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CalwiseSpirits

Precipitate in triple sec

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I'm making a clear orange liqueur by distilling brandy with orange peel in my gin basket and then proofing down with a syrup I make from cane sugar and water. It comes out clear, but I notice a week later there is some precipitate or sediment in it. My best guess is it's the sugar coming out of solution since it's not soluble in alcohol, but I thought I was avoiding that by dissolving it in the water and making the syrup beforehand. Anyone know what's going on and how to fix it?

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If you can get it to entirely dissolve in a room temperature mixture of ethanol/water, it should be stable.  You'd need to go out of your way to create a heated supersaturated solution that would precipitate out when cooled.

Sounds like something else.

What kind of water are you using for proofing and to make your syrup?  Is it at least a good quality RO or RO/DI?

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10 hours ago, Silk City Distillers said:

If you can get it to entirely dissolve in a room temperature mixture of ethanol/water, it should be stable.  You'd need to go out of your way to create a heated supersaturated solution that would precipitate out when cooled.

Sounds like something else.

What kind of water are you using for proofing and to make your syrup?  Is it at least a good quality RO or RO/DI?

Yep, I'm using an RO system from US Water Systems. 

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1 hour ago, CalwiseSpirits said:

Yep, I'm using an RO system from US Water Systems

Just to properly flog this dead horse... you've checked conductivity on the out side of the RO system?

 

 

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7 minutes ago, indyspirits said:

Just to properly flog this dead horse... you've checked conductivity on the out side of the RO system?

 

 

I have not. Has this already been discussed before in another thread?

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34 minutes ago, CalwiseSpirits said:

I have not. Has this already been discussed before in another thread?

Maybe? Im a bit surprised USW didnt give you at least a cheapy TDS pen. You can get them on amazon.

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Very unlikely it is sugar. Silly question, assume you are not using peel from consumer oranges that have protective waxes on them? While the oils from orange should not precipitate, coating materials might.

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On 8/7/2018 at 5:28 PM, indyspirits said:

Maybe? Im a bit surprised USW didnt give you at least a cheapy TDS pen. You can get them on amazon.

Just bought a TDS pen, going to check!

On 8/8/2018 at 1:23 PM, bluestar said:

Very unlikely it is sugar. Silly question, assume you are not using peel from consumer oranges that have protective waxes on them? While the oils from orange should not precipitate, coating materials might.

I've been getting the oranges from a food distributor. Looked at the box, and yes, they are coated with wax. I'm getting another batch of oranges direct from a grower without any coatings. I'm curious to see if that changes things!

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8 minutes ago, CalwiseSpirits said:

Just bought a TDS pen, going to check!

I've been getting the oranges from a food distributor. Looked at the box, and yes, they are coated with wax. I'm getting another batch of oranges direct from a grower without any coatings. I'm curious to see if that changes things!

You DEFINITELY don't want to use wax-coated oranges. And you can't really get the wax off, without also removing some of the oils you are looking to extract from the peel. I would not be surprised if this changes things for the better for you. Good luck!

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On 8/13/2018 at 10:25 AM, bluestar said:

You DEFINITELY don't want to use wax-coated oranges. And you can't really get the wax off, without also removing some of the oils you are looking to extract from the peel. I would not be surprised if this changes things for the better for you. Good luck!

Update... according to my TDS pen my sink water is 635 ppm and my RO water is 265 ppm. This seems awfully high. I'm not sure if I believe it because the water tastes pretty darn neutral to me. My next step is to test it on distilled water to make sure the pen is working right.

However, I switched to oranges straight from the farm that are not wax coated. Haven't seen precipitate show up since. Maybe that was the trick!

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8 hours ago, CalwiseSpirits said:

RO water is 265 ppm

Eeek! That's not good. Our is about 360 coming in (softened) and 3 out. Is your feed water softened? First I'd verify your TDS pen is working with some distilled water.  If it is, looks like you need to replace your membrane.

 

 

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Check the plumbing and RO housing while you are at it.  That high of a TDS sometimes means untreated water is bypassing the membrane to the output.

Also - if you have a holding tank or final polish carbon filter - those could be a problem.

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High TDS permeate can be caused by a lot of factors.  For example:

exhausted carbon prefilter(s) have allowed chlorine to get to the membrane for an extended period
membrane is scaled/fouled and has failed
RO membrane housing/internal orings have failed
and not uncommonly, it's caused by faulty TDS readings.  Make sure you let the system run for sufficient time to get past the TDS Creep period before you take a reading/sample.  Be careful  what you use for a sample container.  ANY contamination in the container will cause faulty readings.

If you need some help troubleshooting the system, feel free to give us a call when you're standing in front of it.
 

Russ @ Buckeye Hydro
513-312-2343 

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On 8/30/2018 at 12:12 AM, CalwiseSpirits said:

Update... according to my TDS pen my sink water is 635 ppm and my RO water is 265 ppm. This seems awfully high. I'm not sure if I believe it because the water tastes pretty darn neutral to me. My next step is to test it on distilled water to make sure the pen is working right.

However, I switched to oranges straight from the farm that are not wax coated. Haven't seen precipitate show up since. Maybe that was the trick!

Did you ever see any further precipitation on the batch done with uncoated oranges? Just thought I would follow up.

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Thank you for that offer @Buckeye Hydro, I may take you up on that soon. 

I have not had any issues since. I'm still not sure what it was because I still use coated oranges sometimes when I can't get them direct from the farmer. 

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On 1/23/2019 at 11:54 AM, CalwiseSpirits said:

Thank you for that offer @Buckeye Hydro, I may take you up on that soon. 

I have not had any issues since. I'm still not sure what it was because I still use coated oranges sometimes when I can't get them direct from the farmer. 

Is it precipitating before or after filtration?  Since it is after proof reduction, it could have been the high TDS since RO should be below 30 PPM (my opinion) and minerals (especially calcium) are known to cause floc - or it could be from the sugar itself.  I'm not sure what it's properly called, but I've found some brands of sugars will form small crystals over a week or so of resting.  Lots of unknowns here but it sounds like you've got it worked out none-the-less. Cheers.

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