Madder & Chalk

Most sources agree that you need chalk to unlock the true reds of madder. I’ve always had a difficult time reconciling that with my own results, so experiments were called for.

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I spent the past summer with a lot of experimental dyeing, and one of my themes was how chalk affects madder red.

Earlier in the year, I had experimented to see if I could remove the yellow tones from madder by soaking the madder in hot or cold water and discarding that water before dyeing (extraction) but according to my experiments, that’s not possible.

So the problem remained: sometimes I get a nice saturated red, other times a less saturated, more orange tone, although I use the same dyeing method.

My earlier experiments didn’t show a large difference between reds from rain water and tap water. The red with rain water is only slightly better than the one with tap water, but that is because the tap water is soft here.

But I have heard from several other Danish dyers that they have hard tap water, and that destroys the madder reds for them. I’ve also seen that myself where I used to live before, in a place with hard water.

This observation is quite consistent – but – is directly contradicted by a large body of work by many different authors, of mostly English-language dyeing books. Here’s a small selection from different authors:

“Chalk or slaked lime is added, particularly in areas with soft water.” John & Margaret Cannon: Dye Plants and Dyeing, p. 76.

“Add a tablespoon of ground limestone or chalk dust.” Rita Buchanan: A Dyer’ Garden, p. 52.

“If the water is deficient in lime, brighter shades are got by adding a little ground chalk to the dye bath.” Ethel Mairet: Vegetable Dyes, p. 42.

“Powdered chalk or limewater should be added to the dye-bath if the madder is ‘acid’.” Quote from Hellot’s “Art de la teinture des laines et étoffes de laine” in Dominique Cardon: Natural Dyes, p. 113.

I could go on like this. Source after source points out that chalk should be added. Some say if there is not “enough” or ir if the madder is “acid”, others just always add it.

It’s not clear where the idea comes from, but it seems to have been in circulation for a very long time. Hellot, quoted by Cardon, published his “Art de la tenture” in 1750, and it has been a very influential book.

The plant it’s all about – madder, Rubia tinctorium. Here a second-year plant growing in my dye garden in the middle of the summer.

In order to understand the effect of madder and chalk, I carried out a series of dyeing experiments on wool.

In all experiments, the proportion of madder to wool was 1:1, and I dyed at approx. 55 degrees C. I let the madder soak in water overnight, then dyed in that dye bath. During dyeing, I held the temperature for an hour, then let the yarn cool off in the bath until the next day.

First, I wanted to find out if it is chalk in tap water that affects the madder color, or something else. And by “something else”, I mostly mean iron, which may be present in tap water, and can affect colors a lot, when present even in small amounts.

For comparison, I began by dyeing a skein in tap water.

Then, I added chalk (from a garden center) in the amount of 4 g/L. That corresponds to about 2 Tsp in 10 L of water, giving a very slightly elevated pH of 7-8 instead of plain 7. The amount was just a guess, at that point in my experiments, I didn’t have a good idea of how much to use. I tried adding that amount both to tap and rain water.

Finally, I tried quicklime, which is a very strong base. So I neutralized it with a strong acid, since base destroys wool.

The results from that first round are below. On the left, yarn dyed in tap water, a paler red, the usual shade with tap water. When I add chalk to tap water, the color darkens slightly, just slightly. With rain water and chalk, the color is a bit lighter that with tap water alone, but very similar. So the conclusion so far is that chalk is the component in tap water that affects the color, not something else like iron.

But to be more sure, and having read that chalk for the garden can contain iron, I also tested quicklime. Calcium in tap water and in chalk for the garden is CaCO3 (calcium carbonate). Quicklime, on the other hand, is Ca(OH)2 (calcium hydroxide), a strong base. It was impossible to measure accurately, so I just took some of the chalky water in my bucket of quicklime and added it to demineralized water. This way, no other metals or minerals are present. I then neutralized the quicklime with a strong acid (I don’t remember which one).

The result of the quicklime experiment is seen at right. A very dusty pale red. So my conclusion so far is that yes, chalk has an effect, which is to make madder red paler and dustier, not more intense red. And yes, the component of tap water to affect the color is chalk. And the more of it (the harder the water), the larger the effect.

Madder dyeing in tap water, tap water with added chalk, rain water with added chalk, and demineralized water with neutralized quicklime.

After this first round of experiments, I started thinking that I had added too much chalk. It might just be that there was a good effect at a certain low amount, but that too much chalk added could ruin the color. Having searched through my entire dye library, I finally found the figure 1-2% mentioned by Mairet. Most books just give nonsensical directions such as “a spoonful per dye pot”.

In order not to miss the sweet spot, I tested addition of 0.2, 1, 5, and 10% chalk. The result below was not entirely what I had expected. There really is no difference between dyeing in pure rain water and adding up to 5% chalk. The color began changing very slightly at 10% added (becoming paler) but the difference is so small that the photo does not capture it.

Wool dyed with madder in rain water with no chalk added, and with 0.2, 1, 5, and 10% chalk added.

I couldn’t really decide if this was a good or bad result. Chalk in relevant amounts does not have an effect. It does not help unlock the good reds, but it also doesn’t do any harm.

But if all the English-language dyeing books are wrong, are the Danish dyers then right? Does the red color improve with less chalk? Below, a comparison of madder dyeing in rain water, tap water, and demineralized water. There is the usual difference between rain and tap water, the former giving the better red.

I took extra care with the yarn dyed in demineralized water. After mordanting, done in tap water as usual, I washed the yarn in rain water several times, and also cleaned the glassware for dyeing in rain water. That treatment gave the best red in the entire experiment, so I have to conclude that less chalk gives better red.

Dyeing with madder in rain water, tap water, and demineralized water. Tap water gives the least good red, demineralized water the best.

Below, I’ve shown all the colors in one picture so it’s easy to compare them.

All colors from the test together. All are 1:1 madder on wool, and cards grouped together were dyed simultaneously in glass jars over a water bath.

So my result is very clear – less chalk gives better reds. But one mystery does remain. Why do all dyeing books from the last 3 centuries state that madder gives better reds when chalk is added?

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Madder’s Family

Madder has several relatives that are also rich in useful reds. These plants are native here in Denmark, and have been used as red dyes a very long time back.

Believe it or not, the year is drawing to a close. So, I want to try to summarize all the many dyeing experiments I did over the year.

This summer, I searched for madder’s relatives, to find as many as possible. Madder, Rubia tinctoria, belongs to the madder family (Rubiaceae) in which you also find the bedstraws (the genus Galium).

Galium species do not contain as large amounts of red dye as cultivated madder does, but several of the species grow wild here in Denmark, and their historical use is well known.

Madder plant growing in my dye garden.

The first Galium species to present itself was cleavers (Galium aparine). It’s everywhere! Anybody who has ever walked outside surely know this plant. Or at least its seeds. They are extremely good at clinging to clothing and dog fur. The whole plant is covered with clingy hooks – the very same that cultivated madder has.

My attempt to dig up cleaver roots quickly came to an end. The roots have the thickness of sewing thread, so a lot of digging is required. But the roots are said to contain dye, so I’m keeping them on my list of maybes.

Cleavers up close. You can see the characteristic clingy hooks on the seeds. The very same that madder is covered with.

Lady’s bedstraw (Galium verum) is the plant mentioned by most natural dyeing books. I tried growing it in the garden this year, seeding it outside in the spring, but nothing grew.

Whenever you’re looking for a specific plant or mushroom, but haven’t found it yet, it’s simply invisible. But, once you find it, you start seeing it everywhere. The relationship between Lady’s bedstraw and myself developed exactly like that over the summer. Once I found it, it was everywhere! For example this coastal grassland:

Coastal grasslands with very sandy and infertile soil, perfect for Lady’s bedstraw. I took this picture in a region of Denmark called Mols.

 

Lady’s bedstraw truly thrives in the nutrient-poor, sandy soil, along with yarrow and St. John’s wort.

Lady’s bedstraw growing in a big cluster.

Unfortunately, several walks with a shovel only yielded a very small handful of Lady’s bedstraw roots – so little that my scale didn’t register. Like with cleavers, the roots are extremely fine, and they tangle up with roots of grass etc. In combination with stony, sandy soil, the digging job gets hard. To get your hands on a larger pile of these roots, I suspect you have to grow them in a well-prepared sandy soil without obstacles. Anyway, I tried dyeing with my small handful of roots, but it gave almost no color.

But then, on a forest walk, this plant turned up – hedge bedstraw (Galium mollugo):

Flowering hedge bedstraw photographed in July.

Hedge bedstraw is also mentioned by different books as a dye plant, so I brought out the shovel once more. Again, it was difficult. The forest soil is obviously full of tree roots that make digging quite impossible. But I managed to get a couple of handfuls of roots, mainly because hedge bedstraw roots are not that thin. I dug up the roots on July 9th. The next day, after cleaning, the slightly dried roots weighed 30 g.

My pile of hedge bedstraw roots, with reds clearly showing under the out bark.

I soaked the roots in cold water overnight, then dyed my usual alum mordanted 12-gram skeins of Fernris to test the dye. I removed the overnight water because Jenny Dean does, but I should have concluded from my madder experiments that it is not necessary to do so. The water used to soak the roots overnight simply contains a small amount of dye, with the same properties as the dye you extract when you heat the roots in water (the small 6-gram skein laying across the others in the picture below was dyed with the discarded water).

Then, I dyed alum mordanted 12-gram skeins in a 1st and 2nd dyebath, in exactly the same way as if it had been madder: heating up to 60 degrees C, then leaving the yarn in the dyebath until the next day. The first bath gave a convincing red-orange, which would not have been a surprise had it been madder I was dyeing with. The dye is less abundant in hedge bedstraw than in madder, but the difference is actually smaller than anticipated. Here, I used 30 g of roots on 12 g of yarn, with madder, you would get this shade with less than 100% weight of fiber.

After the second bath, which also worked well, I was evidently feeling on top of things, and threw in a 50 g skein. There was not much dye left, but to extract everything that was there, I left the bath with yarn in a jar outside. That was in mid-July.

A couple of times, I heated the entire jar over a water bath to give the process a helping hand, but the rest of the time, it was just standing there. I turned over the yarn to get an even dye, and for a while, it also fermented. Both time and fermentation should help release the dye. Also, I imagine that a skein of yarn in the bath will soak up the dye as it is released, permitting more to come out (alizarin has a rather low solubility in water). In any case, my large skein stayed in the jar for 6 weeks, and turned out a pleasing coral color. And, the dye bath ran clear, so there was probably nothing left in the roots.

Dyeing with roots of hedge bedstraw (Galium mollugo). 1st bath (left), 2nd bath (middle), and the large skein on the right is fermentation of the 3rd bath. The small skein across was dyed in the water used to soak the roots overnight.

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Tansy Experiments

Among some natural dyers, tansy is seen as quite boring. It’s a common plant, easy to find, easy to dye with, and it contains the so-common yellow – just like so many other plants. But tansy has a long cultural history, and its yellow dye is of high quality!

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Tansy’s common name is simply an abbreviation of its latin ditto, Tanacetum vulgare. I recently ran into a nice (and plausible) explanation of the name in an old Danish book by an important author on natural dyeing, Esther Nielsen. She writes that Tanacetum is probably a derived form of Athanasia (a-thanasos means immortal). Supposedly, the immortality is a reference to the fact that the flowers keep their strong yellow, also when dry.

Tansy, Tanacetum vulgare.

Tansy has been used in herbal medicine for centuries. The plant is poisonous, especially to insects, and was used against intestinal worms. Today, eating tansy is not recommended, and it’s now known that its toxicity comes from the alpha-thujone content in all parts of the plant.

Nevertheless, it was used as a herb in the past, and it does have a very strong smell. I usually boil tansy dye baths outside!

As a natural dye plant, tansy has a lot of advantages. The plant is very common, so you’ll find it growing at just about any roadside – at least here in Denmark, which is in tansy’s native range. Since the plant is so common, it’s completely fine to harvest as much as you need, as long as you cut the flower stalks of, leaving the rest of the perennial.

The yellow color from tansy is very light fast, in my light tests, it always comes out as more fast than weld yellow, which is known for its good light fastness.

According to this paper (Phytochemistry 51, p. 417, 1999), tansy flowers contain a lot of apigenin and luteolin, the same yellow dyes that you find in weld. The leaves contain slightly different compounds (that are similar to luteolin, but not exactly the same). So it makes perfect sense that leaves and flowers give slightly different yellows. I’m not sure, though, why the light fastness of tansy yellow is better than that of weld yellow in my experiments…

After reading about dye extracts (somewhere), I decided to try making a tansy extract. Extracts are obviously a compact way to store dyes, but I thought that they might be interesting for other reasons, for example printing on fabric.

I even found a paper where the authors described concentrating tansy extract to the point that it became a powder. So this is what I tried:

500 g (just over a pound) of fresh tansy flowers and leaves (picked August 11th) were boiled in enough rain water to cover them. I left the pot until the next day, strained out all the plant material, then boiled the extract to concentrate it until it didn’t loose any more water. I also dried it in the oven at very low heat. And the result was a small amount of extremely sticky tansy syrup:

Tansy syrup – dark brown, smelly, poisonous.

So my extract clearly didn’t turn into a powder, but a very dark and sticky syrup. Ages ago, in organic chemistry class, I was taught that syrup means impure product. But I guess that is expected in this case, since I just concentrated a crude extract of the plant, which is a mix of many different compounds.

To test my syrup, I simply dissolved it in water and used it to dye 100 g (3.5 oz) of wool (Fenris) instead of exploring more exciting options. I wanted to see how the dye was affected by being turned into syrup and back again. Here is a comparison with 100 g of wool dyed with 500 g of fresh leaves and flowers (left), 500 g of fresh leaves and flowers dried and then used (middle) and tansy syrup dissolved in water (right):

Fenris pure lambswool dyed with fresh tansy (left), dry tansy (middle), and tansy syrup (right).

The picture above shows, that the color from tansy is the same, whether fresh or dried flowers and leaves are used. And that is good to know – drying does not affect the dye.

The skein on the right, dyed with tansy syrup, is a bit browner than the two others. But other than that, the syrup treatment didn’t really affect the dye potential. Next year, I want to explore plant syrups more!

But once I got started with tansy experiments, more followed. While cleaning up my dyestuff storage, I found some dry tansy leaves from last year (2016). I wondered if long storage would affect the color – in the picture above, there’s no difference between yellow from fresh and dried tansy, but I only stored the plants for a couple of weeks.

I also wanted to answer another question: In order to extract the dye, is it more efficient to finely crush plant matter, or is it OK to throw whole leaves in the dyepot? So I powdered some dry 2017 leaves in my mortar to see if the color intensified, and the result:

12-gram skeins of Fenris, each dyed with 25 g of dry tansy leaves. Whole 2016 leaves (bottom), whole 2017 leaves (middle), and powdered 2017 leaves (top).

The skein dyed with powdered 2017 leaves has exactly the same color as the skein dyed with whole 2017 leaves, so there’s no gain by powdering the leaves. Luckily, since that process is really cumbersome. The 2016 and 2017 leaves don’t give exactly the same yellow, but very close. I don’t think this small difference is caused by an extra year of storage – rather, the fact that the plants didn’t grow in the same place, the difference in weather and harvest time might have caused the small difference in color.

Red Madder

Madder is one of the most ancient dyes, and one that is described in pretty much any book on natural dyeing. But every book seems to give a slightly different method for obtaining the sought-after madder red. There’s only one thing to do – experiment!

A bunch of madder dyed skeins. They’re all dyed in slightly different ways, so the colors have turned out differently.

Madder was one of the first natural dyestuffs I tried just when I began learning about natural dyeing, many years ago. I followed Jenny Dean’s “Colours from Nature”, the first book I bought back then (now, of course, I have a largish library on natural dyeing).

Dean gives a dyeing method for larger pieces of madder root, not powdered root. She rinses the root in cold water, then boiling water, and then adds the water for the actual dye bath. I tried her method for my first attempts with madder, but only got a series of tan/coral shades. Sometimes slightly more pink, sometimes more towards orange.

After my first attempts, I was ready to just give up. Coral was not exactly my favorite color, and I didn’t make any further attempts with natural dyes. That was until I happened to talk to some dyers at iron age and viking markets. One of them told me, that she always got good reds with madder by using destilled water.

After that, I happened to find a copy of a classic Danish dye book from 1972, “Dyeing with Plants” by Ester Nielsen. Nielsen steeps madder for 24 hours, and mentions nothing about changing the water at any point. Also, she mentions nothing about the type of water. Over time, I arrived at a variant of Nielsen’s method, using rainwater instead of distilled water because rainwater is free. I leave the madder to steep overnight in my dyepot, add alum mordanted wool, heat slowly to 55 C, and then wrap the pot in a blanket and leave it until the next day. So, yarn and madder in the pot together, and no changing the water.

I’ve achieved many clear reds with that method, but sometimes, the color has turned out more orange than red. That’s the case with the yarn for this hat:

Brisingamen hat in madder dyed yarn.

I do like orange, but it’s red you’re after with madder. Also, I’ve become increasingly confused the more I’ve read about madder dyeing, and I am not the only one. As mentioned, Dean uses a hot extraction (a soak in water that is discarded) whereas others, for example Ecotone Threads use a cold extraction.

Madder contains many different dye compounds. According to “Handbook of Natural Colorants” by Berchtold & Mussak, more than 35 different anthraquinones have been detected in madder (anthraquinones are the type of molecules that alizarin, the important red in madder, also belongs to). The different dye compounds have slightly different colors, so the the point of (cold or hot) extraction would be to remove some of the yellow or brownish ones.

I decided to test, whether I could get rid of my orange reds by using an extraction method. For this test, I’ve used my usual 12-gram skeins of Fenris (100% wool) mordanted with 10% alum. In all the experiments, I used 12 grams of madder powder per skein, leaving the madder in the dyepot the entire time. A few writers say that the madder should be removed from the dyepot before fiber is added, but most agree to leave it in.

According to Liles’ “The Art and Craft of Natural Dyeing”, alizarin has a very low solubility in water, and that’s why the madder should stay in the pot. As alizarin in solution is taken up by the yarn, more will be released from the madder. In all cases, I dyed the yarn by heating yarn and madder to 55 degrees C keep it there for 1 hour, and then leave the yarn in the dyebath overnight.

In my little experiment, I tested the following, both with rainwater and tap water: steeping the madder overnight and dyeing in the same water, filtering out the madder and dyeing with it in new water, and finally pouring boiling water over the madder and then dyeing with it in new water.

Filtering a small amount of madder in an old fashioned coffee filter.

Results below:

1: Madder steeped overnight in rainwater, yarn dyed in the same water.

2: Madder steeped overnight in tap water, yarn dyed in the same water.

3: Madder steeped overnight in rainwater, filtered, run-off removed and yarn dyed in new rainwater.

4: Run-off from 3 (the liquid that ran through the filter).

5: Madder steeped overnight in tap water, filtered, run-off removed and yarn dyed in new tap water.

6: Run-off from 5 (the liquid that ran through the filter).

7: Poured boiling water over the madder, filtered immediately, yarn dyed in new rainwater.

8: Poured boiling water over the madder, filtered immediately, yarn dyed in new tap water.

9: Run-off from 7 (not repeated for 8, as it would be identical.

The madder dyed skeins – theme and variations.

Skein 1 is dyed with just one volume of rainwater, which is my usual method. Luckily, skein 1 is one of the good reds in my test. Skein 2 is the same method, but using tap water. Skein 1 is only a slightly bit redder than skein 2, so using rainwater instead of tap doesn’t seem to have the importance that I thought. I measure pH of both baths, and they were both neutral after steeping overnight.

Skein 3 and 5 are dyed with madder that was steeped overnight, and then filtered to remove the first volume of water. If it was true that steeping and removing the water would remove yellow and brown tones, then skein 1 and 3 (both dyed in rainwater) and skein 2 and 5 (both dyed in tap water) should be different, but they are not. My conclusion is, that cold extraction does not remove yellows and browns.

That conclusion also seems to be correct when you look at skein 4 (rainwater) and 6 (tap water), which are dyed with the run-off from 3 and 5. If the extraction removed yellows and browns, then skein 4 and 6 should have those colors, but they don’t. They are tan/coral, exactly the kinds of colors I normally get from second, third and later afterbaths. So this could mean that cold extraction just removes a small fraction of the overall color present in madder.

Finally, the hot extraction. Skein 7 (rain) and 8 (tap) are dyed in new volumes of water added to the madder after the hot extraction. They are weakly colored, and the shades are very similar to those of skein 4 and 6. So most of the color is just gone after the hot extraction, and has ended up in the run-off that was used to dye skein 9.

Skein 9 has a good, saturated red-orange color, which is not that surprising. Temperature is the only factor that more or less all authors agree on. The temperature mustn’t get too high, as that brings out orange or terracotta tones, exactly what I’m seeing here. If  the light fastness turns out to be good, then this is actually a very good method for dyeing orange.

It’s nice to observe that this little experiment fits with my very earliest observations with madder. Deans method gives skein 8, a pale tone that would definitely be disappointing if you are trying to dye red.

So, in summary, the conlusions of my little experiment are:

Reds obtained with rainwater and tap water are not very different, and rainwater gives a red that is only very slightly better than the red with tap water. This conclusion is for my tap water, and may be entirely different elsewhere.

Cold extraction is not efficient for removing yellows, and hot extraction removes almost all the color.

I usually keep the temperature around 55 degrees C, but I have never checked myself to see how sensitive the color is to temperature. And I haven’t even begun to look at pH and calcium. My next experiments will be on those factors.

Hypogymnia Lichen Windfall

I return from many of my walks with pockets full of lichen windfall. One of the common finds under trees is two slightly different species of Hypogymnia, a good dye lichen.

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Lichen windfall is perfect for dyeing, since it does no damage to just pick up the fallen lichens. I’m therefore writing a small series of posts on the different species of lichens typically found in windfall, and I’ve already written about Ramalina fastigiata.

This time, I’ll have a look at Hypogymnia physodes and Hypogymnia tubulosa, two common species that are closely related (that’s why part of the name is the same). Also, they do look alike – both are grey-green and foliose (flattened, leaf-like). Hypogymnia physodes, here seen covering a small branch, has flat lobes, sometimes with soredia on the outer part. Soredia is one of the way that lichens can reproduce, and break through the surface in lots of little dots, making the surface look grainy or powdery. In Hypogymnia species, the soredia are found on the bottom side, which folds up on the tips of the lobes, making the grainy lower surface visible:

Hypogymnia physodes covering a small branch. Detail on the right shows the lobe tips folded up, displaying the graininess because of the soredia.

Hypogymnia tubulosa looks a lot like Hypogymnia physodes, but has hollow lobes. In the right side of the image below, the hollowness is visible since I cut one of the lobes:

Hypogymnia tubulosa with a cut lobe on the right side.

Both species are very common, and grow in many places, including on trees, stones, and wooden surfaces. They like growing on acidic substrates, and Dobson’s “Lichens, An Illustrated Guide to the British and Irish Species” mentions that Hypogymnia physodes is among the species least sensitive to sulfur dioxide pollution. Hypogymnia tubulosa is a bit more sensitive.

The dye content sometimes differs a lot even for species that are otherwise very similar. So I decided to test if the two species give the same color.

I used unmordanted yarn, since lichen colors are substantive. I made one dyebath with 9 g of Hypogymnia tubulosa, and put a 12-gram skein of Fenris (pure wool) and a 5-gram skein of Bestla (merino-silk) in. Another dyebath was 15 g of Hypogymnia physodes, and two 12-gram Fenris skeins and one 5-gram Bestla skein went into that one. So half the weight of lichen compared to fiber in both cases. I modified one of the Fenris skeins in an iron afterbath.

Both lichens give the same color – a fine, dusty yellow, the completely expected shade from bwm lichens. So in conclusion, no reason to sort Hypogymnia physodes and tubulosa. The merino-silk takes the color a little less well than the pure wool, and an iron afterbath does significantly darken/sadden the color at turn it green.

Left: pure wool and merino-silk dyed with Hypogymnia tubulosa. Right: pure wool and merino-silk dyed with Hypogymnia physodes, further right a pure wool skein dyed with the latter, modified with iron.

An Earthball Study

Earthballs contain a yellow-brown dye, but also a large and annoying amount of tiny, black spores. So I set out to find out if the spores contain any dye or if they could just be discarded.

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Common earthball, Scleroderma citrinum.

A couple of years ago, I dyed a lot of yarn with earthballs. The color turned out a nice yellowish brown, but the yarn was simply full of spores that continued to drizzle out, both when winding the yarn into skeins and when knitting with it.

The drizzling pores were obviously annoying, but I also started wondering if the spores are even safe to breathe? It’s usually said that earthballs are “moderately toxic”.

In their book “Färgsvampar & svampfärgning” (Dye mushrooms and dyeing),  Lundmark & Marklund label earthballs “good” dye mushrooms, so it would be a pity to give up on earthballs just because of the spore problem. Lundmark & Marklund mention that earthballs contain the dyes badion A, norbadion A, and sclerocitrin.

Sclerocitrin is also described in the research paper “Unusual Pulvinic Acid Dimers from the Common Fungi Scleroderma citrinum (Common Earthball) and Chalciporous piperatus (Peppery Bolete), Angewandte Chemie International Edition, 2004, 43, 1883-1886 by Winner et al. They show that the “brilliant yellow” dye sclerocitrin is found in “remarkable amounts” in earthballs. As the title says, sclerocitrin is also found in peppery boletes. I haven’t looked for it, but a mental note has been made.

Earthballs have a dark or black spore mass inside, surrounded by a relatively thin outer wall. I decided on a small experiment in order to see if the spores contain any dye. If not, it would make sense to just leave them in the forest.

Halved earthballs with grey and black spores inside.

I used as small amount of earthballs for my experiment, gathered during the fall of 2016 and dried until use (2016 was not a good mushroom year, so not many earthballs were to be found).

Separating the spore mass from the mushroom’s outer wall was incredibly difficult. The parts were completely stuck together in the dry mushrooms, but in the end, I had 23 g of out walls and 10-11 g of spores. I soaked both overnight, the outer walls simply by adding water. The spores were stuck together in stone hard lumps that I separated by grinding them in my mortar. The spores repel water, I solved that by wetting them in denatured alcohol, then adding water.

The next day, I boiled the two dye baths and filtered the spore bath through a coffee filter. It took very long for the liquid to run through, that’s always the case when filtering a solution with many tiny particles. I then dyed a 10-gram alum mordanted test skein (Fenris 100% wool) in each bath, and got the result below – almost the same color from the two.

The top skein of yarn in the picture is dyed with the outer walls, the bottom one with the pores. I had hoped to find that the pores didn’t dye, but clearly that’s not the case. In principle, it’s not surprising, though, to find that sclerocitrin and the other pigments are distributed throughout the mushroom. The dark color of the spores is not caused by a pigment that acts as a dye.

In conclusion, all parts of the earthball contains dye, and discarding the pores would mean discarding a lot of good dye. So the best method for earthball dyeing would be using the entire mushroom, wetting the spores with alcohol, and then investing the time required to filter the entire dye bath before any wool is added.

Yarn dyed with different parts of earthballs. The top skein is dyed with the outer walls only, the bottom skein with pores only.

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Seasonal Color Variation

An experiment with yellow to green tones of birch leaves over the summer. I didn’t see any difference, but most experiments do have different outcomes than expected.

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A fresh new year calls for a new, big series of dye experiments, but I’m going to begin with an old one that was going on for so long that I never wrote about it.

“Yellow can be many things, so for each plant, I will  specify the particular yellow it gives. There will always be differences, the tone being more green earlier in the year.”

This is what Ester Nielsen writes in her introduction to natural sources of yellow in her book “Farvning med planter” (Dyeing with plants). This Danish book, published 1972, is full of useful information, but such a claim as this is just begging to be tested. I decided to use birch leaves for the test.

Birch leaves. It’s impossible to tell from the outside that they contain a good, warm yellow color.

To test the claim that colors are greener early in the growing season, tending towards yellow later, I made two 10 g test skeins of supersoft wool. I dyed each of them with 40 g of fresh birch leaves, since Ester Nielsen recommends 4 times the weight of fiber in fresh plants (twice the weight of fiber if using dried plants). I picked the first portion of leaves on May 11th, the second on July 4th.

The picture below shows the result. The skein in front is dyed with the leaves from May, the back one with thw leaves from July. They’re almost the same color, so my little experiment didn’t back up Nielsen’s claim…

Wool dyed with fresh birch leaves. The front skein is dyed with leaves picked in May, the back one with leaves picked in July.

To check for other possible differences, I tested the light-fastness of the two skeins. But again, no difference. The only thing worth noting in the light test shown below is a really good light-fastness of both yarns. The test took place over more than a month of summer.

Light test of wool dyed with birch leaves picked in May and July.

My conclusion: the time of harvest does not affect the color achieved with birch leaves. But that may only apply to birch leaves. It is possible that other plants to have a variation from yellow-green to yellow as the summer passes.

Harvest

I’ve finally finished harvesting my dye plants and seeds, and it has been an abundant year in the dye garden. In addition to woad seeds, I’ve also harvested seeds of dyer’s coreopsis. I harvested some of them on September 27th, and a lot more when I removed the last plants on October 24th. I don’t know when they should be harvested, but I suppose I’ll see if any of them sprout next year.

coreopsisseeds
Seeds of Dyer’s Coreopsis. Lots of them, and they are tiny.

Then there’s my Japanese indigo, which  grew really well this year. I harvested most of my Japanese indigo, 22 plants, on September 27th. I tried two different ways of drying the leaves.

First, I stripped the leaves off the stems, spread them out outside on a sunny day. They almost dried, and I moved them inside in a mesh hanger before dewfall that evening. In a couple of days, they were completely dry.

dryjapaneseindigo
Drying Japanese indigo bunches. Only the outer leaves dry this way!

Second method (because stripping the leaves off was so time-consuming) was borrowed from Deb McClintock – I hung bunches of leafy stalks to dry inside because by then, the season had changed and the first fall storms and rains were here. But after a week, only the tips of the leaves had dried, because the thick stalks retain all the moisture. I’m sure that would not be a problem under a hot Texas sun, but this isn’t exactly Texas! In the end, I stripped the leaves off the the half-dried stalks and let them dry. So although option two seemed easier, it’s not really an option here – next time, I’ll know there’s no way around a bit of tedious work.

I ended up with a bit more than 400 g of dry leaves, and they are showing a blue tinge. Definitely a good sign.

indigoleaves
My dry Japanese indigo leaves with a blue tinge.

The rest of my Japanese indigo, maybe 8 plants, stayed in the garden. In late September, the plants had quite a few buds, and I wanted to leave some to see if they would flower and maybe even produce seeds. I followed the weather forecast closely to see when the first night frost would come. That was forecast for the evening of October 24th, so I went to our garden that afternoon to harvest the last plants. And they did flower – but no seeds.

indigoflower
Japanese indigo flowering in late October.

The last crop was used for a bit of experimentation, trying to extract indigo from the fresh leaves of Japanese indigo using the instructions from Wild Colours. I stripped the leaves off the stems, washed them briefly, packed them in a pot and filled it with rainwater.

I then left it on my hot plate on low heat, switched on for 15 minutes every 2. hour. This kept the temperature around 35 – 45C, and I left it for 36 hours.

Then, I added sodium carbonate to raise the pH to about 9, and started pouring the liquid back and forth between two buckets. The reddish brown foam is supposed to turn blue (because pouring oxidizes the precursor indican to indigo) but nothing happened. Nothing. The next day, I took out a small part of the liquid, added some sodium dithionite, and tried dipping a scrap of yarn. Again, nothing. So in the end, I tossed the entire experiment. I think the reason for this failure was the very late harvest of my last Japanese indigo. So I haven’t tried my dried leaves yet, but I hope they contain some indigo! I’ll return to the extraction method next year with plants harvested earlier in the season.

Amazing Dyeing Failures 2

The topic of my last post was failures in dyeing, and here’s more. First, my most serious and most annoying failure as a natural dyer.

3: Organic Indigo Failure

A while back, I experimented a bit with an indigo vat with fructose, but my results were not very convincing, in the sense that the amount of blue I got out of the vat was completely underwhelming given the amount of indigo that went in. Mona of Thread Gently on the Earth suggested trying another type of indigo vat that uses madder and bran. So, using what Mona wrote and what her source of the information, Aurora Silk wrote, I tried the madder/bran vat, since I’m still very interested in a natural fermentation vat for indigo.

In the beginning of May, I mixed 34 g of indigo, 17 g of ground madder, 17 g of wheat bran, and 116 g of sodium carbonate. I used at pot with a well-fitting lid, and filled with water so there wasn’t much air in the pot. We had a very warm early summer this year, so I just put the pot outside the house, where it was 27C during the day. But nothing happened. I had suspected that, since the pot would cool off during the night.

My next setup consisted of a simple electric hot plate for cooking. After a bit of experimentation, i figured out that on the lowest setting, and switching it on for 15 minutes out of every 2 hours with an electric timer plug, I could keep the vat around 37C. After a couple of weeks, though, I was forced to admit that nothing much was going on there.

So I started a bit of wild experimentation. Could it be lack of reducing power? I added fructose and more base, but that didn’t get the vat started. I then transferred part of the vat to a large jar, and tried warming it on a water bath. The jar was full and had a tightly closed lid, and that did improve things. The color didn’t shift to yellow-green, it was still blue with just the slightest green tinge (you can see it on the spoon, top left image above), but the jar vat developed the coppery film of a working indigo jar. I dyed small skeins, and they came out a lovely dusty blue.

indigo
Indigo dyeing with a madder/bran vat with a sprinkle of fructose along the way. The vat became slightly green-tinged (top left), but did develop the coppery film that shows it’s working (top right). Bottom, a small skein of yarn dyed dusty blue in the indigo jar.

So it’s sort of working – but not amazingly so. I can only dye very small skeins in this jar, but I did a lot of troubleshooting which may bring me closer to running a fermentation vat properly and over a long time. For now, I do consider it a failure, since I got so little blue out of my 34 g of indigo, but I’m clearly not done with this. Maybe one needs to set up a larger vat, using an amount of indigo that makes abandoning the vat unthinkable.

4: Common Broom Failure

I have tried – and failed – to grow dyer’s greenweed (Genista tinctoria) a couple of times. The seeds need cold stratification, which I have tried to give them, but they never sprouted. Dyer’s greenweed is supposed to grow wild in my part of Denmark, and I have searched for it, but not found it.  Then in June, the landscape was dotted with yellow: it was common (or Scotch) broom (Cytisus scoparius). This plant is considered invasive in many places, but not in Denmark, where it occurs naturally. But it has been spreading in a new way for the past 30 years, so picking it is definitely fine, just keep in mind that the seeds are poisonous.

I studied my old flora a bit, and since both dyer’s greenweed and common broom belong to the legumes (family Fabaceae), I convinced myself that common broom would be worth a try in the dye pot. At that time (June), the flowers were already past their prime, but i picked some branches at the roadside.

Common broom is spreading, adding splashes of yellow to the roadside.

The result was not impressive – good old failure beige once again:

Wool dyed with common broom – hello beige…

I would have called it a failure and left it at that if I hadn’t come across an entry on common broom in John & Margaret Cannon’s excellent book “Dye Plants and Dyeing” (I recently bought a second hand copy). This book tells you that the part of the plant used for dyeing is young branches, picked in April or early May, not the flowering stalks picked in June as I did. The young branches should produce shades of yellow-green with alum and green with copper. I might try this again next year.

“Dye Plants and Dyeing” also mentions some confusion in the dye literature between common broom and dyer’s greenweed, since the latter is sometimes referred to as dyer’s broom. Not surprisingly, Cannon & Cannon (in a book published in association with The Royal Botanic Gardens, Kew) recommend that the dyer relies on scientific nomenclature for dye plants. Actually the same conclusion is reached by Catharine Ellis in her run-in with “broom”.

5: Reindeer Lichen Failure

During my summer holiday, I gathered some lichen of the Cladonia family, I believe it’s reindeer lichen (Cladonia portentosa). In “Lichen Dyes: The New Source Book”, Casselman lists this lichen as a boiling water method lichen that should give a “leaf green” color. So into the dye pot it went, with a test skein of unmordanted wool, since lichen dyes are substantive. The result is not what I hoped. Beige, despite the fact that I used a large amount of lichen relative to yarn:

lichen
Reindeer lichen (Cladonia portentosa) and yarn dyed with the lichen.

6: Cold Dyeing Failure

mommywitch
Mommy is a witch. Check out my cauldron, a dye pot with mushrooms and wool.

At some point, I tried dyeing with old polypores, in the usual hot dyeing process, and that actually gave me a good yellowish brown. Recently, when cleaning up outside, a big hoard of old polypores surfaced. I don’t have enough space to store dyestuffs inside, so they were outside and were damp and looked like they would spoil.

I had a thousand other projects going, so I wasn’t really ready to dye with them – so I decided to try a very lazy experiment: cold dyeing (which I normally never do because it seems to me that it doesn’t really work). The experiment amounted to throwing the polypores into a bucket with rainwater that was just standing there, then put in a small, 12 g test skein of alum mordanted wool, and then letting it stand there for about 3 weeks. You have probably already guessed that it produced a smelly skein of beige wool, which I cannot even find now (I think I overdyed it with indigo). So all I have to show for this experiment is my 6-year old Dagmar’s drawing showing that “Mommy is a witch”. I am taking it as a compliment.

PS: Just as I wrote this, light samples of both the cold dye and hot dye with old polypores surfaced on my desk. None of them have the light-fastness achieved with fresh polypores in a hot dye bath.

Amazing Dyeing Failures 1

Failure in natural dyeing is commonly defined as not getting the result you expected. Beige, off white, baby yellow and other tones of grime are all examples of colors I have made no attempt to acheive, and yet, I have a big pile of skeins just like that. But there’s actually a lot to be learned from failures. Some give new ideas of what to try next. Others just tell you what not to do. Below, I’ll describe some of my failures – actually, I’ve failed so many times that this will only be the first installment, more to follow.

Alle de mislykkede og uønskede farver. Efter billedet blev taget overfarvede jeg med indigo.
Skeins of failure. They were all overdyed with indigo after taking the photo.

1: Bark Failure

Several books on dyeing will tell you that different types of barks are good dyestuffs. For example, Jenny Dean’s “Wild Color” mentions these barks and the color they should produce on alum mordanted wool: alder (brown-green), barberry (yellow), ash (bright yellow-green), apple (warm yellow), oak and willow (beige), and finally elm, birch, cherry, pear, and plum (pink).

For a while, the theme of my walks was bark; in the end, I found enough of these three to try them as dyestuffs:

  1. Birch (Betula) – I’ve used birch leaves several times for a sunny yellow, but not the bark. Some trees were cut down near our house, and I jumped at the chance. The trees had been left in a big pile, which I obviously had to climb to get to the good parts, and since I was of course wearing clogs, I fell down from that big pile in the end. With 60 g of birch bark in my pockets.
  2. Another day I hear some men working outside, shredding logs. On their day off, I casually walked by and managed to peel a good amount of bark off. The logs turned out to be alder (Alnus), the kind with the tiny cones. 70 g of bark.
  3. Last one is some bark from a forest walk. I jumped over a big, big ditch to get this. I’m pretty sure it’s beech (Fagus). My daughter jumped it too, so I had to save her afterwards. 94 g of bark.
Dagmar tæt på at falde i grøften
Dagmar, seen moping, came close to falling into a large ditch.

I used Jenny Dean’s general dyeing method for bark. She says that “barks are best soaked for several days or even weeks in cold water before processing. Then simmer them for one hour. Never boil bark, as this will release too much tannin”. So that’s what I did – left the three types of bark to soak for a couple of weeks. That was long enough that they started fermenting, and I can tell you that it didn’t smell that good.

But when I simmered 10 g test skeins of alum mordanted wools in the three bark dye baths, the color in the end was pale beige. I didn’t even bother taking pictures (because when you’ve seen one skein of pale beige wool, you really have seen them all), but you can see one sticking out between the pale pink skeins in the left side of the first picture above.

I have seen other dyers experiment with bark (for example, at my wool group’s dyeing day) and also get pale beige or off white. So right now, I’m not even convinced that it would ever work, and I probably won’t try it again unless someone can tell me what went wrong (please comment below if you know or if you’ve had good results dyeing with bark).

2: Slimy/Moldy Avocado Failures

There are established procedures for dyeing with avocados, but I’ve been experimenting with slightly different ways of doing it. I suppose to make the procedure easier and better, but of course ending up making it messy and complicated.

According to Carol Lee, avocado pits should not be allowed to dry before use because they will become so hard that they are impossible to chop. Instead, they should be frozen until use. I wanted to find a way to dry them anyway because my freezer is small.

So I chopped the pits and skins and then left them to dry. This worked well on a couple of occasions, but most times it did not because they became completely overgrown with mold before they had time to dry. Moldy materials may still work as dyes, but I think it is generally unwise to handle them repeatedly around the house, since many molds produce toxins that may be inhaled. So I went back to freezing the skins and pits.

dryavocado
Avocado pits and skin turn red as they dry, so it’s not that surprising that the dye bath they produce is also red.

Another experiment was to ferment the pits and shells for a looong time to see if they yielded more color that way. I used my dry material, soaked overnight, but I suspect the results would have been the same had I used frozen dyestuff.

I usually ferment avocado pits and skins by heating them up once in brine, then just leaving them. Normally for a few weeks or a month, this time for six months. And the dye bath did develop a deep red, but it also became extremely slimy.

Despite the sliminess, I tried dyeing a small test skein in this dye bath, but it didn’t yield good color. My guess is that the slime prevented good contact between yarn and dye. But I’m not convinced that a long fermentation couldn’t yield good color. I’ve been adviced to put avocado pits and skins in jars, close the jars, heat them up, and then ferment. Such jars should not go slimy. I’ll try that next time.

Beige med lidt rødlige striber
Beige with a red streak, that’s the look of yarn dyed with avocado slime.

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