearts (about 170 proof) back down to about 100 proof and let it rest for a couple of days. All was well until we found a layer of oil and the distillate milky, I assume from the oils.

We've done other distillations and vapor infusions with other botanicals without this problem so we're wondering if anyone could help us answer these questions:

1) Why did it happen?
2) How can it be prevented if we insist to do a vapor infusion with citruses? (E.g. Put less citrus? Use lower proof to distill? Faster/slower distillation...?)
3) Any techniques to clear up the currently "oily" distillate?

Any advice would be highly appreciated!

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Are you making a heads cut to avoid louching of juniper and citrus oils? I sample my gin distillate and dilute 50/50 with RO and don't start my hearts collection until I reach a sample that doesn't louche. Has worked well for me

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On 4/5/2021 at 3:42 AM, tgf said:

3) Any techniques to clear up the currently "oily" distillate?

The best way I've been taught to clear up cloudy distillate is to blend more of your neutral spirit in at the same proof that you're hoping to bottle at. For example, it's currently at 100 proof, correct? Dilute down neutral spirit to 100 proof and slowly blend that into the cloudy gin. Depending on how bad the louch is, you may need to blend quite a bit of NGS in. After enough neutral is blended in, the oils that causes louching will remain dissolved and the spirit will clear up.

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Did you bring it straight from 170 down to 100? Try stepping the proof down more gradually to prevent flocc/haze, especially when approaching that 100 proof mark or lower. 

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Also, don't use the entire citrus - rather, just use the zest. We've found using the whole fruit does tend to create more of a problem. 

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  • 2 weeks later...

Thank you everyone for your insights!

We did a couple more distillations and got some very interesting findings, perhaps this will help shine a light on what's going on and hopefully we can find out how to stabilize distilling whole citrus fruits via vapor infusion.

Our method largely remained unchanged:
1. We cut up the citruses in half, placed them all in the basket for vapor infusion (no juniper berries for now to eliminate a factor)
2. We used about 90 proof to run a distillation
3. The hearts came out about 170 proof and we diluted it with RO down to 100 proof.


First Batch Trial:
1. Followed @Brewstilla's advice and sampled the heads cut - diluting the distillate with 50/50 RO until no louching was found before collecting hearts.
2. Found that the heads did indeed louch with the added 50/50 RO, but after ten minutes or so, every single louched sample cleared up magically after some stirring and never turned hazy again. On average they were about 100 proof.
3. The hearts, however came out extremely louched after diluting it down to about 100 proof, even after letting it rest for a week.


Second Batch Trial:
1. Followed @kleclerc77's advice and diluted the hearts slowly this time to prevent haze while simultaneously stirring vigorously. The hearts did not louch - amazing.
2. After seeing the successful result of our second batch, we returned back to the louched first batch and gave it some vigorous stirring and magically, the hearts cleared up completely.


Bottling:
After doing the two trial runs above, we decided to bottle the first batch and see what would happened. All was good until about an hour or so after bottling and more than half the bottles began to show up hazy again, while some remained clear. We decided not to do anything just yet and let them sit overnight... and found all the bottles cleared up again by itself the next morning.


Major Questions:
1. Could anyone help draw some conclusions as to why the hearts clear up initially after a long time of vigorous stirring?
2. After the hearts cleared up, why did it louch temporarily after bottling, then cleared up by itself again?


Again, we appreciate any advice and thanks everyone for your input.

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7 hours ago, tgf said:

Major Questions:
1. Could anyone help draw some conclusions as to why the hearts clear up initially after a long time of vigorous stirring?
2. After the hearts cleared up, why did it louch temporarily after bottling, then cleared up by itself again?


Again, we appreciate any advice and thanks everyone for your input.

1. This question is a bit tricky. One of the main reasons I could think of is stratification due to inadequate mixing when you originally added the water.

2. Were the bottles cold? Was the bottling room cold? Temperature also affects solubility of oils in spirits and could account for a temporary louching if they got cold during bottling

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It's oils that have been shocked out of solution and will not re-dissolve. Once they have come out of solution, getting them back in solution is challenging. The best way we have found (without chill filtering, anyway) is as soon as you notice any haze/flocc, bring the proof up with higher proof spirits. Heating and agitating can also help, but maybe not permanently. It's the cold that really does it for us. Because of the extreme cold temps in the winter, we find ourselves needing to bottle at a higher proof. If you're not willing to make that trade-off, chill filtration may be your only foolproof way to avoid haze/flocc.

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