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Seth_Leigh

let's make some madder lake

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Along with my other thread on making mastic varnish, I decided to make another thread on making madder lake. This stuff isn't hard to make. You don't have to be a rocket scientist to do it. It's a little more involved than making mastic varnish, but it's not a big deal. Trust me. Hopefully these pictures will help demonstrate that.

I decided to follow the David Rubio recipe again, which I've done a couple times before back in 2004, but this time I decided on a couple of modifications. In conversation with Fiddlecollector I've learned that exposing the roots to some acid (he has used acetic acid, and some French recipe he emailed me used sulfuric acid!) can free up some more dye molecules from being bound to a sugar molecule, resulting in more madder color. I say huzzah to that. I want the deepest, darkest madder lake possible. I'll describe my vinegar modification to the Rubio method later in the post.

I also decided not to mess around, and to double the Rubio recipe that can be found at this link. So, whereas he said to use up to 180 grams or so of madder roots, I'm using a whole 390 grams of roots. I wish I'd only multiplied the recipe by 1.5x though, since these roots have expanded so much in the bottle I'm a little worried about how much free liquid I'll have in there to slosh around and accept the coloring as it comes out.

But anyhow, I used 390 grams of roots, so there we are. I put them, a cup or so at a time, into the blender and reduced them a bit over how they'd come from Kremer. I didn't reduce it all though, just some. I didn't reduce the root pieces at all when I made it before in 2004 and it seemed to work out well, so this ought to be fine.

I added the roots to the pickle jar, added in a lot of water (I didn't measure the water, as Rubio does in his recipe, I just tried to use "enough"), and then added around a cup of vinegar. This I did last night, and by the time I go to the next step, the roots will have been exposed to the vinegar for 30-35 hours. This vinegar exposure is a modification of the Rubio recipe.

I don't really want the acetic acid to be in the jar still when it's time to go to the next step. Fiddlecollector has informed me that acetic acid evaporates really quickly. I've got the roots sitting in a double boiler right now at a fairly low simmer. Hopefully over night the acetic acid will be gone. I'll probably crank up the heat a little in the morning and let it boil, or nearly so, for a few more hours to help make sure the acetic acid is gone.

The next step will be to dissolve 120 grams of potash in some water and add it to the roots. I will then let that sit in a nearly-boiling double boiler for a few hours. Note: The Rubio recipe says not to let the liquid get very hot, like over 110 F or so. I've had multiple people on Maestronet tell me they boil their stewing madder roots without the deleterious effect Rubio warns of. I'm taking their word for it, and I will boil, or nearly boil, my roots.

After the roots have stewed in the potash water for a few hours, probably overnight, I'll go ahead and pour out all the madder dye liquor into another jar, and strain out all the wood chunks. I'll add the alum water, stir it up, and after the reaction has ceased, start the washing. I'm going to wash this stuff a lot, and I'm going to take my time doing it. It'll probably take me a few days to get done washing it.

The water I'm using is coming out of my reverse osmosis system. This means it will have very little minerals in it, but will not be "soft" water in the traditional sense. I have a water softener, but I won't be using the soft tap water for any part of this. Yes, I will even wash the lake in RO water. One of the problems I had with my previous batches of madder lake has been that it's been very difficult to grind into a very fine powder successfully. One of the worries I have is that minerals from my New Hampshire water may have accumulated in the lake and made it harder to grind. That's just a guess. Now with my Arizona RO water, that's not going to be a problem.

My plan here, as I enter seriously into my cello project, is to have a large quantity of madder lake, and a large quantity of mastic varnish. I also have a, wait for it, large quantity of asphalt that I will be using to color the varnish along with the madder lake. I want to make a fairly large jar of colored varnish that looks good, and will last not only for this cello project but for quite a few instruments in the future. I'd like to start settling in towards some kind of consistency in my varnish, and doing a large batch at once should help me achieve that.

Here are all the "chemical" ingredients used for making madder lake. Some tools like a couple of buckets, a plastic tube for syphoning the water off during the washing phase, and a strainer and coffee filters, are not shown. In fact, I'm going to have to drop by Home Depot and pick up a couple of new, clean buckets for this. And I'm not sure where the strainer ended up after the move either, so who knows.

madder lake ingredients_9535.jpg

Here's the jar with 390 grams of roots in it, a lot of water (at least a couple of liters) and a cup or so of white vinegar.

soaking madder mnet 9539.jpg

Here's the jar sitting in a double boiler on the stove, where it's been simmering for several hours already. I'm going to let it simmer overnight, and then turn the heat up some and let it nearly boil until noon on Wednesday. This is to hopefully drive off most of the acetic acid before I add the potash water.

stewing madder mnet 9543.jpg

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Seth, ive just finished filtering some lake made using that French method i mentioned. I used 400 gms of chopped madder.Along with all the acid cleaning first . Filtering was a pain so ive got it fixed up to a filter flask, a large plastic buchner funnel and a hand held vacuum pump.(speeds the filtering up no end).

I had an accident spilling around a third of the lake over the floor ,with what i have left i reckon i have enough lake for around 20-30 violins.

A couple of pics attached of the filtering , to give you an idea of the size, the funnel alone is 4 litre capacity(largest i could find).

The lake on the filter paper is approx. half of the finished amount.

89267599-DSC_0012.JPG

123931066-DSC_0014.JPG

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I dont read any newspapers,

i got them from a neighbour,we keep a lot of pets!

Yes its one method described by Perego,attributed to JFL Merimee.

Merimee was the father of Prosper Merimee.He was also the uncle of Fresnel( those into astronomy will know him).He also wrote the first in depth study into pigments.

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Hmm, that looks like some very nice madder lake, Fiddlecollector. I guess what scared me off about the method described by Perego was the seeming waste of so much dye stuff in the initial washings. But hey, I can't argue with success, and the stuff you've got there looks fantastic. I'll reread that recipe again and consider doing it just that way for my next go around. I also covet your filter flask. That's just brilliant. Filtering the water out of the lake through a coffee filter, as you know well but others don't, takes seemingly forever.

This morning I'm going to dissolve the 120 grams of potash into some nice reverse-osmosis filtered water and get ready to add it to the stewing madder roots. Man oh man, as I type this I keep looking at that lake Fiddlecollector's got there, and it's just the nicest looking stuff, and significantly darker red than the stuff I made back in 2004. One last question, Fiddlecollector. When you were washing the roots using the Perego method, did you ever get the feeling you were wasting a ton of dye stuff through the washings?

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Seth,

Yes i was abit put off by all the acid washing but ,it seems to leave all the right dyes in the root .The ones you want are only leached out when you add the base(sodium carbonate),plus the acid does a good job of hydrolysing the dyes so your yield can be improved by about up to 50%. The process involving boiling ,but you can have the lake made in an afternoon and just leave it to settle and to wash it.I have decided to try a slightly different mordant combination in the next batch(alum + maybe tin and some copper) ,hopefully to darken it even further, but keeping it bright and transparent.

If you want to darken the lake usually you try and concentrate the madder colour extract ,keeping the dye solution in a small a volume as is practical.Also you can try leaving the lake for around a week to set the colour better before you start the washings.

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Hi fiddlecollector,

your madder looks fantastic!!! Very good colour. What about the french method you were useing, you mentioned that you had mentioned it before, would you give me a hint where to find it? I had a search through old threads about Perego madder, I found one, interesting one too but it didn´t include any info about the making process...

martina

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Seth, forgot to mention you dont really need to go to too much trouble to remove the vinegar,last time i made it, i l added the vinegar left for a few days in a warm place and just added the carbonate.Then i left it in a warm place for another couple of weeks, it seemed to ferment alot and had a distinct smell of salty seawater/or rock pools.Only then did i remove all the madder root and sediment before adding the alum.

It seemed to be worth all the waiting.

If you want to be very authentic ,you can use old urine and woodash,instead of the carbonate.

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Fiddlecollector, if you don't mind I have another question for you.

A lot of the liquid is taken up by the roots. Do you press this, or use a centrifuge, or in any other way try to recapture the liquid from the roots, which presumably will have a lot more dye stuff in it?

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quote:


Originally posted by:
Seth_Leigh

Fiddlecollector, if you don't mind I have another question for you.

A lot of the liquid is taken up by the roots. Do you press this, or use a centrifuge, or in any other way try to recapture the liquid from the roots, which presumably will have a lot more dye stuff in it?

I dont have access to a centrifuge any more , i just squeeze it the best i can and wash it with a little more water .I suppose an old press like you often see on ebay would be useful for that.

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Today, just after noon, I added 120 grams of potash dissolved in water to the stewing roots, and let it stew for around 12 hours. Tonight I ran the roots through a coarse strainer to remove all the bulky root chunks. This left a very large amount of particulate matter still in the liquid that went through the strainer, mostly because I'd run the roots briefly through the blender to break them down into smaller pieces.

On second thought, running the roots through the blender was a dumb idea. I don't know how much advantage I got from reducing a lot of the chunks into smaller pieces, but I sure did generate a lot of hassle for myself. In the second picture, below, I'm running the dye liquor through an old t-shirt stretched over a 5 gallon plastic bucket to strain out the fine particles. The problem is that there was so much particulate that the shirt shown in the picture clogged up and the flow of liquid through it all but stopped. I took some cheescloth and lined the strainer with it and ran the liquid through that to remove some more of the particulate, and then had to stretch another tshirt over the bucket and try again. It's going very slowly, and I'm going to have to leave it and hopefully it'll be all filtered by morning. And I still won't be done. I really want to get all the particulate out, so I'm probably going to run it all through a tshirt again, and then through a coffee filter. This would be a lot easier with Fiddlecollector's filter and flash with the little hand pump for generating a bit of vacuum in the flask to help suck the liquid through the filter.

I would not have had nearly the amount of particles to filter out if I hadn't put the roots through the blender, so I'm going to warn you all and say "Don't do this! It's a big huge hassle!"

Anyhow, when I've got just a nice dye liquor with no particulate matter in it as far as is in my power, I will make a solution of 120 grams of alum in water and add it to this liquor and actually make the lake. What happens is the alum and the potash react chemically to produce a particulate that is not soluble in water and so it settles out to the bottom of the bucket. Washing this particulate lake so that it's free of any residual unbound dye and unreacted potash and alum is all that's left, and then filtering the lake so that it's more like a paste, as Fiddlecollector shows, and then drying it out, is all that's left.

straining out the roots 9551.jpg

filtering out fine particles 9552.jpg

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Ouch. I have to admit something here. I'm really embarassed by this. The reduction of the madder root chunks in the blender was more than I'd done in the past, and it's turned out to be a real disaster. There is so much particulate matter that it's been a real bear trying to filter it all out. I have finally, after several different tries, got it all filtered through tshirt cloth. The buildup of fine mud on the shirt that clogged it and stopped the flow was so rapid, and so complete, that it took me around five different attempts to get it all through just one time. Then I filtered it through shirt cloth again, and this time it took me two different filterings to get it all through. Then I filtered it all through again, and this time all the liquid went through in one pass, but there's still some fine particulate left in there.

So, I tried the coffee filter. Unfortunately the fine particulate that's left clogged it nearly instantly, so I tried paper towel instead. Ditto. So I pulled the two-ply paper towel apart and used, literally, half a thickness of paper towel, and I'm having success getting the liquid through it, albeit slowly and over a few different pieces of paper towel. I believe, however, that when I've got it all filtered through half a paper towel, I'll probably be able to filter it through a coffee filter and have it all go through.

One good thing is that the quality of the liquor that I got through the coffee filter earlier is outstanding, and particulate-free. It looks great. The bad news is with all this filtering through absorbant material, and with all the mush that I collected out of the liquid on the tshirts and had to rinse off and whatnot, I've lost probably half the volume, or more, of my liquor. I'm seriously considering starting over from scratch, and not reducing the root chunks at all. In fact, when I do this again in the future, I'm probably going to put all the roots into the bear strainer and filter out anything small enough to get through the strainer, and use only the chunks large enough not to get through the strainer.

I think what I'll do for now, however, is just finish filtering what I have and continue with the making process, and see how it turns out. I have enough roots left to do another batch (not sure if I have 400 grams though, but I could do a small batch), so if my colossal screwup here causes my lake not to be colored enough, I'll just start over.

Man, I'm pretty embarassed to have done this in public, in the process of showing "how it's done". I'd reduced the roots to some extent in a previous batch, but not generated as much "dust" that time, and it was with a vastly smaller quantity of roots so that it didn't amount to nearly as much trouble as I've had with this one. So much for innovating during a demonstration.

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Here's a picture I took tonight showing the fine particulate matter that clogs up the paper filters and slows the passage of the liquid down to single drops at a time, very quickly. The liquid that left this particulate in the coffee filter had by this time already passed through an old tshirt at least three times, and passed through a single layer from sheets of two-ply paper towels about four times. I've got some more of my madder liquor to pass through coffee filters, and then I'm going to stop filtering and get on with it. Without the kind of filtering gear that Fiddlecollector has, this is about as good as it's going to get for me.

Since I've lost the majority of my liquor, I'm not going to continue with the original amounts of potash and alum. Rather than 120 grams of alum, I'm going to use 100 grams, and I'm going to add 40 grams of potash to the liquor before I mix in the alum. I have no idea which of the two will be left in excess after the reaction, but since they're both soluble in water I'm not worried about it. The washing process will take care of eliminating any extra potash or alum from the lake.

filter residue 9555.jpg

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I've got some completed madder lake. I have to run off right now to a recital my daughter's playing in. I'll take a picture of it when I get back. My wife accidentally threw away about half of the dried lake that was sitting on a couple of shriveled up coffee filters because she didn't know what it was (the ARGGGGGGGGGGGG heard round the world when I found out), when she was doing some cleanup in the kitchen area. It's also a good color, but it's unfortunately lighter and not as strongly colored as yours.

I'm going to make some more as soon as my filtering setup gets here, which I told you about. For those who don't know, I ordered off eBay a filtration flask and funnel, with some filter paper, and a hand vacuum pump, for a system like Fiddlecollectors'. It'll make my next batch (which I intend to do this week, hopefully) go a lot more quickly. I'm shooting for a lake that looks like the stuff you posted a pic of.

Fiddlecollector, by the way, in that picture you said you'd used 400 grams of roots. How many grams of potash and alum did you use?

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Fiddlecollector, that photo essay was awesome! That's pretty much what I was trying to do, basically demonstrate how to make this stuff. Only I messed up bigtime when I ground a lot of the root into practically dust, causing me to lose the majority of my dye. Also, I had all the different dyes in it, not just the really beautiful red that you got. I haven't photographed the lake that I made yet. I'll photograph it tonight and show what it looks like. It's OK, it's just not nearly as strongly colored as I wanted. I want very, very strongly colored lake so that I can get an effect with as little of it as possible. Oh well, my mastic photo thread has worked out well.

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