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Freeze distillation

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  • waljaco
    Although the article is cloaked in pseudo-alchemy jargon, and purports to be aboutr distilling vinegar, the technique applies to spirit of wine also: Spirit
    Message 1 of 9 , Mar 17, 2003
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      Although the article is cloaked in pseudo-alchemy jargon, and
      purports to be aboutr distilling vinegar, the technique applies
      to 'spirit of wine' also:
      Spirit of Vinegar
      http://www.terravista.pt/mussulo/2005/spvinegr_e.htm

      Wal
    • Timothy C Smoth
      I thought it might do good to recommend reading about freeze distillation. There are quite a few write ups available on line. One of the easiest to understand
      Message 2 of 9 , Dec 26, 2012
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        I thought it might do good to recommend reading about freeze distillation.
        There are quite a few write ups available on line. One of the easiest to understand is at home distillers dot org wiki page. A simple web search can lead to many good reads.

        Freeze distillation has been used ever since fermentation got noticed thousands of years ago. It's not a new discovery by any means. There are a lot of good reasons not to rely on the final product. A bad hang over is nothing compared to toxicity from ingesting acetone or methanol.
        Even as a method to concentrate a ferment before distillation, freezing allows a certain percentage of ethanol to get stuck in with the ice. Freezing does not allow many unwanted by-products to be removed.
        I have read of a few methods that over came some of the basic drawbacks. One of which is to freeze, slightly thaw, freeze at colder temperature, raise temp. slightly, freeze colder again, and do that repeatedly until the coldest temperature your freezer can achieve is met. What a hassle.

        Sent from Tim's iPhone
      • henry sangret
        I have read up on the process and experienced the results first hand LOL. I will stay with the tried and true  process and continue to enjoy the results.
        Message 3 of 9 , Dec 26, 2012
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          I have read up on the process and experienced the results first hand LOL. I will stay with the tried and true  process and continue to enjoy the results. Happy Holidays.

          From: Timothy C Smoth <timothyc.smith@...>
          To: "Distillers@yahoogroups.com" <Distillers@yahoogroups.com>
          Sent: Wednesday, December 26, 2012 10:01 AM
          Subject: [Distillers] Freeze distillation
           
          I thought it might do good to recommend reading about freeze distillation.
          There are quite a few write ups available on line. One of the easiest to understand is at home distillers dot org wiki page. A simple web search can lead to many good reads.

          Freeze distillation has been used ever since fermentation got noticed thousands of years ago. It's not a new discovery by any means. There are a lot of good reasons not to rely on the final product. A bad hang over is nothing compared to toxicity from ingesting acetone or methanol.
          Even as a method to concentrate a ferment before distillation, freezing allows a certain percentage of ethanol to get stuck in with the ice. Freezing does not allow many unwanted by-products to be removed.
          I have read of a few methods that over came some of the basic drawbacks. One of which is to freeze, slightly thaw, freeze at colder temperature, raise temp. slightly, freeze colder again, and do that repeatedly until the coldest temperature your freezer can achieve is met. What a hassle.

          Sent from Tim's iPhone
        • RLB
          Thank you for this info, and you are correct about everything that you stated pertaining to Freeze Distillation.  Those possible dangers are why I have not
          Message 4 of 9 , Dec 26, 2012
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            Thank you for this info, and you are correct about everything that you stated pertaining to Freeze Distillation.  Those possible dangers are why I have not tried consuming my concentrated wash.  My future plans include processing my concentrate through a still, which I hope to acquire in January to further my experiments.

            Freeze distillation is very labor intensive, but my wash samples need to be reduced for storage until they can be processed further.  Since freeze distillation is an interesting process that allows for the removal of water without the dangers of explosions, my experiments will review whether or not freeze distillation offers any benefit to the production of Ethanol for use as spirits.

            I am new to distillation, so my experiments will wander in many directions to obtain answers to my many questions.  In my readings, there are a minimum of 6 different types of Monohydric alcohols with different boiling points.   Can freeze distillation be used to remove some of these unwanted alcohol compounds from wash prior to distillation?

            Robert
             






            From: Timothy C Smoth <timothyc.smith@...>
            To: "Distillers@yahoogroups.com" <Distillers@yahoogroups.com>
            Sent: Wednesday, December 26, 2012 10:01 AM
            Subject: [Distillers] Freeze distillation

             
            I thought it might do good to recommend reading about freeze distillation.
            There are quite a few write ups available on line. One of the easiest to understand is at home distillers dot org wiki page. A simple web search can lead to many good reads.

            Freeze distillation has been used ever since fermentation got noticed thousands of years ago. It's not a new discovery by any means. There are a lot of good reasons not to rely on the final product. A bad hang over is nothing compared to toxicity from ingesting acetone or methanol.
            Even as a method to concentrate a ferment before distillation, freezing allows a certain percentage of ethanol to get stuck in with the ice. Freezing does not allow many unwanted by-products to be removed.
            I have read of a few methods that over came some of the basic drawbacks. One of which is to freeze, slightly thaw, freeze at colder temperature, raise temp. slightly, freeze colder again, and do that repeatedly until the coldest temperature your freezer can achieve is met. What a hassle.

            Sent from Tim's iPhone


          • Fredrick Lee
            You have to know the freezing point of each alcohol and solve the math for the eutectic state of that solution. Since many of these alcohols freeze in the
            Message 5 of 9 , Dec 26, 2012
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              You have to know the freezing point of each alcohol and solve the math for the eutectic state of that solution. Since many of these alcohols freeze in the -70°F range you probably aren't going to be able to do it at home. Accurate fractional freezing requires the math and knowledge of the items in solution.  Freeze distillation is essentially the opposite problem of solving for your azeotrope when regular distilling.  Since ethanol is soluble in water, you probably will see a limit around 40% abv in a regular home freezer. The colder it gets, the more ethanol that's being trapped in your ice water, and you'll end up throwing away much more than you could distill out by volume. It's fun to play with booze though! 



              Again, if its just about storage, then sterility and keeping it closed up until ready to use, is the easiest way to store alcohol indefinitely. 

              On Dec 26, 2012, at 12:59 PM, RLB <last2blast@...> wrote:

               

              Thank you for this info, and you are correct about everything that you stated pertaining to Freeze Distillation.  Those possible dangers are why I have not tried consuming my concentrated wash.  My future plans include processing my concentrate through a still, which I hope to acquire in January to further my experiments.

              Freeze distillation is very labor intensive, but my wash samples need to be reduced for storage until they can be processed further.  Since freeze distillation is an interesting process that allows for the removal of water without the dangers of explosions, my experiments will review whether or not freeze distillation offers any benefit to the production of Ethanol for use as spirits.

              I am new to distillation, so my experiments will wander in many directions to obtain answers to my many questions.  In my readings, there are a minimum of 6 different types of Monohydric alcohols with different boiling points.   Can freeze distillation be used to remove some of these unwanted alcohol compounds from wash prior to distillation?

              Robert
               






              From: Timothy C Smoth <timothyc.smith@...>
              To: "Distillers@yahoogroups.com" <Distillers@yahoogroups.com>
              Sent: Wednesday, December 26, 2012 10:01 AM
              Subject: [Distillers] Freeze distillation

               
              I thought it might do good to recommend reading about freeze distillation.
              There are quite a few write ups available on line. One of the easiest to understand is at home distillers dot org wiki page. A simple web search can lead to many good reads.

              Freeze distillation has been used ever since fermentation got noticed thousands of years ago. It's not a new discovery by any means. There are a lot of good reasons not to rely on the final product. A bad hang over is nothing compared to toxicity from ingesting acetone or methanol.
              Even as a method to concentrate a ferment before distillation, freezing allows a certain percentage of ethanol to get stuck in with the ice. Freezing does not allow many unwanted by-products to be removed.
              I have read of a few methods that over came some of the basic drawbacks. One of which is to freeze, slightly thaw, freeze at colder temperature, raise temp. slightly, freeze colder again, and do that repeatedly until the coldest temperature your freezer can achieve is met. What a hassle.

              Sent from Tim's iPhone


            • RLB
              40% abv. at least because I can know longer work around my considerate it without getting a buzz from those fumes.  There is most likely a little alcohol in
              Message 6 of 9 , Dec 26, 2012
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                40% abv. at least because I can know longer work around my considerate it without getting a buzz from those fumes.  There is most likely a little alcohol in the ice after its pressed, but I am able to recover most of the free liquid.  At this time, 23 oz. of  considerate is being stored from sample 12/16/12, and it will be interesting to see how much water remains after my first striping run.  This sample tested at 10 proof at 35 F, and all of the other samples tested at "0" proof at 35 F.  It's not a true reading, but it gives me a future reference point.  

                Another thought, do I really need to drink if all I have to do is open a jar of considerate to get a buzz?

                I freeze distill only to reduce storage capacity until a still can be obtained.  Freeze distilling will stop once a still is available unless there is an unforeseen  benefit to freeze distillation.

                Robert



                From: Fredrick Lee <fredrick@...>
                To: "Distillers@yahoogroups.com" <Distillers@yahoogroups.com>
                Sent: Wednesday, December 26, 2012 1:56 PM
                Subject: Re: [Distillers] Freeze distillation

                 
                You have to know the freezing point of each alcohol and solve the math for the eutectic state of that solution. Since many of these alcohols freeze in the -70°F range you probably aren't going to be able to do it at home. Accurate fractional freezing requires the math and knowledge of the items in solution.  Freeze distillation is essentially the opposite problem of solving for your azeotrope when regular distilling.  Since ethanol is soluble in water, you probably will see a limit around 40% abv in a regular home freezer. The colder it gets, the more ethanol that's being trapped in your ice water, and you'll end up throwing away much more than you could distill out by volume. It's fun to play with booze though! 



                Again, if its just about storage, then sterility and keeping it closed up until ready to use, is the easiest way to store alcohol indefinitely. 

                On Dec 26, 2012, at 12:59 PM, RLB <last2blast@...> wrote:

                 
                Thank you for this info, and you are correct about everything that you stated pertaining to Freeze Distillation.  Those possible dangers are why I have not tried consuming my concentrated wash.  My future plans include processing my concentrate through a still, which I hope to acquire in January to further my experiments.

                Freeze distillation is very labor intensive, but my wash samples need to be reduced for storage until they can be processed further.  Since freeze distillation is an interesting process that allows for the removal of water without the dangers of explosions, my experiments will review whether or not freeze distillation offers any benefit to the production of Ethanol for use as spirits.

                I am new to distillation, so my experiments will wander in many directions to obtain answers to my many questions.  In my readings, there are a minimum of 6 different types of Monohydric alcohols with different boiling points.   Can freeze distillation be used to remove some of these unwanted alcohol compounds from wash prior to distillation?

                Robert
                 






                From: Timothy C Smoth <timothyc.smith@...>
                To: "Distillers@yahoogroups.com" <Distillers@yahoogroups.com>
                Sent: Wednesday, December 26, 2012 10:01 AM
                Subject: [Distillers] Freeze distillation

                 
                I thought it might do good to recommend reading about freeze distillation.
                There are quite a few write ups available on line. One of the easiest to understand is at home distillers dot org wiki page. A simple web search can lead to many good reads.

                Freeze distillation has been used ever since fermentation got noticed thousands of years ago. It's not a new discovery by any means. There are a lot of good reasons not to rely on the final product. A bad hang over is nothing compared to toxicity from ingesting acetone or methanol.
                Even as a method to concentrate a ferment before distillation, freezing allows a certain percentage of ethanol to get stuck in with the ice. Freezing does not allow many unwanted by-products to be removed.
                I have read of a few methods that over came some of the basic drawbacks. One of which is to freeze, slightly thaw, freeze at colder temperature, raise temp. slightly, freeze colder again, and do that repeatedly until the coldest temperature your freezer can achieve is met. What a hassle.

                Sent from Tim's iPhone




              • abbababbaccc
                It s no more dangerous than drinking wine or beer in excess. Freeze distilled stuff is just beer or wine (or whatever mash you use) where water content has
                Message 7 of 9 , Dec 27, 2012
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                  It's no more dangerous than drinking wine or beer in excess. Freeze distilled stuff is just beer or wine (or whatever mash you use) where water content has been reduced. If you start with good product you'll end up with good product and vice versa.

                  Slainte, Riku

                  --- In Distillers@yahoogroups.com, Timothy C Smoth <timothyc.smith@...> wrote:
                  >
                  > I thought it might do good to recommend reading about freeze distillation.
                  > There are quite a few write ups available on line. One of the easiest to understand is at home distillers dot org wiki page. A simple web search can lead to many good reads.
                  >
                  > Freeze distillation has been used ever since fermentation got noticed thousands of years ago. It's not a new discovery by any means. There are a lot of good reasons not to rely on the final product. A bad hang over is nothing compared to toxicity from ingesting acetone or methanol.
                  > Even as a method to concentrate a ferment before distillation, freezing allows a certain percentage of ethanol to get stuck in with the ice. Freezing does not allow many unwanted by-products to be removed.
                  > I have read of a few methods that over came some of the basic drawbacks. One of which is to freeze, slightly thaw, freeze at colder temperature, raise temp. slightly, freeze colder again, and do that repeatedly until the coldest temperature your freezer can achieve is met. What a hassle.
                  >
                  > Sent from Tim's iPhone
                  >
                • henry sangret
                  I have tried the freeze process and the unwanted s seem to have increased by 5 to 7% in volume and the ABV dropped by aprox the same. I think the Methanol and
                  Message 8 of 9 , Dec 29, 2012
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                    I have tried the freeze process and the unwanted's seem to have increased by 5 to 7% in volume and the ABV dropped by aprox the same. I think the Methanol and MEK normally lost in distiillation stays trapped in the unfrozen liquids and some of the alcohol stays trapped in the ice, which accou nts for the increases and losses.
                     
                    For storage I use a simple pot still to reduce the volume by aprox half and save the distillate in a large carbloy until enough is saved to do a large batch run again.

                    From: Fredrick Lee <fredrick@...>
                    To: "Distillers@yahoogroups.com" <Distillers@yahoogroups.com>
                    Sent: Wednesday, December 26, 2012 1:56 PM
                    Subject: Re: [Distillers] Freeze distillation
                     
                    You have to know the freezing point of each alcohol and solve the math for the eutectic state of that solution. Since many of these alcohols freeze in the -70°F range you probably aren't going to be able to do it at home. Accurate fractional freezing requires the math and knowledge of the items in solution.  Freeze distillation is essentially the opposite problem of solving for your azeotrope when regular distilling.  Since ethanol is soluble in water, you probably will see a limit around 40% abv in a regular home freezer. The colder it gets, the more ethanol that's being trapped in your ice water, and you'll end up throwing away much more than you could distill out by volume. It's fun to play with booze though! 



                    Again, if its just about storage, then sterility and keeping it closed up until ready to use, is the easiest way to store alcohol indefinitely. 
                    On Dec 26, 2012, at 12:59 PM, RLB <last2blast@...> wrote:
                     
                    Thank you for this info, and you are correct about everything that you stated pertaining to Freeze Distillation.  Those possible dangers are why I have not tried consuming my concentrated wash.  My future plans include processing my concentrate through a still, which I hope to acquire in January to further my experiments. Freeze distillation is very labor intensive, but my wash samples need to be reduced for storage until they can be processed further.  Since freeze distillation is an interesting process that allows for the removal of water without the dangers of explosions, my experiments will review whether or not freeze distillation offers any benefit to the production of Ethanol for use as spirits. I am new to distillation, so my experiments will wander in many directions to obtain answers to my many questions.  In my readings, there are a minimum of 6 different types of Monohydric alcohols with different boiling points.   Can freeze distillation be used to remove some of these unwanted alcohol compounds from wash prior to distillation? Robert  

                    From: Timothy C Smoth <timothyc.smith@...>
                    To: "Distillers@yahoogroups.com" <Distillers@yahoogroups.com>
                    Sent: Wednesday, December 26, 2012 10:01 AM
                    Subject: [Distillers] Freeze distillation
                     
                    I thought it might do good to recommend reading about freeze distillation. There are quite a few write ups available on line. One of the easiest to understand is at home distillers dot org wiki page. A simple web search can lead to many good reads. Freeze distillation has been used ever since fermentation got noticed thousands of years ago. It's not a new discovery by any means. There are a lot of good reasons not to rely on the final product. A bad hang over is nothing compared to toxicity from ingesting acetone or methanol. Even as a method to concentrate a ferment before distillation, freezing allows a certain percentage of ethanol to get stuck in with the ice. Freezing does not allow many unwanted by-products to be removed. I have read of a few methods that over came some of the basic drawbacks. One of which is to freeze, slightly thaw, freeze at colder temperature, raise temp. slightly, freeze colder again, and do that repeatedly until the coldest temperature your freezer can achieve is met. What a hassle. Sent from Tim's iPhone
                     
                  • RLB
                    Normally, I would agree with you on freeze distillation but try pressing the ice to remove as much liquid as possible.  In my last 2 freeze distilled samples,
                    Message 9 of 9 , Dec 30, 2012
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                      Normally, I would agree with you on freeze distillation but try pressing the ice to remove as much liquid as possible.  In my last 2 freeze distilled samples, my liquid reached 23 oz., and I was feeling fairly good.  If you can achieve a buzz like that from just inhaling the wash fumes, it says a great deal about the Ethanol content.  One showed no proof, and the second sample was listed at 10 proof @ 33 F.  Since those 2 sample still contain yeast and solids, any alcohol reading would not be correct.

                      Robert



                      From: henry sangret <henrysangret@...>
                      To: "Distillers@yahoogroups.com" <Distillers@yahoogroups.com>
                      Sent: Saturday, December 29, 2012 3:32 PM
                      Subject: Re: [Distillers] Freeze distillation

                       
                      I have tried the freeze process and the unwanted's seem to have increased by 5 to 7% in volume and the ABV dropped by aprox the same. I think the Methanol and MEK normally lost in distiillation stays trapped in the unfrozen liquids and some of the alcohol stays trapped in the ice, which accou nts for the increases and losses.
                       
                      For storage I use a simple pot still to reduce the volume by aprox half and save the distillate in a large carbloy until enough is saved to do a large batch run again.

                      From: Fredrick Lee <fredrick@...>
                      To: "Distillers@yahoogroups.com" <Distillers@yahoogroups.com>
                      Sent: Wednesday, December 26, 2012 1:56 PM
                      Subject: Re: [Distillers] Freeze distillation
                       
                      You have to know the freezing point of each alcohol and solve the math for the eutectic state of that solution. Since many of these alcohols freeze in the -70°F range you probably aren't going to be able to do it at home. Accurate fractional freezing requires the math and knowledge of the items in solution.  Freeze distillation is essentially the opposite problem of solving for your azeotrope when regular distilling.  Since ethanol is soluble in water, you probably will see a limit around 40% abv in a regular home freezer. The colder it gets, the more ethanol that's being trapped in your ice water, and you'll end up throwing away much more than you could distill out by volume. It's fun to play with booze though! 



                      Again, if its just about storage, then sterility and keeping it closed up until ready to use, is the easiest way to store alcohol indefinitely. 
                      On Dec 26, 2012, at 12:59 PM, RLB <last2blast@...> wrote:
                       
                      Thank you for this info, and you are correct about everything that you stated pertaining to Freeze Distillation.  Those possible dangers are why I have not tried consuming my concentrated wash.  My future plans include processing my concentrate through a still, which I hope to acquire in January to further my experiments. Freeze distillation is very labor intensive, but my wash samples need to be reduced for storage until they can be processed further.  Since freeze distillation is an interesting process that allows for the removal of water without the dangers of explosions, my experiments will review whether or not freeze distillation offers any benefit to the production of Ethanol for use as spirits. I am new to distillation, so my experiments will wander in many directions to obtain answers to my many questions.  In my readings, there are a minimum of 6 different types of Monohydric alcohols with different boiling points.   Can freeze distillation be used to remove some of these unwanted alcohol compounds from wash prior to distillation? Robert  

                      From: Timothy C Smoth <timothyc.smith@...>
                      To: "Distillers@yahoogroups.com" <Distillers@yahoogroups.com>
                      Sent: Wednesday, December 26, 2012 10:01 AM
                      Subject: [Distillers] Freeze distillation
                       
                      I thought it might do good to recommend reading about freeze distillation. There are quite a few write ups available on line. One of the easiest to understand is at home distillers dot org wiki page. A simple web search can lead to many good reads. Freeze distillation has been used ever since fermentation got noticed thousands of years ago. It's not a new discovery by any means. There are a lot of good reasons not to rely on the final product. A bad hang over is nothing compared to toxicity from ingesting acetone or methanol. Even as a method to concentrate a ferment before distillation, freezing allows a certain percentage of ethanol to get stuck in with the ice. Freezing does not allow many unwanted by-products to be removed. I have read of a few methods that over came some of the basic drawbacks. One of which is to freeze, slightly thaw, freeze at colder temperature, raise temp. slightly, freeze colder again, and do that repeatedly until the coldest temperature your freezer can achieve is met. What a hassle. Sent from Tim's iPhone
                       


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