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Seth_Leigh

A new Madder Lake experiment. EASY grinding.

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I've been thinking for a while about how to make Madder Lake and remove the difficult process of grinding it fine enough for use in varnish. The first batch of madder lake I made was very difficult to grind into a powder that worked well in varnish.

I had an idea I've just tried over the last week or so and I'd like to report how it went.

I thought it would be very helpful if I could avoid grinding it altogether. That is, if I could take the madder lake as it was suspended in liquid while making it and get it in that form in turpentine, then I could mix this into varnish and never dried it at all, nor ground it.

I thought ok you make the lake with water, and water and turpentine don't mix. But water and alcohol mix, and alcohol and turpentine mix.

So I made the madder lake more or less as David Rubio's site shows, washing it with water several times until the water above the settled lake was fairly clear.

I then drained this water above the settled lake and poured the lake into a coffee filter (set into a sieve) and let it drain water until it was just a nice red slime. Without letting it dry at all I scraped the lake into a smaller jar and filled it with denatured alcohol. I washed it in alcohol two more times, so that in my estimation after this the concentration of water must have been below 1% and I thought this lake, now suspended in alcohol, would mix well with turpentine.

Well it didn't. After draining the alcohol the last time and pouring the settled lake onto a coffee filter to further reduce the liquid, I scraped the lake back into the jar and filled the jar with turpentine. The lake did not mix. I shook it violently for multiple minutes and it seemed that there was water or alcohol or something stuck to the individual molecules of madder lake that rendered it incapable of mixing with the turpentine.

Instead it was like fifty zillion individual spheres of non-mixable lake suspended in turpentine. The lake would settle to the bottom and you couldn't see individual balls of it or anything but you could tell it was not mixed in with the turpentine the way it had with the water and alcohol.

OK, so my experiment had failed. I decided to see what would happen when I dried this out. I drained off the turpentine and poured the settled lake into a coffee filter again and let this dry out for a couple of days.

This is where it gets really beautiful. The dried lake was very fragile to the touch, and when I looked at my fingertip where I'd touched it there was finely powdered lake on my finger. The dried pieces of lake were extremely porous, as in on a molecular level! This stuff had not dried into very hard pieces that required grinding as it does when it's made in water and left to dry.

I put all of the dried lake into my mortar and pestle and within about 20 seconds I had reduced all of my dried lake into a very, very fine powder. It still smells of turpentine, and it's not a "dry" powder in the sense that it still tends to sort of stick together, but it's very, very finely divided.

I mixed some into some varnish last night and it mixed extremely easily.

This is fantastic. While my original goal of having a jar of turpentine with fine, undried lake settled at the bottom of it failed, I still now have madder lake which is extremely fine and I didn't have to spend hours grinding it. Now I have to work out how much of this to put into some varnish to get the right color and whatnot.

I'm going to experiment with this some more. This was a very small batch of lake, only a fraction of the recipe Rubio's site recommends. I need to make some more and repeat the experiment and verify that I will always get easily powderable lake.

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Thanks for sharing your work, Seth. I had the same thing happen with my only attempt at madder lake making. I still have mine, mixed with oil, but too coarse to use. I ground it for a couple hours in oil with out success. You've given me some good ideas.

Don

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Bud, I made it the normal way, precipating it on alum, as David Rubio's site shows, all the way up to the point where on Rubio's site he lays it out on a filter to dry, and instead I scraped it off the filter and went to the alcohol stage.

Honestly, the alcohol was there mainly because I thought I could get the alcohol to mix with the turpentine. The alcohol was there mainly to dilute the water so I could get the turpentine mix. Now that I'm not going to get the lake from water into turpentine in the way I originally thought, I do not know if washing in alcohol is strictly necessary.

I'll make some more, and this time I'm going to see if I can go straight from taking the lake from the water off the filter paper back into a jar with turpentine immediately, shake it up vigorously and lay it out on filter paper and get the same effect.

If this works, then I'll be really stoked. Grinding dried, caked madder lake is a real chore.

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I'm afraid I am not familiar with Rubio's method... I assume it is similar to other methods?

Anyway, if I understand you, the texture you describe is what I've obtained when you make the "tea" with alum and precipitated with lye; then wash the heck out of it. I end up with flakes made up of fine powder.

When I make a lake the other way 'round, I end up with a pretty crunchy substance.

The color is different depending on which method is used, so I use both.

Still, I'm having trouble understanding the griding problem. I really don't have much trouble (even with the crunchy stuff). Are you all trying to grind a large amount at a time?

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Jeffery, with Rubio's method you make a solution of potash and water and soak the roots in that for a while with some heat, then strain out the roots and when it's clean you mix in a solution of alum and the precipitate forms. After washing this a number of times and pouring it onto a filter paper or coffee filter and it dries out, it's caked into a very compact form which requires grinding, and it's tough stuff to grind into a fine powder. With my first batch I ground and ground and never did get it into the fine powder I got it into this time around.

By the way I really like the color I get from the potash and alum method. It's a deep ruby red, not pinkish like the madder lake I bought from Kremer.

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Thanks for the info! I'll try it with some pigment I keep stored wet. One way I have found to reduce the grinding problem is to just rub wet pigment onto a violin and sand it with micromesh, let it dry and then sand off the dry pigment and save it---this is very fine. Some also remains in the varnish and lights up after the following coat---call it dry glazing if you like.

I also find if making pigment with propolis it is always very soft , chalky, and easy to grind.

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I thought I'd resurrect this old thread to add a further result.

I went out last week and bought a cheap espresso maker at Walmart, and made some madder lake using the method described by Neal Ertz, which uses nothing but hot water under pressure in the espresso maker to leach out the dyestuff from the roots, then mixes in alum, then precipitates the pigment out using dissolved potash.

Neal mentions this, but I think he understates it:  this stuff is an absolute dream to grind.  The dried lake I made using the Espresso Method practically dissolved into a few drops of mastic varnish.  I literally mulled a largish chunk of this pigment into the mastic varnish using nothing but a pallet knife on a sheet of glass, in just a couple minutes.  It ended up better mixed than any madder lake I've ever made.

In contrast, I spend a good 45 minutes grinding a sample (probably 10 grams) of the large batch of lake I made last week using the typical Rubio-esque method, but which I'd used all that vinegar on.  After all that grinding, it's still got tons and tons of sand-like particles which are far too large to use in a varnish.

I will say that the color I got from the Espresso Method is different from the color I've gotten using the more traditional methods.  This Espresso-made lake is a brighter, ruby-er red.

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Hi Seth- if you want to make madder soluble in varnish, altering a step in what you are doing will make this possible. Your  first step  in this process is to add the ground root to hot water with soap added. Soap is an olefin with the glycerin end( the water soluble end) removed and replaced with a caustic that makes it soluble in water. If the alkaline end is removed from the olefin it is no longer soluble in water, but is now soluble in oils, turp, etc because it an oil. So taking advantage of this you add madder to hot soap solution, the madder is soluble because  it is an alkaline solution. Now when you add your alum it replaces the alkaline end of the fatty acid, the alum forms the lake you have been making,  precipitates out for it is no longer soluble in water, but having a fatty acid attached, it will now be soluble in oil varnish components. I've done this many times with ferric sulphate, (green vitriol) which will give you a nice violin brown oil varnish. A very permanent coloring, the only problem is it keeps getting darker for around 6 months, but still a nice color. I had never tried alum and when I read your post I tried it and I obtained a reddish orange in turp, similar to using lead acetate.

I'm a super senior, gave away all my chemicals  to N. Bennet Street School violin making section and it is better if someone else who can remember what they did 2 minutes ago to pick it up. Also, I color the wood, not the varnish, easy stuff, and it  appears as if it is colored varnish, so I don't use this procedure. The process is really simple, and if you are interested in pursuing it, i'll provide greater detail on starting up. Fred

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FredN,

Thanks for posting this. I am tempted to try some of the things you mentioned.

 

I put too much ferrous sulphate on a violin year ago. Ruined it because it got so dark with a greenish brown color.

 

Still, I like playing with stuff.

 

I wish you would write and write and write.

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Hi Seth- if you want to make madder soluble in varnish, altering a step in what you are doing will make this possible. Your  first step  in this process is to add the ground root to hot water with soap added. Soap is an olefin with the glycerin end( the water soluble end) removed and replaced with a caustic that makes it soluble in water. If the alkaline end is removed from the olefin it is no longer soluble in water, but is now soluble in oils, turp, etc because it an oil. So taking advantage of this you add madder to hot soap solution, the madder is soluble because  it is an alkaline solution. Now when you add your alum it replaces the alkaline end of the fatty acid, the alum forms the lake you have been making,  precipitates out for it is no longer soluble in water, but having a fatty acid attached, it will now be soluble in oil varnish components. I've done this many times with ferric sulphate, (green vitriol) which will give you a nice violin brown oil varnish. A very permanent coloring, the only problem is it keeps getting darker for around 6 months, but still a nice color. I had never tried alum and when I read your post I tried it and I obtained a reddish orange in turp, similar to using lead acetate.

I'm a super senior, gave away all my chemicals  to N. Bennet Street School violin making section and it is better if someone else who can remember what they did 2 minutes ago to pick it up. Also, I color the wood, not the varnish, easy stuff, and it  appears as if it is colored varnish, so I don't use this procedure. The process is really simple, and if you are interested in pursuing it, i'll provide greater detail on starting up. Fred

 

 

Fred, could you explain further, I mean, make it simpler? Could you give us a simple recipe/procedure to repeat this?

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Fred is mentioning making a madder (or other colourant) soap instead of a lake.(in a roundabout way). John Masters has mentioned this many times on here over the years . Ive tried it quite a few times and it is interesting but my varnish was becoming slower to dry. (not sure why).

Heres what it looks like before driving off the water content,its like a paste.

Here what a tiny bit of the madder soap looks like in just linseed oil on bare wood.(not the best photo)The intensity and colour shades can be altered depending on strength of madder /alizarin extract and what metal you use.But its perfectly transparent when added to oil varnish and doesnt need grinding.

post-3446-0-49035500-1394016378_thumb.jpg

post-3446-0-96700000-1394016386_thumb.jpg

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About that Espresso Method, pardon my ignorance, but does it have to be an Espresso machine? Will a filter coffee maker also work perhaps? Something like:

post-63555-0-20451500-1394014800_thumb.jpg

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FredN can you explain what you do with ferric sulfate to get a brown? I once put some dissolved in water directly on wood and it just made an ugly gray black color.

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About that Espresso Method, pardon my ignorance, but does it have to be an Espresso machine? Will a filter coffee maker also work perhaps? Something like:

Kallie, every other madder lake experiment I've ever done until now used normal coffee filters and gravity to filter things, and the problem is that the filter clogs up with debris really quickly and the flow slows down to just a drip, and takes forever to complete.  The beauty of the espresso maker method is that the hot water is forced under pressure through the filter cup.  It doesn't get clogged and slow to a trickle, but is finished in just a couple minutes.

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Seth

Nice to see you back and Thanks for starting this thread. Until now I've been using Kremer made madder lakes. I've found them nice for color but hard to grind smooth. Always debris left. A friend gave me a $50.00 gift card from Amazon and after reading this thread I knew what I'd spend it on. A Krups espresso machine($49.99). Perfect timing.

I'm looking forward to trying Neils pigment. It looks great on his blog.

http://www.amazon.com/KRUPS-XP100050-Espresso-Frothing-Cappuccino/dp/B008EYPKB8/ref=sr_1_26?ie=UTF8&qid=1394052348&sr=8-26&keywords=espresso+machine

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Kallie, every other madder lake experiment I've ever done until now used normal coffee filters and gravity to filter things, and the problem is that the filter clogs up with debris really quickly and the flow slows down to just a drip, and takes forever to complete.  The beauty of the espresso maker method is that the hot water is forced under pressure through the filter cup.  It doesn't get clogged and slow to a trickle, but is finished in just a couple minutes.

 

Thank you for explaining. Reason I asked is because I do have an old filter coffee maker which I can use, but it seems I'll be going to the shop soon to buy an espresso machine then. :)

 

Oh and on another note, can someone tell me what kind of places would sell Alum and Potash? Is there a wrong and right type which is available? Already got the madder roots a while back, but never got 'round to actually using it.

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Hi CShabbon,

As a  test run with alum, I used about a tablespoon of ground madder added to about 2Oz  v hot water with about a teaspoon of grated soap.  Stir and let it set for for a couple minutes, then filter through a coffee filter in a funnel, then carefully wring the filter like you would clothes to get  all the liquid through the filter. To precipitate the dye out of this liquid, make about 6 oz saturated solution of alum and water (room temp ok). Add this with vigorous stirring for ca minute, then let it settle. The liquid in the container with the settled dye is carefully drawn off with a baster, and if it hasn't settled enough to do this, pour it all into a coffee filter and rinse 3-4X or until it has lost its yellow color. Take the filter out and spread it out to dry ( I put it on the edge of my wood stove). When it is dried, scrape off and add to turp. I don't know if I would add to a varnish cause adding to turp gives you another chance to filter. The color was a bright  reddish orange after dissolved in turp. I used about an ounce of turp, and the color was  almost solid enough that would give color  if applied as a varnish. Of the tablespoon of madder I probably only dissolved about a quarter of the dye on the filter, so this indicates there isn't much loss of color. 

There are a lot of unknowns, eg, how much to use of each, durability, etc. From my observations with iron sulphate, the color is very durable. I extracted color out of madder using lead acetate that I spread on wood that lasted for years (in my cellar)  with no change, so I think fading might not be a problem.

Alizarin is a very intense dye, but it only makes up about 1% of the madder molecule, most of it is complex glucose, so the method seems to get most of the dye. Hopefully we have a good inorganic chemist that can review what I think happens. As I stated in an earlier post, this method was used to waterproof cloth, etc, the only addition was adding madder.  fred

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