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Re: [Distillers] Soxhlet Extractors & Rotary Evaporators

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  • Bryan Bornais
    Soxhlet extration is good for extracting very insoluble materials. I suppose you could use it to extract botanicals into a super concentrated tincture. The
    Message 1 of 20 , May 8, 2012
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      Soxhlet extration is good for extracting very insoluble materials. I suppose you could use it to extract botanicals into a super concentrated tincture. The reflux would be pretty harsh on the plant matter, so long run times would probably not be recommended. I would think of shaping a piece of SS mesh into something that fits into it, so it is food grade, and re-usable.
       
      The rotovap is designed for removing solvent and keeping the organic compounds left behind. The solvent (pot) side is heated with a water bath, and vacuum is applied to cause evaporation below the bp of many solvents. The biggest issue I have had with those is 'bumping', where the solvent jumps over to your recovery flask, and you have to start the whole distillation over, after cleaning the condenser and recovery flask. My advice would be to watch your vacuum, and purge as needed, or just scrap the vacuum all together, and run your boiler hotter. The volume is low on these devices, so I am not sure how useful they will be in the long run.
       
      Cheers

      From: daryl_bee <darylbender@...>
      To: Distillers@yahoogroups.com
      Sent: Saturday, May 5, 2012 10:54:16 AM
      Subject: [Distillers] Soxhlet Extractors & Rotary Evaporators

       
      Hi

      I thought I'd take distilling to a whole new level and picked up a giant Soxhlet extractor and a Buchi Rotary evaporator (still need to get some glassware for it). I was wondering if anybody here has any experience using either of these and could offer advice before I dive in?

      The cellulose extractor thimbles for the giant Soxhlet are $50-$60 each ($460 for 25). I was wondering if sterile gauze (some on the bottom, under the botanicals, some on top) would work as well?

      The one thing I don't have for the rotary evaporator is a vacuum controller and would like some advice on this. Any advice or experience operating one would be welcome too. So far the best I found was this from the French Culinary Institutes's Tech Blog;

      http://www.cookingissues.com/primers/rotovap/

      My initial aim is to generate essential oils from botanicals which could be used for flavouring and aroma of a whole myriad of things. By all accounts this should be a powerful combination beating water distillation by a long shot (although I could do that too). The possibilities seem endless. Everything from rose petals, gin, herbs etc. In the link above they even mentioned going into the deep forest for earth (to strip the essentials) to impart a woodsy flavour to a dish! Stripping the flavours off Habernero peppers & leaving the hot behind. The nice thing about the rotary evaporator is I can distill at room temperature not damaging flavour & aroma with heat.

      I tried asking about the Soxhlet in new distillers and was met with resounding silence so, now that I also have the Rotary Evaporator, I thought I'd try here in the advanced forum.

      Thanks



    • daryl_bee
      Hi I was initially a little worried about scratching the glass with a metal mesh but on thinking about it I could probably use silcone O rings as bumpers for
      Message 2 of 20 , May 8, 2012
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        Hi

        I was initially a little worried about scratching the glass with a metal mesh but on thinking about it I could probably use silcone "O" rings as bumpers for when putting it into the receiver. My "solvent" flask is 3 liters and the receiver (for the botanicals) is 1.5 liter and 3.75" inside dia! Like I said this thing is big ~ 4ft tall without the heating mantle! Unfortunately I'm still waiting for a heating mantle power cord, some silicone tubing for cooling lines and the arrival of my 26 gal compound still to finalize the "solvent".

        I'm thinking that a single soxhlet cycle on something like berries would be like 2 week soak in a bottle of alcohol where as something like wood chips would take several cycles. Does this sound right?

        My rotary evaporator will have 2 liter solvent & recovery flasks which I think should harmonize well with the soxhlet. I'm only using it to generate the essentials/flavours so 2 liters should be lots

        How do you control the vacuum? I have heard some people use needle valves and some use a controller ($$). How do you gauge the vacuum with a needle valve? The vacuum gauges I've seen are 0 to -30"hg and not what I would think are accurate for controlling vacuum in the millibar range (my Welch vacuum pump should go down to .02 torr (0.0003867355psi) so somewhere between there and 50 torr is where all the action is (atmosphere is 760 torr).

        Maybe I'm crazy for undertaking this but the idea of things like fresh vanilla (vs bought extract) or making my own Benedictine from scratch seem irresistible to me.

        Thanks!



        --- In Distillers@yahoogroups.com, Bryan Bornais <bbornais@...> wrote:
        >
        > Soxhlet extration is good for extracting very insoluble materials. I suppose you could use it to extract botanicals into a super concentrated tincture. The reflux would be pretty harsh on the plant matter, so long run times would probably not be recommended. I would think of shaping a piece of SS mesh into something that fits into it, so it is food grade, and re-usable.
        >  
        > The rotovap is designed for removing solvent and keeping the organic compounds left behind. The solvent (pot) side is heated with a water bath, and vacuum is applied to cause evaporation below the bp of many solvents. The biggest issue I have had with those is 'bumping', where the solvent jumps over to your recovery flask, and you have to start the whole distillation over, after cleaning the condenser and recovery flask. My advice would be to watch your vacuum, and purge as needed, or just scrap the vacuum all together, and run your boiler hotter. The volume is low on these devices, so I am not sure how useful they will be in the long run.
        >
        > Cheers
        >
        >
        >
        > ________________________________
        > From: daryl_bee <darylbender@...>
        > To: Distillers@yahoogroups.com
        > Sent: Saturday, May 5, 2012 10:54:16 AM
        > Subject: [Distillers] Soxhlet Extractors & Rotary Evaporators
        >
        >
        >  
        > Hi
        >
        > I thought I'd take distilling to a whole new level and picked up a giant Soxhlet extractor and a Buchi Rotary evaporator (still need to get some glassware for it). I was wondering if anybody here has any experience using either of these and could offer advice before I dive in?
        >
        > The cellulose extractor thimbles for the giant Soxhlet are $50-$60 each ($460 for 25). I was wondering if sterile gauze (some on the bottom, under the botanicals, some on top) would work as well?
        >
        > The one thing I don't have for the rotary evaporator is a vacuum controller and would like some advice on this. Any advice or experience operating one would be welcome too. So far the best I found was this from the French Culinary Institutes's Tech Blog;
        >
        > http://www.cookingissues.com/primers/rotovap/
        >
        > My initial aim is to generate essential oils from botanicals which could be used for flavouring and aroma of a whole myriad of things. By all accounts this should be a powerful combination beating water distillation by a long shot (although I could do that too). The possibilities seem endless. Everything from rose petals, gin, herbs etc. In the link above they even mentioned going into the deep forest for earth (to strip the essentials) to impart a woodsy flavour to a dish! Stripping the flavours off Habernero peppers & leaving the hot behind. The nice thing about the rotary evaporator is I can distill at room temperature not damaging flavour & aroma with heat.
        >
        > I tried asking about the Soxhlet in new distillers and was met with resounding silence so, now that I also have the Rotary Evaporator, I thought I'd try here in the advanced forum.
        >
        > Thanks
        >
      • abbababbaccc
        That article is very interesting, I just wonder why do they need the rotating boiler? I mean the rolling action of the boil should be plenty enough. Without
        Message 3 of 20 , May 8, 2012
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          That article is very interesting, I just wonder why do they need the rotating boiler? I mean the rolling action of the boil should be plenty enough. Without the rotation that would be really simple system to set up, well except for the vacuum and bain marie but you get my point.

          I'd suggest you try the system without the vacuum and rotation first. Then if you are not satisfied with the results add vacuum.

          Slainte, Riku

          --- In Distillers@yahoogroups.com, "daryl_bee" <darylbender@...> wrote:
          >
          > Hi
          >
          > I thought I'd take distilling to a whole new level and picked up a giant Soxhlet extractor and a Buchi Rotary evaporator (still need to get some glassware for it). I was wondering if anybody here has any experience using either of these and could offer advice before I dive in?
          >
          > The cellulose extractor thimbles for the giant Soxhlet are $50-$60 each ($460 for 25). I was wondering if sterile gauze (some on the bottom, under the botanicals, some on top) would work as well?
          >
          > The one thing I don't have for the rotary evaporator is a vacuum controller and would like some advice on this. Any advice or experience operating one would be welcome too. So far the best I found was this from the French Culinary Institutes's Tech Blog;
          >
          > http://www.cookingissues.com/primers/rotovap/
          >
          > My initial aim is to generate essential oils from botanicals which could be used for flavouring and aroma of a whole myriad of things. By all accounts this should be a powerful combination beating water distillation by a long shot (although I could do that too). The possibilities seem endless. Everything from rose petals, gin, herbs etc. In the link above they even mentioned going into the deep forest for earth (to strip the essentials) to impart a woodsy flavour to a dish! Stripping the flavours off Habernero peppers & leaving the hot behind. The nice thing about the rotary evaporator is I can distill at room temperature not damaging flavour & aroma with heat.
          >
          > I tried asking about the Soxhlet in new distillers and was met with resounding silence so, now that I also have the Rotary Evaporator, I thought I'd try here in the advanced forum.
          >
          > Thanks
          >
        • waljaco
          See also - http://www.conetech.com/spinning-cone-column.html http://www.conetech.com/spinning-cone-column-video.html Used in the wine industry. wal
          Message 4 of 20 , May 9, 2012
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            See also -

            http://www.conetech.com/spinning-cone-column.html
            http://www.conetech.com/spinning-cone-column-video.html

            Used in the wine industry.

            wal

            --- In Distillers@yahoogroups.com, "abbababbaccc" <abbababbaccc@...> wrote:
            >
            > That article is very interesting, I just wonder why do they need the rotating boiler? I mean the rolling action of the boil should be plenty enough. Without the rotation that would be really simple system to set up, well except for the vacuum and bain marie but you get my point.
            >
            > I'd suggest you try the system without the vacuum and rotation first. Then if you are not satisfied with the results add vacuum.
            >
            > Slainte, Riku
            >
            > --- In Distillers@yahoogroups.com, "daryl_bee" <darylbender@> wrote:
            > >
            > > Hi
            > >
            > > I thought I'd take distilling to a whole new level and picked up a giant Soxhlet extractor and a Buchi Rotary evaporator (still need to get some glassware for it). I was wondering if anybody here has any experience using either of these and could offer advice before I dive in?
            > >
            > > The cellulose extractor thimbles for the giant Soxhlet are $50-$60 each ($460 for 25). I was wondering if sterile gauze (some on the bottom, under the botanicals, some on top) would work as well?
            > >
            > > The one thing I don't have for the rotary evaporator is a vacuum controller and would like some advice on this. Any advice or experience operating one would be welcome too. So far the best I found was this from the French Culinary Institutes's Tech Blog;
            > >
            > > http://www.cookingissues.com/primers/rotovap/
            > >
            > > My initial aim is to generate essential oils from botanicals which could be used for flavouring and aroma of a whole myriad of things. By all accounts this should be a powerful combination beating water distillation by a long shot (although I could do that too). The possibilities seem endless. Everything from rose petals, gin, herbs etc. In the link above they even mentioned going into the deep forest for earth (to strip the essentials) to impart a woodsy flavour to a dish! Stripping the flavours off Habernero peppers & leaving the hot behind. The nice thing about the rotary evaporator is I can distill at room temperature not damaging flavour & aroma with heat.
            > >
            > > I tried asking about the Soxhlet in new distillers and was met with resounding silence so, now that I also have the Rotary Evaporator, I thought I'd try here in the advanced forum.
            > >
            > > Thanks
            > >
            >
          • waljaco
            Vanilla extracts are normally just alcohol infusions. Most elite cooks just scrape the insides of the pod. How do you intend to make Benedictine - a secret
            Message 5 of 20 , May 10, 2012
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              Vanilla extracts are normally just alcohol infusions. Most elite cooks just scrape the insides of the pod.
              How do you intend to make Benedictine - a secret recipe of apparently 27 herbs?
              wal

              --- In Distillers@yahoogroups.com, "daryl_bee" <darylbender@...> wrote:
              >
              > Hi
              >
              > I was initially a little worried about scratching the glass with a metal mesh but on thinking about it I could probably use silcone "O" rings as bumpers for when putting it into the receiver. My "solvent" flask is 3 liters and the receiver (for the botanicals) is 1.5 liter and 3.75" inside dia! Like I said this thing is big ~ 4ft tall without the heating mantle! Unfortunately I'm still waiting for a heating mantle power cord, some silicone tubing for cooling lines and the arrival of my 26 gal compound still to finalize the "solvent".
              >
              > I'm thinking that a single soxhlet cycle on something like berries would be like 2 week soak in a bottle of alcohol where as something like wood chips would take several cycles. Does this sound right?
              >
              > My rotary evaporator will have 2 liter solvent & recovery flasks which I think should harmonize well with the soxhlet. I'm only using it to generate the essentials/flavours so 2 liters should be lots
              >
              > How do you control the vacuum? I have heard some people use needle valves and some use a controller ($$). How do you gauge the vacuum with a needle valve? The vacuum gauges I've seen are 0 to -30"hg and not what I would think are accurate for controlling vacuum in the millibar range (my Welch vacuum pump should go down to .02 torr (0.0003867355psi) so somewhere between there and 50 torr is where all the action is (atmosphere is 760 torr).
              >
              > Maybe I'm crazy for undertaking this but the idea of things like fresh vanilla (vs bought extract) or making my own Benedictine from scratch seem irresistible to me.
              >
              > Thanks!
              >
              >
              >
              > --- In Distillers@yahoogroups.com, Bryan Bornais <bbornais@> wrote:
              > >
              > > Soxhlet extration is good for extracting very insoluble materials. I suppose you could use it to extract botanicals into a super concentrated tincture. The reflux would be pretty harsh on the plant matter, so long run times would probably not be recommended. I would think of shaping a piece of SS mesh into something that fits into it, so it is food grade, and re-usable.
              > >  
              > > The rotovap is designed for removing solvent and keeping the organic compounds left behind. The solvent (pot) side is heated with a water bath, and vacuum is applied to cause evaporation below the bp of many solvents. The biggest issue I have had with those is 'bumping', where the solvent jumps over to your recovery flask, and you have to start the whole distillation over, after cleaning the condenser and recovery flask. My advice would be to watch your vacuum, and purge as needed, or just scrap the vacuum all together, and run your boiler hotter. The volume is low on these devices, so I am not sure how useful they will be in the long run.
              > >
              > > Cheers
              > >
              > >
              > >
              > > ________________________________
              > > From: daryl_bee <darylbender@>
              > > To: Distillers@yahoogroups.com
              > > Sent: Saturday, May 5, 2012 10:54:16 AM
              > > Subject: [Distillers] Soxhlet Extractors & Rotary Evaporators
              > >
              > >
              > >  
              > > Hi
              > >
              > > I thought I'd take distilling to a whole new level and picked up a giant Soxhlet extractor and a Buchi Rotary evaporator (still need to get some glassware for it). I was wondering if anybody here has any experience using either of these and could offer advice before I dive in?
              > >
              > > The cellulose extractor thimbles for the giant Soxhlet are $50-$60 each ($460 for 25). I was wondering if sterile gauze (some on the bottom, under the botanicals, some on top) would work as well?
              > >
              > > The one thing I don't have for the rotary evaporator is a vacuum controller and would like some advice on this. Any advice or experience operating one would be welcome too. So far the best I found was this from the French Culinary Institutes's Tech Blog;
              > >
              > > http://www.cookingissues.com/primers/rotovap/
              > >
              > > My initial aim is to generate essential oils from botanicals which could be used for flavouring and aroma of a whole myriad of things. By all accounts this should be a powerful combination beating water distillation by a long shot (although I could do that too). The possibilities seem endless. Everything from rose petals, gin, herbs etc. In the link above they even mentioned going into the deep forest for earth (to strip the essentials) to impart a woodsy flavour to a dish! Stripping the flavours off Habernero peppers & leaving the hot behind. The nice thing about the rotary evaporator is I can distill at room temperature not damaging flavour & aroma with heat.
              > >
              > > I tried asking about the Soxhlet in new distillers and was met with resounding silence so, now that I also have the Rotary Evaporator, I thought I'd try here in the advanced forum.
              > >
              > > Thanks
              > >
              >
            • daryl_bee
              Hi The rotation of the flask exposes more of the solvent promoting easier evaporation and lessening the need for more heat. While the rotary evaporator does
              Message 6 of 20 , May 10, 2012
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                Hi

                The rotation of the flask exposes more of the "solvent" promoting easier evaporation and lessening the need for more heat. While the rotary evaporator does all this (and I already have that part) I suppose you could simulate it with an aggressive magnetic stirring set-up under the flask and avoid the rotating vacuum tight seal/joint.

                Cheers

                --- In Distillers@yahoogroups.com, "abbababbaccc" <abbababbaccc@...> wrote:
                >
                > That article is very interesting, I just wonder why do they need the rotating boiler? I mean the rolling action of the boil should be plenty enough. Without the rotation that would be really simple system to set up, well except for the vacuum and bain marie but you get my point.
                >
                > I'd suggest you try the system without the vacuum and rotation first. Then if you are not satisfied with the results add vacuum.
                >
                > Slainte, Riku
                >
                > --- In Distillers@yahoogroups.com, "daryl_bee" <darylbender@> wrote:
                > >
                > > Hi
                > >
                > > I thought I'd take distilling to a whole new level and picked up a giant Soxhlet extractor and a Buchi Rotary evaporator (still need to get some glassware for it). I was wondering if anybody here has any experience using either of these and could offer advice before I dive in?
                > >
                > > The cellulose extractor thimbles for the giant Soxhlet are $50-$60 each ($460 for 25). I was wondering if sterile gauze (some on the bottom, under the botanicals, some on top) would work as well?
                > >
                > > The one thing I don't have for the rotary evaporator is a vacuum controller and would like some advice on this. Any advice or experience operating one would be welcome too. So far the best I found was this from the French Culinary Institutes's Tech Blog;
                > >
                > > http://www.cookingissues.com/primers/rotovap/
                > >
                > > My initial aim is to generate essential oils from botanicals which could be used for flavouring and aroma of a whole myriad of things. By all accounts this should be a powerful combination beating water distillation by a long shot (although I could do that too). The possibilities seem endless. Everything from rose petals, gin, herbs etc. In the link above they even mentioned going into the deep forest for earth (to strip the essentials) to impart a woodsy flavour to a dish! Stripping the flavours off Habernero peppers & leaving the hot behind. The nice thing about the rotary evaporator is I can distill at room temperature not damaging flavour & aroma with heat.
                > >
                > > I tried asking about the Soxhlet in new distillers and was met with resounding silence so, now that I also have the Rotary Evaporator, I thought I'd try here in the advanced forum.
                > >
                > > Thanks
                > >
                >
              • daryl_bee
                Hi Benedictine (one of my favourite drinks) was just an example. I have a recipe (and it is a daunting list of herbs & oils) but I should now have the
                Message 7 of 20 , May 10, 2012
                • 0 Attachment
                  Hi

                  Benedictine (one of my favourite drinks) was just an example. I have a recipe (and it is a daunting list of herbs & oils) but I should now have the capability to generate all those extracts and in fairly large quantities. In essence, no pun intended, I'll be going back to alchemy which is the root of distillation. Picture dusty shelves full of bottles of tincture, essences, oils & extracts. :-D As for vanilla I'm thinking all I might need to do is slice and dice them up, throw them in the soxhlet receiver, run a few cycles with alcohol and I should have a super concentrate 3 liter tincture. If I wanted to I could put that tincture in the rotary evaporator and remove/recover the alcohol although in this case I'm not sure it would be required.

                  This morning I took the plunge and placed the order for the rest of the rotary evaporator glass-work, clamps, stopcock, a thimble etc and 3 rolls of silicone tubing. That's everything except the vacuum set-up (I have the pump) & the pointy hat and robe :-D. I only got the cellulose thimble as an example. I like the stainless screen idea offered here before. I was looking and you can get stainless screen very very fine, .002" wire with .002" openings, like a woven cloth. Just have to figure out a way *I* in my shop can make it into a thimble.

                  Cheers

                  --- In Distillers@yahoogroups.com, "waljaco" <waljaco@...> wrote:
                  >
                  > Vanilla extracts are normally just alcohol infusions. Most elite cooks just scrape the insides of the pod.
                  > How do you intend to make Benedictine - a secret recipe of apparently 27 herbs?
                  > wal
                  >
                  > --- In Distillers@yahoogroups.com, "daryl_bee" <darylbender@> wrote:
                  > >
                  > > Hi
                  > >
                  > > I was initially a little worried about scratching the glass with a metal mesh but on thinking about it I could probably use silcone "O" rings as bumpers for when putting it into the receiver. My "solvent" flask is 3 liters and the receiver (for the botanicals) is 1.5 liter and 3.75" inside dia! Like I said this thing is big ~ 4ft tall without the heating mantle! Unfortunately I'm still waiting for a heating mantle power cord, some silicone tubing for cooling lines and the arrival of my 26 gal compound still to finalize the "solvent".
                  > >
                  > > I'm thinking that a single soxhlet cycle on something like berries would be like 2 week soak in a bottle of alcohol where as something like wood chips would take several cycles. Does this sound right?
                  > >
                  > > My rotary evaporator will have 2 liter solvent & recovery flasks which I think should harmonize well with the soxhlet. I'm only using it to generate the essentials/flavours so 2 liters should be lots
                  > >
                  > > How do you control the vacuum? I have heard some people use needle valves and some use a controller ($$). How do you gauge the vacuum with a needle valve? The vacuum gauges I've seen are 0 to -30"hg and not what I would think are accurate for controlling vacuum in the millibar range (my Welch vacuum pump should go down to .02 torr (0.0003867355psi) so somewhere between there and 50 torr is where all the action is (atmosphere is 760 torr).
                  > >
                  > > Maybe I'm crazy for undertaking this but the idea of things like fresh vanilla (vs bought extract) or making my own Benedictine from scratch seem irresistible to me.
                  > >
                  > > Thanks!
                  > >
                  > >
                  > >
                  > > --- In Distillers@yahoogroups.com, Bryan Bornais <bbornais@> wrote:
                  > > >
                  > > > Soxhlet extration is good for extracting very insoluble materials. I suppose you could use it to extract botanicals into a super concentrated tincture. The reflux would be pretty harsh on the plant matter, so long run times would probably not be recommended. I would think of shaping a piece of SS mesh into something that fits into it, so it is food grade, and re-usable.
                  > > >  
                  > > > The rotovap is designed for removing solvent and keeping the organic compounds left behind. The solvent (pot) side is heated with a water bath, and vacuum is applied to cause evaporation below the bp of many solvents. The biggest issue I have had with those is 'bumping', where the solvent jumps over to your recovery flask, and you have to start the whole distillation over, after cleaning the condenser and recovery flask. My advice would be to watch your vacuum, and purge as needed, or just scrap the vacuum all together, and run your boiler hotter. The volume is low on these devices, so I am not sure how useful they will be in the long run.
                  > > >
                  > > > Cheers
                  > > >
                  > > >
                  > > >
                  > > > ________________________________
                  > > > From: daryl_bee <darylbender@>
                  > > > To: Distillers@yahoogroups.com
                  > > > Sent: Saturday, May 5, 2012 10:54:16 AM
                  > > > Subject: [Distillers] Soxhlet Extractors & Rotary Evaporators
                  > > >
                  > > >
                  > > >  
                  > > > Hi
                  > > >
                  > > > I thought I'd take distilling to a whole new level and picked up a giant Soxhlet extractor and a Buchi Rotary evaporator (still need to get some glassware for it). I was wondering if anybody here has any experience using either of these and could offer advice before I dive in?
                  > > >
                  > > > The cellulose extractor thimbles for the giant Soxhlet are $50-$60 each ($460 for 25). I was wondering if sterile gauze (some on the bottom, under the botanicals, some on top) would work as well?
                  > > >
                  > > > The one thing I don't have for the rotary evaporator is a vacuum controller and would like some advice on this. Any advice or experience operating one would be welcome too. So far the best I found was this from the French Culinary Institutes's Tech Blog;
                  > > >
                  > > > http://www.cookingissues.com/primers/rotovap/
                  > > >
                  > > > My initial aim is to generate essential oils from botanicals which could be used for flavouring and aroma of a whole myriad of things. By all accounts this should be a powerful combination beating water distillation by a long shot (although I could do that too). The possibilities seem endless. Everything from rose petals, gin, herbs etc. In the link above they even mentioned going into the deep forest for earth (to strip the essentials) to impart a woodsy flavour to a dish! Stripping the flavours off Habernero peppers & leaving the hot behind. The nice thing about the rotary evaporator is I can distill at room temperature not damaging flavour & aroma with heat.
                  > > >
                  > > > I tried asking about the Soxhlet in new distillers and was met with resounding silence so, now that I also have the Rotary Evaporator, I thought I'd try here in the advanced forum.
                  > > >
                  > > > Thanks
                  > > >
                  > >
                  >
                • waljaco
                  I have my doubts about the story around the authentic Benedictine let alone numerous clone recipes which are all discredited by the company. The liqueur is
                  Message 8 of 20 , May 11, 2012
                  • 0 Attachment
                    I have my doubts about the story around the authentic Benedictine let alone numerous clone recipes which are all discredited by the company. The liqueur is apparently based on infusion rather than distillation. Distillation will give you a different character and you will need to rely on caramel to give the appropriate coloring.
                    Commercially a "Dictine" essence is available so you might be on the same track.
                    wal

                    --- In Distillers@yahoogroups.com, "daryl_bee" <darylbender@...> wrote:
                    >
                    > Hi
                    >
                    > Benedictine (one of my favourite drinks) was just an example. I have a recipe (and it is a daunting list of herbs & oils) but I should now have the capability to generate all those extracts and in fairly large quantities. In essence, no pun intended, I'll be going back to alchemy which is the root of distillation. Picture dusty shelves full of bottles of tincture, essences, oils & extracts. :-D As for vanilla I'm thinking all I might need to do is slice and dice them up, throw them in the soxhlet receiver, run a few cycles with alcohol and I should have a super concentrate 3 liter tincture. If I wanted to I could put that tincture in the rotary evaporator and remove/recover the alcohol although in this case I'm not sure it would be required.
                    >
                    > This morning I took the plunge and placed the order for the rest of the rotary evaporator glass-work, clamps, stopcock, a thimble etc and 3 rolls of silicone tubing. That's everything except the vacuum set-up (I have the pump) & the pointy hat and robe :-D. I only got the cellulose thimble as an example. I like the stainless screen idea offered here before. I was looking and you can get stainless screen very very fine, .002" wire with .002" openings, like a woven cloth. Just have to figure out a way *I* in my shop can make it into a thimble.
                    >
                    > Cheers
                    >
                    > --- In Distillers@yahoogroups.com, "waljaco" <waljaco@> wrote:
                    > >
                    > > Vanilla extracts are normally just alcohol infusions. Most elite cooks just scrape the insides of the pod.
                    > > How do you intend to make Benedictine - a secret recipe of apparently 27 herbs?
                    > > wal
                    > >
                    > > --- In Distillers@yahoogroups.com, "daryl_bee" <darylbender@> wrote:
                    > > >
                    > > > Hi
                    > > >
                    > > > I was initially a little worried about scratching the glass with a metal mesh but on thinking about it I could probably use silcone "O" rings as bumpers for when putting it into the receiver. My "solvent" flask is 3 liters and the receiver (for the botanicals) is 1.5 liter and 3.75" inside dia! Like I said this thing is big ~ 4ft tall without the heating mantle! Unfortunately I'm still waiting for a heating mantle power cord, some silicone tubing for cooling lines and the arrival of my 26 gal compound still to finalize the "solvent".
                    > > >
                    > > > I'm thinking that a single soxhlet cycle on something like berries would be like 2 week soak in a bottle of alcohol where as something like wood chips would take several cycles. Does this sound right?
                    > > >
                    > > > My rotary evaporator will have 2 liter solvent & recovery flasks which I think should harmonize well with the soxhlet. I'm only using it to generate the essentials/flavours so 2 liters should be lots
                    > > >
                    > > > How do you control the vacuum? I have heard some people use needle valves and some use a controller ($$). How do you gauge the vacuum with a needle valve? The vacuum gauges I've seen are 0 to -30"hg and not what I would think are accurate for controlling vacuum in the millibar range (my Welch vacuum pump should go down to .02 torr (0.0003867355psi) so somewhere between there and 50 torr is where all the action is (atmosphere is 760 torr).
                    > > >
                    > > > Maybe I'm crazy for undertaking this but the idea of things like fresh vanilla (vs bought extract) or making my own Benedictine from scratch seem irresistible to me.
                    > > >
                    > > > Thanks!
                    > > >
                    > > >
                    > > >
                    > > > --- In Distillers@yahoogroups.com, Bryan Bornais <bbornais@> wrote:
                    > > > >
                    > > > > Soxhlet extration is good for extracting very insoluble materials. I suppose you could use it to extract botanicals into a super concentrated tincture. The reflux would be pretty harsh on the plant matter, so long run times would probably not be recommended. I would think of shaping a piece of SS mesh into something that fits into it, so it is food grade, and re-usable.
                    > > > >  
                    > > > > The rotovap is designed for removing solvent and keeping the organic compounds left behind. The solvent (pot) side is heated with a water bath, and vacuum is applied to cause evaporation below the bp of many solvents. The biggest issue I have had with those is 'bumping', where the solvent jumps over to your recovery flask, and you have to start the whole distillation over, after cleaning the condenser and recovery flask. My advice would be to watch your vacuum, and purge as needed, or just scrap the vacuum all together, and run your boiler hotter. The volume is low on these devices, so I am not sure how useful they will be in the long run.
                    > > > >
                    > > > > Cheers
                    > > > >
                    > > > >
                    > > > >
                    > > > > ________________________________
                    > > > > From: daryl_bee <darylbender@>
                    > > > > To: Distillers@yahoogroups.com
                    > > > > Sent: Saturday, May 5, 2012 10:54:16 AM
                    > > > > Subject: [Distillers] Soxhlet Extractors & Rotary Evaporators
                    > > > >
                    > > > >
                    > > > >  
                    > > > > Hi
                    > > > >
                    > > > > I thought I'd take distilling to a whole new level and picked up a giant Soxhlet extractor and a Buchi Rotary evaporator (still need to get some glassware for it). I was wondering if anybody here has any experience using either of these and could offer advice before I dive in?
                    > > > >
                    > > > > The cellulose extractor thimbles for the giant Soxhlet are $50-$60 each ($460 for 25). I was wondering if sterile gauze (some on the bottom, under the botanicals, some on top) would work as well?
                    > > > >
                    > > > > The one thing I don't have for the rotary evaporator is a vacuum controller and would like some advice on this. Any advice or experience operating one would be welcome too. So far the best I found was this from the French Culinary Institutes's Tech Blog;
                    > > > >
                    > > > > http://www.cookingissues.com/primers/rotovap/
                    > > > >
                    > > > > My initial aim is to generate essential oils from botanicals which could be used for flavouring and aroma of a whole myriad of things. By all accounts this should be a powerful combination beating water distillation by a long shot (although I could do that too). The possibilities seem endless. Everything from rose petals, gin, herbs etc. In the link above they even mentioned going into the deep forest for earth (to strip the essentials) to impart a woodsy flavour to a dish! Stripping the flavours off Habernero peppers & leaving the hot behind. The nice thing about the rotary evaporator is I can distill at room temperature not damaging flavour & aroma with heat.
                    > > > >
                    > > > > I tried asking about the Soxhlet in new distillers and was met with resounding silence so, now that I also have the Rotary Evaporator, I thought I'd try here in the advanced forum.
                    > > > >
                    > > > > Thanks
                    > > > >
                    > > >
                    > >
                    >
                  • daryl_bee
                    Hmmmmm.... am I in the right group (Distillers · For Advanced Beverage Ethanol Distillers)? You want me to buy and dump? (maybe I m misreading you) I want to
                    Message 9 of 20 , May 11, 2012
                    • 0 Attachment
                      Hmmmmm.... am I in the right group (Distillers · For Advanced Beverage Ethanol Distillers)? You want me to buy and dump? (maybe I'm misreading you) I want to explore and discover new things. To boldly go where few home distillers have gone before! :-) I'm sure I'll meet a few Romulans along the way but there's just so much tremendous potential and, I think, fun.

                      Again Benedictine was just an example (my plans are much broader) and the recipe I have is sort of a double infusion. One to get the concentrate and the second to use that to make the drink prior to aging. The thing is you have to start with the raw ingredients and that is where the soxhlet/evaporator come in. I have bought Ragu spaghetti sauce and I've made my own from scratch and there's no comparison!

                      At first I thought these things were esoteric too but as I looked into it they are used in labs all over the world by people/companies who make this their bread and butter. The food industry, perfume industry, cosmetic industry, pharmaceutical & research companies etc etc etc. That's when I started rubbing my chin about the possibilities. Who knows, maybe I'll meet "the Borg" and the whole thing will be a fiasco but I have to try.

                      What I really need at the moment is somebody "down in engineering" to help with controlling vacuums cheap and effectively but I'm getting worried I'm out in the delta quadrant and I've lost contact with the federation. ;-D

                      Cheers
                      (or perhaps, live long & prosper)
                      nothing above should be taken too seriously

                      --- In Distillers@yahoogroups.com, "waljaco" <waljaco@...> wrote:
                      >
                      > I have my doubts about the story around the authentic Benedictine let alone numerous clone recipes which are all discredited by the company. The liqueur is apparently based on infusion rather than distillation. Distillation will give you a different character and you will need to rely on caramel to give the appropriate coloring.
                      > Commercially a "Dictine" essence is available so you might be on the same track.
                      > wal
                      >
                      > --- In Distillers@yahoogroups.com, "daryl_bee" <darylbender@> wrote:
                      > >
                      > > Hi
                      > >
                      > > Benedictine (one of my favourite drinks) was just an example. I have a recipe (and it is a daunting list of herbs & oils) but I should now have the capability to generate all those extracts and in fairly large quantities. In essence, no pun intended, I'll be going back to alchemy which is the root of distillation. Picture dusty shelves full of bottles of tincture, essences, oils & extracts. :-D As for vanilla I'm thinking all I might need to do is slice and dice them up, throw them in the soxhlet receiver, run a few cycles with alcohol and I should have a super concentrate 3 liter tincture. If I wanted to I could put that tincture in the rotary evaporator and remove/recover the alcohol although in this case I'm not sure it would be required.
                      > >
                      > > This morning I took the plunge and placed the order for the rest of the rotary evaporator glass-work, clamps, stopcock, a thimble etc and 3 rolls of silicone tubing. That's everything except the vacuum set-up (I have the pump) & the pointy hat and robe :-D. I only got the cellulose thimble as an example. I like the stainless screen idea offered here before. I was looking and you can get stainless screen very very fine, .002" wire with .002" openings, like a woven cloth. Just have to figure out a way *I* in my shop can make it into a thimble.
                      > >
                      > > Cheers
                      > >
                      > > --- In Distillers@yahoogroups.com, "waljaco" <waljaco@> wrote:
                      > > >
                      > > > Vanilla extracts are normally just alcohol infusions. Most elite cooks just scrape the insides of the pod.
                      > > > How do you intend to make Benedictine - a secret recipe of apparently 27 herbs?
                      > > > wal
                      > > >
                      > > > --- In Distillers@yahoogroups.com, "daryl_bee" <darylbender@> wrote:
                      > > > >
                      > > > > Hi
                      > > > >
                      > > > > I was initially a little worried about scratching the glass with a metal mesh but on thinking about it I could probably use silcone "O" rings as bumpers for when putting it into the receiver. My "solvent" flask is 3 liters and the receiver (for the botanicals) is 1.5 liter and 3.75" inside dia! Like I said this thing is big ~ 4ft tall without the heating mantle! Unfortunately I'm still waiting for a heating mantle power cord, some silicone tubing for cooling lines and the arrival of my 26 gal compound still to finalize the "solvent".
                      > > > >
                      > > > > I'm thinking that a single soxhlet cycle on something like berries would be like 2 week soak in a bottle of alcohol where as something like wood chips would take several cycles. Does this sound right?
                      > > > >
                      > > > > My rotary evaporator will have 2 liter solvent & recovery flasks which I think should harmonize well with the soxhlet. I'm only using it to generate the essentials/flavours so 2 liters should be lots
                      > > > >
                      > > > > How do you control the vacuum? I have heard some people use needle valves and some use a controller ($$). How do you gauge the vacuum with a needle valve? The vacuum gauges I've seen are 0 to -30"hg and not what I would think are accurate for controlling vacuum in the millibar range (my Welch vacuum pump should go down to .02 torr (0.0003867355psi) so somewhere between there and 50 torr is where all the action is (atmosphere is 760 torr).
                      > > > >
                      > > > > Maybe I'm crazy for undertaking this but the idea of things like fresh vanilla (vs bought extract) or making my own Benedictine from scratch seem irresistible to me.
                      > > > >
                      > > > > Thanks!
                      > > > >
                      > > > >
                      > > > >
                      > > > > --- In Distillers@yahoogroups.com, Bryan Bornais <bbornais@> wrote:
                      > > > > >
                      > > > > > Soxhlet extration is good for extracting very insoluble materials. I suppose you could use it to extract botanicals into a super concentrated tincture. The reflux would be pretty harsh on the plant matter, so long run times would probably not be recommended. I would think of shaping a piece of SS mesh into something that fits into it, so it is food grade, and re-usable.
                      > > > > >  
                      > > > > > The rotovap is designed for removing solvent and keeping the organic compounds left behind. The solvent (pot) side is heated with a water bath, and vacuum is applied to cause evaporation below the bp of many solvents. The biggest issue I have had with those is 'bumping', where the solvent jumps over to your recovery flask, and you have to start the whole distillation over, after cleaning the condenser and recovery flask. My advice would be to watch your vacuum, and purge as needed, or just scrap the vacuum all together, and run your boiler hotter. The volume is low on these devices, so I am not sure how useful they will be in the long run.
                      > > > > >
                      > > > > > Cheers
                      > > > > >
                      > > > > >
                      > > > > >
                      > > > > > ________________________________
                      > > > > > From: daryl_bee <darylbender@>
                      > > > > > To: Distillers@yahoogroups.com
                      > > > > > Sent: Saturday, May 5, 2012 10:54:16 AM
                      > > > > > Subject: [Distillers] Soxhlet Extractors & Rotary Evaporators
                      > > > > >
                      > > > > >
                      > > > > >  
                      > > > > > Hi
                      > > > > >
                      > > > > > I thought I'd take distilling to a whole new level and picked up a giant Soxhlet extractor and a Buchi Rotary evaporator (still need to get some glassware for it). I was wondering if anybody here has any experience using either of these and could offer advice before I dive in?
                      > > > > >
                      > > > > > The cellulose extractor thimbles for the giant Soxhlet are $50-$60 each ($460 for 25). I was wondering if sterile gauze (some on the bottom, under the botanicals, some on top) would work as well?
                      > > > > >
                      > > > > > The one thing I don't have for the rotary evaporator is a vacuum controller and would like some advice on this. Any advice or experience operating one would be welcome too. So far the best I found was this from the French Culinary Institutes's Tech Blog;
                      > > > > >
                      > > > > > http://www.cookingissues.com/primers/rotovap/
                      > > > > >
                      > > > > > My initial aim is to generate essential oils from botanicals which could be used for flavouring and aroma of a whole myriad of things. By all accounts this should be a powerful combination beating water distillation by a long shot (although I could do that too). The possibilities seem endless. Everything from rose petals, gin, herbs etc. In the link above they even mentioned going into the deep forest for earth (to strip the essentials) to impart a woodsy flavour to a dish! Stripping the flavours off Habernero peppers & leaving the hot behind. The nice thing about the rotary evaporator is I can distill at room temperature not damaging flavour & aroma with heat.
                      > > > > >
                      > > > > > I tried asking about the Soxhlet in new distillers and was met with resounding silence so, now that I also have the Rotary Evaporator, I thought I'd try here in the advanced forum.
                      > > > > >
                      > > > > > Thanks
                      > > > > >
                      > > > >
                      > > >
                      > >
                      >
                    • abbababbaccc
                      Well, you seem to be drinking good stuff. What is it, Romulan ale? Anyway, my suggestion would be to use bain marie and use the cooling water to create enough
                      Message 10 of 20 , May 11, 2012
                      • 0 Attachment
                        Well, you seem to be drinking good stuff. What is it, Romulan ale?

                        Anyway, my suggestion would be to use bain marie and use the cooling water to create enough vacuum without the rolling boiler stuff. That would have no moving parts and you could then adjust the vacuum (i.e. water flow) and heating to fit your running parameters that you want for each batch

                        Slainte, Riku

                        --- In Distillers@yahoogroups.com, "daryl_bee" <darylbender@...> wrote:
                        >
                        > Hmmmmm.... am I in the right group (Distillers · For Advanced Beverage Ethanol Distillers)? You want me to buy and dump? (maybe I'm misreading you) I want to explore and discover new things. To boldly go where few home distillers have gone before! :-) I'm sure I'll meet a few Romulans along the way but there's just so much tremendous potential and, I think, fun.
                        >
                        > Again Benedictine was just an example (my plans are much broader) and the recipe I have is sort of a double infusion. One to get the concentrate and the second to use that to make the drink prior to aging. The thing is you have to start with the raw ingredients and that is where the soxhlet/evaporator come in. I have bought Ragu spaghetti sauce and I've made my own from scratch and there's no comparison!
                        >
                        > At first I thought these things were esoteric too but as I looked into it they are used in labs all over the world by people/companies who make this their bread and butter. The food industry, perfume industry, cosmetic industry, pharmaceutical & research companies etc etc etc. That's when I started rubbing my chin about the possibilities. Who knows, maybe I'll meet "the Borg" and the whole thing will be a fiasco but I have to try.
                        >
                        > What I really need at the moment is somebody "down in engineering" to help with controlling vacuums cheap and effectively but I'm getting worried I'm out in the delta quadrant and I've lost contact with the federation. ;-D
                        >
                        > Cheers
                        > (or perhaps, live long & prosper)
                        > nothing above should be taken too seriously
                        >
                        > --- In Distillers@yahoogroups.com, "waljaco" <waljaco@> wrote:
                        > >
                        > > I have my doubts about the story around the authentic Benedictine let alone numerous clone recipes which are all discredited by the company. The liqueur is apparently based on infusion rather than distillation. Distillation will give you a different character and you will need to rely on caramel to give the appropriate coloring.
                        > > Commercially a "Dictine" essence is available so you might be on the same track.
                        > > wal
                        > >
                        > > --- In Distillers@yahoogroups.com, "daryl_bee" <darylbender@> wrote:
                        > > >
                        > > > Hi
                        > > >
                        > > > Benedictine (one of my favourite drinks) was just an example. I have a recipe (and it is a daunting list of herbs & oils) but I should now have the capability to generate all those extracts and in fairly large quantities. In essence, no pun intended, I'll be going back to alchemy which is the root of distillation. Picture dusty shelves full of bottles of tincture, essences, oils & extracts. :-D As for vanilla I'm thinking all I might need to do is slice and dice them up, throw them in the soxhlet receiver, run a few cycles with alcohol and I should have a super concentrate 3 liter tincture. If I wanted to I could put that tincture in the rotary evaporator and remove/recover the alcohol although in this case I'm not sure it would be required.
                        > > >
                        > > > This morning I took the plunge and placed the order for the rest of the rotary evaporator glass-work, clamps, stopcock, a thimble etc and 3 rolls of silicone tubing. That's everything except the vacuum set-up (I have the pump) & the pointy hat and robe :-D. I only got the cellulose thimble as an example. I like the stainless screen idea offered here before. I was looking and you can get stainless screen very very fine, .002" wire with .002" openings, like a woven cloth. Just have to figure out a way *I* in my shop can make it into a thimble.
                        > > >
                        > > > Cheers
                        > > >
                        > > > --- In Distillers@yahoogroups.com, "waljaco" <waljaco@> wrote:
                        > > > >
                        > > > > Vanilla extracts are normally just alcohol infusions. Most elite cooks just scrape the insides of the pod.
                        > > > > How do you intend to make Benedictine - a secret recipe of apparently 27 herbs?
                        > > > > wal
                        > > > >
                        > > > > --- In Distillers@yahoogroups.com, "daryl_bee" <darylbender@> wrote:
                        > > > > >
                        > > > > > Hi
                        > > > > >
                        > > > > > I was initially a little worried about scratching the glass with a metal mesh but on thinking about it I could probably use silcone "O" rings as bumpers for when putting it into the receiver. My "solvent" flask is 3 liters and the receiver (for the botanicals) is 1.5 liter and 3.75" inside dia! Like I said this thing is big ~ 4ft tall without the heating mantle! Unfortunately I'm still waiting for a heating mantle power cord, some silicone tubing for cooling lines and the arrival of my 26 gal compound still to finalize the "solvent".
                        > > > > >
                        > > > > > I'm thinking that a single soxhlet cycle on something like berries would be like 2 week soak in a bottle of alcohol where as something like wood chips would take several cycles. Does this sound right?
                        > > > > >
                        > > > > > My rotary evaporator will have 2 liter solvent & recovery flasks which I think should harmonize well with the soxhlet. I'm only using it to generate the essentials/flavours so 2 liters should be lots
                        > > > > >
                        > > > > > How do you control the vacuum? I have heard some people use needle valves and some use a controller ($$). How do you gauge the vacuum with a needle valve? The vacuum gauges I've seen are 0 to -30"hg and not what I would think are accurate for controlling vacuum in the millibar range (my Welch vacuum pump should go down to .02 torr (0.0003867355psi) so somewhere between there and 50 torr is where all the action is (atmosphere is 760 torr).
                        > > > > >
                        > > > > > Maybe I'm crazy for undertaking this but the idea of things like fresh vanilla (vs bought extract) or making my own Benedictine from scratch seem irresistible to me.
                        > > > > >
                        > > > > > Thanks!
                        > > > > >
                        > > > > >
                        > > > > >
                        > > > > > --- In Distillers@yahoogroups.com, Bryan Bornais <bbornais@> wrote:
                        > > > > > >
                        > > > > > > Soxhlet extration is good for extracting very insoluble materials. I suppose you could use it to extract botanicals into a super concentrated tincture. The reflux would be pretty harsh on the plant matter, so long run times would probably not be recommended. I would think of shaping a piece of SS mesh into something that fits into it, so it is food grade, and re-usable.
                        > > > > > >  
                        > > > > > > The rotovap is designed for removing solvent and keeping the organic compounds left behind. The solvent (pot) side is heated with a water bath, and vacuum is applied to cause evaporation below the bp of many solvents. The biggest issue I have had with those is 'bumping', where the solvent jumps over to your recovery flask, and you have to start the whole distillation over, after cleaning the condenser and recovery flask. My advice would be to watch your vacuum, and purge as needed, or just scrap the vacuum all together, and run your boiler hotter. The volume is low on these devices, so I am not sure how useful they will be in the long run.
                        > > > > > >
                        > > > > > > Cheers
                        > > > > > >
                        > > > > > >
                        > > > > > >
                        > > > > > > ________________________________
                        > > > > > > From: daryl_bee <darylbender@>
                        > > > > > > To: Distillers@yahoogroups.com
                        > > > > > > Sent: Saturday, May 5, 2012 10:54:16 AM
                        > > > > > > Subject: [Distillers] Soxhlet Extractors & Rotary Evaporators
                        > > > > > >
                        > > > > > >
                        > > > > > >  
                        > > > > > > Hi
                        > > > > > >
                        > > > > > > I thought I'd take distilling to a whole new level and picked up a giant Soxhlet extractor and a Buchi Rotary evaporator (still need to get some glassware for it). I was wondering if anybody here has any experience using either of these and could offer advice before I dive in?
                        > > > > > >
                        > > > > > > The cellulose extractor thimbles for the giant Soxhlet are $50-$60 each ($460 for 25). I was wondering if sterile gauze (some on the bottom, under the botanicals, some on top) would work as well?
                        > > > > > >
                        > > > > > > The one thing I don't have for the rotary evaporator is a vacuum controller and would like some advice on this. Any advice or experience operating one would be welcome too. So far the best I found was this from the French Culinary Institutes's Tech Blog;
                        > > > > > >
                        > > > > > > http://www.cookingissues.com/primers/rotovap/
                        > > > > > >
                        > > > > > > My initial aim is to generate essential oils from botanicals which could be used for flavouring and aroma of a whole myriad of things. By all accounts this should be a powerful combination beating water distillation by a long shot (although I could do that too). The possibilities seem endless. Everything from rose petals, gin, herbs etc. In the link above they even mentioned going into the deep forest for earth (to strip the essentials) to impart a woodsy flavour to a dish! Stripping the flavours off Habernero peppers & leaving the hot behind. The nice thing about the rotary evaporator is I can distill at room temperature not damaging flavour & aroma with heat.
                        > > > > > >
                        > > > > > > I tried asking about the Soxhlet in new distillers and was met with resounding silence so, now that I also have the Rotary Evaporator, I thought I'd try here in the advanced forum.
                        > > > > > >
                        > > > > > > Thanks
                        > > > > > >
                        > > > > >
                        > > > >
                        > > >
                        > >
                        >
                      • geoff burrows
                        Hi, I think what Daryl bee, is inferring is the old well established proven steam engineering principles of cooling steam which has enough power to lift vast
                        Message 11 of 20 , May 11, 2012
                        • 0 Attachment

                           

                          Hi,

                          I think what Daryl bee, is inferring is the old well established proven steam engineering principles of cooling steam which has enough power to lift vast steel pistons and I mean big pistons with a 2 foot diameter piston head.  This is only from memory so please bear with me The old steam engineers would inject pressurized steam into the cylinder head when the piston was dropping to bottom dead centre then they would condense the steam with a fine spray of  cold water creating a vacum.  This created a very powerful vacuum in the bore which dragged the piston back up the bore moving a big overhead oak rocking  beam in the process. These really old stem machines were used to pump water out of the mines and to pump sewage in London.  I’ve probably got it all arse about tit, so research it it’s worth looking into.  But it was the sudden cooling of the steam that created the colossal vacuum. 

                               Not satisfied with using it once they would use the exiting steam and inject it into a smaller steam engine and usually a third time as well.  Read up on the principle of extracting power from steam with steam engines and they will explain it better.

                          Geoff       

                        • daryl_bee
                          Just in from a night out chasing green women & I read your post 5 minutes ago - I m still chuckling :-D Here s my issue. I have a rotary evaporator and a Welch
                          Message 12 of 20 , May 12, 2012
                          • 0 Attachment
                            Just in from a night out chasing green women & I read your post 5 minutes ago - I'm still chuckling :-D

                            Here's my issue. I have a rotary evaporator and a Welch vacuum pump. If I don't use the pump it will essentially be regular (hot) distillation. i.e. why use the rotary evaporator at all. If I turn my pump on and let it reach *full* vacuum capability I could set up in my deep freezer and boil so hard it will overpower the condenser. I want to finely control it somewhere in between.

                            On a regular still you tweak the heat input to control the boil, taking the fluid temperature up to the boiling point. Here you want to tweak the vacuum input to control the boil, taking the boiling point down to the fluid temperature. In fact with this I can control both. I'll be cooling with tap water so some heat will be added in the bain marie. I'll note that they do make cold feet condensers for use with liquid nitrogen for running a full hard vacuum at low temperature although that's way beyond what I want to do. I just want to boil at 30-40C. In essence I need to put some "black box' between the pump and the evaporator for vacuum control.

                            I have no experience playing with/controlling vacuums. Lab controllers are expensive. Maybe there's no way around it. I've heard that simple needle valves are sometimes used although I don't know how accurate or steady they are. An idea just sprang to mind that maybe I should go off and look into set-ups for plastic bag vacuum clamps used in woodworking.

                            Aye, it just might work... :-)


                            --- In Distillers@yahoogroups.com, "abbababbaccc" <abbababbaccc@...> wrote:
                            >
                            > Well, you seem to be drinking good stuff. What is it, Romulan ale?
                            >
                            > Anyway, my suggestion would be to use bain marie and use the cooling water to create enough vacuum without the rolling boiler stuff. That would have no moving parts and you could then adjust the vacuum (i.e. water flow) and heating to fit your running parameters that you want for each batch
                            >
                            > Slainte, Riku
                          • daryl_bee
                            I think I ve just found it!!! There s an absolutely wonderful site which explains a vacuum system very well;
                            Message 13 of 20 , May 12, 2012
                            • 0 Attachment
                              I think I've just found it!!! There's an absolutely wonderful site which explains a vacuum system very well;

                              http://www.joewoodworker.com/veneering/EVS/concept.htm There's even a PDF download
                              http://www.joewoodworker.com/docs/ProjectEVS.pdf

                              The rig is for vacuum clamping. It's very similar to an air compressor set-up but with negative pressure. In my application I'll need a way better high resolution controller (switches the pump on and off between the two vacuum set points similar to a heat controller) but that's basically the set-up right there. Now I understand what all is needed and what each part does. Since my pump is much bigger (doesn't have to be) I'll likely need larger components too (my vacuum port is 1.5" pipe thread because the pump is over 10CFM). I'm even thinking I can get large cheap reservoir air tanks locally. Larger tanks should allow me to set the upper and lower bounds on the vacuum much closer without start/stopping the pump all the time. That should also allow for smoother operation.

                              I'm inexpressibly grateful to your post for in replying to it the seed of an idea came. I hope others here, or in future, might find the above site as useful as I have.

                              Oh happy day!!

                              Cheers

                              --- In Distillers@yahoogroups.com, "daryl_bee" <darylbender@...> wrote:
                              >
                              > Just in from a night out chasing green women & I read your post 5 minutes ago - I'm still chuckling :-D
                              >
                              > Here's my issue. I have a rotary evaporator and a Welch vacuum pump. If I don't use the pump it will essentially be regular (hot) distillation. i.e. why use the rotary evaporator at all. If I turn my pump on and let it reach *full* vacuum capability I could set up in my deep freezer and boil so hard it will overpower the condenser. I want to finely control it somewhere in between.
                              >
                              > On a regular still you tweak the heat input to control the boil, taking the fluid temperature up to the boiling point. Here you want to tweak the vacuum input to control the boil, taking the boiling point down to the fluid temperature. In fact with this I can control both. I'll be cooling with tap water so some heat will be added in the bain marie. I'll note that they do make cold feet condensers for use with liquid nitrogen for running a full hard vacuum at low temperature although that's way beyond what I want to do. I just want to boil at 30-40C. In essence I need to put some "black box' between the pump and the evaporator for vacuum control.
                              >
                              > I have no experience playing with/controlling vacuums. Lab controllers are expensive. Maybe there's no way around it. I've heard that simple needle valves are sometimes used although I don't know how accurate or steady they are. An idea just sprang to mind that maybe I should go off and look into set-ups for plastic bag vacuum clamps used in woodworking.
                              >
                              > Aye, it just might work... :-)
                              >
                              >
                              > --- In Distillers@yahoogroups.com, "abbababbaccc" <abbababbaccc@> wrote:
                              > >
                              > > Well, you seem to be drinking good stuff. What is it, Romulan ale?
                              > >
                              > > Anyway, my suggestion would be to use bain marie and use the cooling water to create enough vacuum without the rolling boiler stuff. That would have no moving parts and you could then adjust the vacuum (i.e. water flow) and heating to fit your running parameters that you want for each batch
                              > >
                              > > Slainte, Riku
                              >
                            • Timothy C Smoth
                              My buddy used a cold finger set up that had food grade antifreeze running throughout it. It was chilled using a setup almost like an ice machine. Sent from
                              Message 14 of 20 , May 14, 2012
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                                My buddy used a cold finger set up that had food grade antifreeze running throughout it. It was chilled using a setup almost like an ice machine.

                                Sent from Tim's iPhone
                              • snoozer219
                                ... Youve pricked my interest there about that process. Id be interested to hear more!
                                Message 15 of 20 , May 15, 2012
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                                  --- In Distillers@yahoogroups.com, Timothy C Smoth <timothyc.smith@...> wrote:
                                  >
                                  > My buddy used a cold finger set up that had food grade antifreeze running throughout it. It was chilled using a setup almost like an ice machine.
                                  >
                                  > Sent from Tim's iPhone
                                  >
                                  Youve pricked my interest there about that process. Id be interested to hear more!
                                • bob@4agoodauction.com
                                  3 Large barrels (99 Francois Freres Tonnellerie, St Romain Cote D Or, France, T, MT, Qualite CTB Certifiee no 1 Fot de Tradition Francaise). A picture can be
                                  Message 16 of 20 , May 15, 2012
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                                    3 Large barrels (99 Francois Freres Tonnellerie, St Romain Cote D’ Or, France, T, MT, Qualite CTB Certifiee no 1 Fot de Tradition Francaise). A picture can be found at http://www.4agoodauction.com/4a/current/mainpage.htm  There is supposed to be one more of these barrels coming in this afternoon.  Does anybody on the list have an idea of the value for a barrel? They look to be lightly charred on the inside. I don’t write very often and mostly lurk BUT this looks like it might be interesting. They look and I am guessing to be about 40 to 50 gallons.

                                     

                                    Bob C

                                     

                                  • White Bear
                                    Friends-   My Uncle use to test the ABV of his stripping run by collecting 5 drops of distillate on a small flat piece of metal such as a canning jar flat. 
                                    Message 17 of 20 , May 15, 2012
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                                      Friends-
                                        My Uncle use to test the ABV of his stripping run by collecting 5 drops of distillate on a small flat piece of metal such as a canning jar flat.  He would set it to flame and after it burned out, tip the flat and count the drops that drip off.
                                        QUESTION:  would this be a reliable test for ABV?  If so, why or why not. 
                                      Thanks
                                      White Bear 
                                    • Bryan Bornais
                                      Best thing to do would be to take a sample (enough to fill an alcoholometer jar). Experiment with number of drops, and test out your observations against the
                                      Message 18 of 20 , May 15, 2012
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                                        Best thing to do would be to take a sample (enough to fill an alcoholometer jar). Experiment with number of drops, and test out your observations against the true reading on your alcoholometer. It may be that it is consistent enough to give you a ball park idea of where you are in the run. Thanks for sharing this idea.
                                         



                                        From: White Bear <sha_man_1@...>
                                        To: Distillers@yahoogroups.com
                                        Sent: Tuesday, May 15, 2012 3:37:26 PM
                                        Subject: [Distillers] Quick Question / ABV Test?

                                         
                                        Friends-
                                          My Uncle use to test the ABV of his stripping run by collecting 5 drops of distillate on a small flat piece of metal such as a canning jar flat.  He would set it to flame and after it burned out, tip the flat and count the drops that drip off.
                                          QUESTION:  would this be a reliable test for ABV?  If so, why or why not. 
                                        Thanks
                                        White Bear 


                                      • Timothy C Smoth
                                        It s been a long time since I saw it. But I think it had some coils running inside of the chiller and a pump to circulate the anti freeze. He was using some
                                        Message 19 of 20 , May 16, 2012
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                                          It's been a long time since I saw it. But I think it had some coils running inside of the chiller and a pump to circulate the anti freeze. He was using some kind of plastic hose to connect everything. I would think stainless tubing would be the way to go if you could work it in.
                                          The food grade antifreeze was purple. But I don't think it was the RV anti freeze. That's non toxic though.
                                          I'll bet you could find a laboratory setup on line. I've never looked.

                                          Sent from Tim's iPhone
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