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Still Operating Proceedures

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  • charles55me@yahoo.com
    Hello, I m new to the group although I have been lurking around reading hundreds of posts for a while. I need help from the members to set up a step by step
    Message 1 of 8 , Oct 28, 2001
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      Hello,

      I'm new to the group although I have been lurking around reading
      hundreds of posts for a while.
      I need help from the members to set up a step by step guide to
      operating a Nixon Stone fractionating still. The pot is 23L, column
      diam. is 50mm, 120cm tall, 2x 180W elements.
      There is plenty of theory on this wonderful site, and Tonys Acklands,
      but I'm not confident yet on how to approach the practical.
      Help needed please!

      Graeme
    • klcampbell
      G day Graeme,I run an S/N unit,that is the tee d version not the straight through column. Firstly do you mean 2x1800w.elements?,if yes you can use both for
      Message 2 of 8 , Oct 28, 2001
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        G'day Graeme,I run an S/N unit,that is the tee'd version not the straight
        through column.
        Firstly do you mean 2x1800w.elements?,if yes you can use both for heat up
        but will need to turn one off for the distillation run. Now what type of
        temperature control do you have?,I run a digital controller with a solid
        state relay which I assembled from some spare components left over from a
        work project.This controller is so good that the output from the condenser
        stops when the temperature in the tower increases by 8/10 of 1oC.

        Make sure that the thermocouple is protruding into the vapour stream the
        same depth as the digital thermometer,this needs to be just where the vapour
        goes into the tee'd section,this gives very good control and also temp.
        reading.Monitor the water flow and discharge temperature from the
        condenser,it should come out at about 22-24oC and the distillate should be
        at around 28oC.Allow the discharge to drip into a funnel,not plastic,and
        then into your collection jars.By following John and Mike's directions plus
        all the info on Tony's site you will be allright but if there is a muck up
        just put it back in the pot and run it again,hasten slowly,Regards,Ken.
        ----- Original Message -----
        From: <charles55me@...>
        To: <new_distillers@yahoogroups.com>
        Sent: Monday, 29 October 2001 13:00
        Subject: [new_distillers] Still Operating Proceedures


        > Hello,
        >
        > I'm new to the group although I have been lurking around reading
        > hundreds of posts for a while.
        > I need help from the members to set up a step by step guide to
        > operating a Nixon Stone fractionating still. The pot is 23L, column
        > diam. is 50mm, 120cm tall, 2x 180W elements.
        > There is plenty of theory on this wonderful site, and Tonys Acklands,
        > but I'm not confident yet on how to approach the practical.
        > Help needed please!
        >
        > Graeme
        >
        >
        >
        > To unsubscribe from this group, send an email to:
        > new_distillers-unsubscribe@onelist.com
        >
        >
        >
        > Your use of Yahoo! Groups is subject to http://docs.yahoo.com/info/terms/
        >
        >
      • charles55me@yahoo.com
        Thanks Ken, The elements are 1380W each. When I was doing initial reading I could not find any feference to controllers, thermostats etc. So I have decided to
        Message 3 of 8 , Oct 29, 2001
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          Thanks Ken,

          The elements are 1380W each. When I was doing initial reading I could
          not find any feference to controllers, thermostats etc. So I have
          decided to adopt Tony Acklands proceedure of dropping out one element.
          Hey its interesting the Brisbanes water temp is 24+c and will go to 27
          c over the next few months. So I will have to adjust to allow for
          these differences on your figures.

          Graeme

          --- In new_distillers@y..., "klcampbell" <klcampbell@o...> wrote:
          > G'day Graeme,I run an S/N unit,that is the tee'd version not the
          straight
          > through column.
          > Firstly do you mean 2x1800w.elements?,if yes you can use both for
          heat up
          > but will need to turn one off for the distillation run. Now what
          type of
          > temperature control do you have?,I run a digital controller with a
          solid
          > state relay which I assembled from some spare components left over
          from a
          > work project.This controller is so good that the output from the
          condenser
          > stops when the temperature in the tower increases by 8/10 of 1oC.
          >
          > Make sure that the thermocouple is protruding into the vapour
          stream the
          > same depth as the digital thermometer,this needs to be just where
          the vapour
          > goes into the tee'd section,this gives very good control and also
          temp.
          > reading.Monitor the water flow and discharge temperature from the
          > condenser,it should come out at about 22-24oC and the distillate
          should be
          > at around 28oC.Allow the discharge to drip into a funnel,not
          plastic,and
          > then into your collection jars.By following John and Mike's
          directions plus
          > all the info on Tony's site you will be allright but if there is a
          muck up
          > just put it back in the pot and run it again,hasten
          slowly,Regards,Ken.
          > ----- Original Message -----
          > From: <charles55me@y...>
          > To: <new_distillers@y...>
          > Sent: Monday, 29 October 2001 13:00
          > Subject: [new_distillers] Still Operating Proceedures
          >
          >
          > > Hello,
          > >
          > > I'm new to the group although I have been lurking around reading
          > > hundreds of posts for a while.
          > > I need help from the members to set up a step by step guide to
          > > operating a Nixon Stone fractionating still. The pot is 23L,
          column
          > > diam. is 50mm, 120cm tall, 2x 180W elements.
          > > There is plenty of theory on this wonderful site, and Tonys
          Acklands,
          > > but I'm not confident yet on how to approach the practical.
          > > Help needed please!
          > >
          > > Graeme
          > >
          > >
          > >
          > > To unsubscribe from this group, send an email to:
          > > new_distillers-unsubscribe@onelist.com
          > >
          > >
          > >
          > > Your use of Yahoo! Groups is subject to
          http://docs.yahoo.com/info/terms/
          > >
          > >
        • distiller@mafudesigns.com
          Hi everyone, I too would like to see a kind of step by step guide to running the still - I have nearly finished building a Nixon Stone style still, and have
          Message 4 of 8 , Oct 29, 2001
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            Hi everyone,

            I too would like to see a kind of 'step by step' guide to running the
            still - I have nearly finished building a Nixon Stone style still,
            and have both the corn whiskey (Smiley) and Vodka (Stone) books -
            both have great info, but a step by step guide of what to do, expect
            etc etc would be great to see.

            Also, I am planning on running two 1380 elements for heat up, and
            then only one for the boil. Today it came to me that instead of
            running just one element for the boil, it would be better to run them
            both, but at half the wattage by running them in parallel. Has
            anyone tried this? The circuit would be pretty easy with just a
            switch to change from one circuit to the other. The advantage would
            be the increased heat distribution through the wash, and decreased
            use/wear on the elements. Thoughts anyone?

            Matt
          • Tony & Elle Ackland
            ... Here s how I run mine ..... I run mine with a 1800W element, normally about 20-25L of wash (30L pot), in a column 1.2m x 1.5 diameter Before I use the
            Message 5 of 8 , Oct 30, 2001
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              > I too would like to see a kind of 'step by step' guide to running the
              > still - I have nearly finished building a Nixon Stone .....

              Here's how I run mine .....

              I run mine with a 1800W element, normally about 20-25L of wash (30L pot),
              in a column 1.2m x 1.5" diameter

              Before I use the column, I usually pour 2L of boiling water down through
              it, to help clean it.

              The pot takes about 50 minutes to heat up. I usually put the cooling water
              on about half way through, well before any vapour starts coming up the
              column. The cooling water is about 500 mL/min - using a 3/16" tube for the
              coil makes it pretty hard to push any more through it, but its more than
              enough.

              Close the off-take valve.

              The heat up time is fairly repeatable, but I still monitor its progress by
              seeing how long I can hold my hand against the side of the boiler - a
              fairly good guide as to if its 60/70/80C etc (I callibrated my hand to
              temperature a few years ago at work ...) As the wash develops towards a
              boil you can start to hear a difference in the "boiling noise" too. At
              this stage I normally have to readjust the postion of the lead weight belt
              that sits on the lid, to help seal it better.

              At the full time mark, the temperature in the column rises fairly rapidly -
              going from 15C up to 80C within a couple of minutes. Incase I miss it, I
              make sure that when I put the water on, that I fully closed the needle
              valve.

              With this rise in temperature, i also notice some vapour escaping out the
              top of the condensor. This isn't alcohol, but rather the air that had been
              in the pots headspace & in the column.

              The temperature may initially get up into the 80's, but then start
              dropping. This is because there was no reflux happening to begin with, and
              it needs to get established. In a minute or so, the temperature will start
              to slowly drop back. Depending on how many impurities are in the wash is
              how low it will go. Eg a clean sugar-water wash that fermented well &
              fully may only settle back to 78C, whereas failed grain experiments can
              result in a temperature in the low 70's / late 60's. This is because of
              the presence of methanol, actetone, and other foreshots.

              Leave the column running in total reflux for 15-20 minutes. During this
              time, check that the cooling water is running fast enough (eg the water
              return can be quite warm (OK) but you don't want it scalding hot.

              The idea of this period at total reflux is to help get all the foreshots
              present to congregate up in the top of the column.

              After 15-20 min, slowly open the offtake valve a little. You only want to
              take the foreshots out at 1 drip per second. Collect these in a small jar
              / measuring cylinder etc.

              You only collect them very slowly so that the equilbrium in the column
              never gets too upset. If you were to suddenly open the valve wide at this
              stage, you'd reduce the amount of reflux happening, the precise seperation
              of this fraction wouldn't be so precise, and it would require more spirits
              to be removed so as to get it all.

              This first stuff (the "foreshots") really stinks - the acetate is nail
              polish remover.
              Collect 50 mL and throw it away.

              After the first 50 mL, start capturing the occasional drip, and smelling it
              (eg rub on the back of your hand, or over a spoon etc). When the smell has
              gone, then you're ready to begin collecting the heads. While you still
              smell nail polish remover, you're only collecting BBQ lighter material.

              During this process, keep an eye on the temperature. What you'll notice is
              that at some point the temperature will begin to increase. If you've got a
              really tight seperation happening, it will sit on the 70 or so for ages,
              and then sudddenly jump up to around 78.2C. If you're collecting it a
              little too fast, the temperature might instead slowly creep up to 78.2C
              over time.

              Either way, you'll probably notice the smell stops when you've got to 78.2C
              and been there a couple of minutes.

              You're now onto collecting the "heads". So put your good collection jar in
              place Heads are mostly good ethanol, however they may have a little
              flavour/smell of their own. If you're into doing a really pure gin/vodka,
              then you may want to keep the first litre or so seperate, away from the
              ultra-pure "middle run". I dont bother, as I figure theres no real
              difference between the two. But some guys can smell it, and make a deal of
              keeping them seperate.

              Maybe for the first couple of runs you collect the distillate in 500mL
              lots, and smell/taste test them seperately - judge for yourself.

              Once you're onto collecting the heads, you can open the valve open quite a
              bit more. I'll open mine until the temperature has risen to around 78.4C.
              For me this is a good compromise between time and purity. If I'm after
              some 96% stuff to show off to someone, I'll screw it back down and keep it
              at 78.2C, but usually this is too slow for me. So I open it up until I get
              78.4 ish This usually starts off around 30 mL/minute - eg a healthy
              dribble.

              The aim for the next 3-4 hours is to keep the vapour temperature at this
              78.4C. Check the still every 15-20 minutes (eg each add break on TV), and
              adjust the reflux ratio. What you'll find is that as the amount of alcohol
              in the pot reduces, you'll need slightly more reflux happening to keep the
              same purity. This is just a small nudge to slightly close the valve every
              so often.

              Again - be your own judge. If you're happy with spirits at 90%, and like
              the faster collection speed, thats your call.

              Keep in mind the maths re how much alcohol you're expecting to collect
              ...eg if it was 25L at 18%, then there is 25 x 0.18 = 4.5L of pure (100%)
              alcohol present. We're collecting it say at 94%, so we'd expect say 4.5 /
              0.94 = 4.78 L if perfect. But some will always remain uncaptured. But as
              a guideline, when we've got say 4.5L we know we're towards the end of it.

              This should have been pretty apparent to you by then anyhow - you've now
              probably got the off-take valve closed right down to a slow drip.

              Maybe you've instead got to the point where no matter how much reflux you
              offer, the temperature persists in climbing. That will instead be your
              indication to quit. If this is the case, then you probably don't want to
              collect past about 82C

              So now you make your cut to the "tails" These will still have a fair bit
              of ethanol in them, but also an increasing amount of the other cogeners.
              Collect the tails into their own container. We're not after purity at
              this stage, so you can open the valve quite wide. Don't have it fully
              open, as you still want a little of the reflux action happening, but its
              not critical. Collect the tails up to about 96C. This is probalby about
              another 200-400 mL. The tails can either be added to the next wash, or
              collected up over a few runs & distilled on their own.

              After that, turn off the power, then after a few more minutes, when the
              temperature is dropping fast and is below 60C, kill the cooling water.

              What I've described is for a sugar-water wash for make a neutral vodka. If
              you want to do a flavored run, then you would still do the foreshots bit,
              but when collecting the head & middle run, you'd have slightly less reflux
              happening (eg maybe sit it less than 80C without being too fussy). You'd
              make the cut to tails quite a bit later too - collecting the flavourful
              cogeners up to say 91C This final cut point is based on whether you're
              after a lighter spirit (stop sooner), or a heavier one (wait for say
              92-93C).

              Tip out the spent wash, and clean all the equipment really thoroughly, and
              also dry it well. Rinse the column really well - say 2L of boiling water
              in the top of it, then a good rinsing with the garden hose.

              What can go wrong ? Say at some point you hear the column change sound,
              and it starts to gurgle or splutter. Maybe the lid also decides to start
              leaking heaps more too. This would indicated that the column has got a
              little clogged (eg some foam has boiled up into it and gunged it up). Kill
              the power, take the head off the column, and pour 1-2L of boiling water in
              the top. Add power, and keep going from where you were (maybe put it into
              total reflux for a while to restablish the equilbbrium, then slowly open
              the offtake until you're back to the steady state offtake rate).

              If you need to turn off the power etc & interupt the game for a while (eg
              unexpected visitors drop by who really shouldn't know about it), you can
              easily pick up from where you left off - eg if you've already removed the
              foreshots, then you don't need to remove them a second time (cos they won't
              be there). It keeps it really simple - eg instructions for non-distilling
              spouses if you have to pop out for a while = "turn off the power if
              anything changes" this covers all situations from leaking lids, to tap
              connections blowing off, to visitors etc. The main thing is just to ensure
              that you've always got cooling water when the vapour is above 60C

              Well - thats how I do it. Others may do it quite differently.

              Tony
              http:\\homedistiller.org
            • distiller@mafudesigns.com
              ... Tony, What a great description/list/instructions/post! Thanks so much - Thats *exactly* the kind of thing I wanted to see - now I feel like I can
              Message 6 of 8 , Oct 31, 2001
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                > Here's how I run mine .....

                <snip>

                Tony,

                What a great description/list/instructions/post! Thanks so much -
                Thats *exactly* the kind of thing I wanted to see - now I feel like I
                can approach the first run with a heaps better idea of what to expect
                and do!

                Now if the other bits and pieces for the still would arrive, I could
                finish it off and actually put it all to use....

                Thanks again for all your posts/info/site etc.

                Matt
              • Tony & Elle Ackland
                Matt, ... With a 2 column, theres a good chance that you might be able to run both of them (2760W) still during the boil. Knowing that 1800W works well with
                Message 7 of 8 , Oct 31, 2001
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                  Matt,

                  > Also, I am planning on running two 1380 elements for heat up, and
                  > then only one for the boil.

                  With a 2" column, theres a good chance that you might be able to run both
                  of them (2760W) still during the boil. Knowing that 1800W works well with
                  1.5" columns, and that a 2" column has 1.77 times the cross-sectional area,
                  this would put 3200W still in the happy zone. Worth a crack.

                  Tony
                • charles55me@yahoo.com
                  Thank you very much for your help on operating proceedures, and your time in putting your post on this subject together. Your enthusiasim, time devoted and
                  Message 8 of 8 , Nov 1, 2001
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                    Thank you very much for your help on operating proceedures, and your
                    time in putting your post on this subject together.
                    Your enthusiasim, time devoted and patience displayed with people who
                    need help is awesome.

                    Graeme








                    --- In new_distillers@y..., Tony & Elle Ackland <Tony.Ackland@c...>
                    wrote:
                    > Matt,
                    >
                    > > Also, I am planning on running two 1380 elements for heat up, and
                    > > then only one for the boil.
                    >
                    > With a 2" column, theres a good chance that you might be able to
                    run both
                    > of them (2760W) still during the boil. Knowing that 1800W works
                    well with
                    > 1.5" columns, and that a 2" column has 1.77 times the cross-
                    sectional area,
                    > this would put 3200W still in the happy zone. Worth a crack.
                    >
                    > Tony
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