Water Survey results pt 1

I’m not going to bury the lead on this one, now that I’ve taken my many many skeins of red yarn to show people at last weekend’s Kingdom A&S in Ealdormere, I’m happy sharing it with the blog world too. This is going to be a series of posts over the coming weeks. Starting with the pretty colours today, but then continuing into the water chemistry that affects the dye baths over further weeks. We started that last time with pH, but we’ll also touch on dissolved solids, iron and chlorinated water (and whatever else comes to mind as we go).

I detailed out the premise of the experiment in this blog post, but long story short; in late 2021, I had a hare brained scheme to request water samples from all over the kingdom (and beyond!) to do a selection of dye baths from to illustrate the variation that could be obtained while only changing one variable, the water. Note that photos do not do any of these colours justice, come see my samples at in person events!

Methodology

With 68 samples to work through, it was clear that a traditional ‘pot on the stove’ style of dyebath for each one was not at all going to be feasible. I have used a water bath method to do batch samples before and it is very effective.

For each water sample the pH, TDS and iron content was measured and noted down. The sample then had 600 ml measured into a clean (rinsed with distilled water) glass jar, if the sample contained less than 600 ml, it was topped up with distilled water to a total volume of 600 ml. Each of these jars had 3 g of madder powder added to them. The water bath was set up to hold 15 jars per batch, and the water temperature was held constant at 65C with a sous vide appliance. The dye liquor was brought up to temperature, and then held at 65C for two hours.

The yarn had been skeined off, weighed dry, mordanted in batches with alum at 10% wof and dried. Before dyeing, the skeins were soaked in distilled water to ensure they were fully wet.

After the dye liquor had steeped for two hours, the wet wool was added and stirred with a disposable bamboo skewer. The wool was held at temperature for an hour (stirred again at 30 minutes for Batch 2-6), and then was removed from the water bath after the hour had passed. The wool remained in the dye bath to cool naturally overnight. After 12 hours of cooling, the wool was removed to a drying rack to dry. The wool was left to dry for approximately 10 days before rinsing with distilled water and being left to dry again.

Everything was recorded in a giant spreadsheet that you are welcome to have a look at here.

Equipment

We had a quick look at the equipment that I used over in another blog post, go have a look there for all of my meters and strips and the like. The only addition to that list is my newest toy, a Color Muse colour meter. This little gadget is designed for interior designers to be able to match paint to fabric swatches, but also very helpfully provides a standardized reading of colour. The one that I’ve chosen to use is the CIE L*a*b* colourspace, which is specifically designed for comparisons. More on that in a future blog post, I have done little beyond take the readings at this point.

Results

The main form of showing my results is the photo at the top of this post. I embroidered a map of the relevant section of Ealdormere and then tied a loop of wool in the approximate location of its water. (Linen map, outlines in walnut dyed silk, compass point also in silk dyed with indigo, cochineal and mystery yellow.) The sample cards are a little bit easier to look things up and compare numbers and those are arranged by dye batch, shown below.

We’ve started talking about the water chemistry involved, looking at pH first in this post. We’ll move on in future posts to talk about total dissolved solids, iron levels, chlorine in city tap water and ultimately the results of the colour meter, but I’m aiming for this post not to turn into a thesis. When all is said and done, I’ll gather everything up into one document and stick it on my website such that people don’t have to scroll through blog posts to find the information. For the moment, however, stick around for the serialized version. Questions and comments are very welcome!

Let’s talk plants: Madder

I’ve talked about dyeing with madder more than a few times. I’ve written up documentation about some of my early madder experiments. I don’t think anyone would be surprised to know that I am really rather fond of playing with madder. So let’s do a little bit of a wander down the botanical path with the plant.

NB. I am a terrible gardener. I managed to kill a mint plant, that’s the level of terrible we are talking here. I do not grow my own. I let professionals (or awesome friends) do that for me and reap the bounty of their labours with gratitude (and/or payment.)

Franz Eugen Köhler, Köhler’s Medizinal-Pflanzen, Public domain, via Wikimedia Commons

Right, we’re talking about Madder. Most commonly, when the word madder is tossed around in the dye world, folks are meaning the dried and ground roots of Rubia tinctorum. Also referred to as common madder or European madder. It is, however, not the only madder plant out there that has dyestuff for us! It’s not even the only madder plant we can buy. The other one that’s easy to find at the dye supplier is Rubia cordifolia. Also referred to as Indian madder, or munjeet. But yet again that’s not the only other madder out there, there’s more! Wild madder, Rubia peregrina and Japanese madder, Rubia akane and there are others in the Rubia family.. but the first two are the most commonly used.

R. tinctorum is a perennial that was cultivated throughout Europe and the Middle East, with the highest quality coming from Turkey, Holland and France. It is native to western and central Asia and naturalized itself in central and southern Europe. Munjeet (R. cordifolia) comes from moutainous regions of Asia, from the Himalayas to Japan and also in tropical Africa. Wild madder (R. peregrina) is a native of Europe, Turkey and North Africa as well as the coastal regions of southern England and some bits of Wales and Ireland. The roots of wild madder are smaller than that of madder, requiring more dye stuff to gain a strong colour than one would require from madder, although that can be mitigated by waiting longer to harvest the wild madder roots (five years, rather than three for R. tinctorum)

Madder dyed wool

All of the various versions of madder have been used since antiquity, with evidence in extant items from Mohenjo-Daro in the Indus vally (approx 3000 BCE) and mentions in Pliny the Elder’s Naturalis Historia and recipes using madder are found in the Papyrus Graecus Holmiensis (approx 4th century) Assumptions about which madder was being used are usually based on geography. The East was more likely to be using R. cordifolia, the West more likely to be using R. tinctorum or R. peregrina. Local traditions using local plants, as the Rubia plant family is happy to grow in so very many different places.

All of them contain similar dye molecules, although different plant species have them in different combinations and concentrations. This chart from “The Colourful Past” by Judith H. Hofenk de Graaff is an excellent summary of who has what, with some extra plants that also contain anthraquinones.

Forgive me for being the kind of person who casually drops words like ‘anthraquinones’ in conversation, but in a nutshell.. those are the dye molecules that provide the red colour. For the curious, these are their structures (why this graphic is missing alizarin, I have no idea but it’s below):

Mohd Yusuf et al., “Eco-Dyeing of Wool Using Aqueous Extract of the Roots of Indian Madder (Rubia Cordifolia) as Natural Dye,” Journal of Natural Fibers 10 (March 13, 2013): 14–18.
George B. Kauffman, ed., Coordination Chemistry: A Century of Progress, vol. 565, ACS Symposium Series (Washington, DC: American Chemical Society, 1994), accessed February 18, 2021, https://pubs.acs.org/doi/book/10.1021/bk-1994-0565.

Phew, okay.. still with me after the brief foray into chemistry? (If you’re interested, the handout for my class on dye molecules can be found here. If you have a virtual event you’d like me to teach it at, just ping me.)

At the end of the day, if you have madder, munjeet or wild madder, you’re getting a dose of very similar dye molecules and just enjoy the ride. All of them function pretty similarly, and the reds are just so much fun to work with. I have an experiment in progress comparing R. tinctorum with R. cordifolia, through a collection of exhaust baths, so look for that coming soon!

Bibliography:

Hofenk de Graaff, Judith H., Wilma G. Th Roelofs, and Maarten R. van Bommel. The Colourful Past: Origins, Chemistry and Identification of Natural Dyestuffs. London: Archetype Publ, 2004.

Dean, Jenny. Wild Color: The Complete Guide to Making and Using Natural Dyes. Rev. and Updated ed., 1st rev. U.S. ed. New York: Watson-Guptill, 2010.

Cannon, John, and Gretel Dalby-Quenet, eds. Dye Plants and Dyeing. Repr. London: Black, 2002.

Yusuf, Mohd, Mohammad Shahid, Shafat Khan, Mohd Khan, Shahid Salam, Faqeer Mohammad, and Mohd Khan. “Eco-Dyeing of Wool Using Aqueous Extract of the Roots of Indian Madder (Rubia Cordifolia) as Natural Dye.” Journal of Natural Fibers 10 (March 13, 2013): 14–18. https://doi.org/10.1080/15440478.2012.738026.

Kauffman, George B., ed. Coordination Chemistry: A Century of Progress. Vol. 565. ACS Symposium Series. Washington, DC: American Chemical Society, 1994. https://doi.org/10.1021/bk-1994-0565.

Water, water, everywhere!

My first major project for 2022 is one that I’ve wanted to do for a long while, and I’m getting a whole lot of help with. How big of a difference does water source really make in one’s dye projects? Well! I decided to experiment with that premise, and asked people to share a water sample from their house. (And barns, streams, lakes..) My reenactment group is very generous and now I have water samples from all over the province, and beyond! 60 samples! I was hoping there’d be 20 or so, I certainly have my work cut out for me.

A messy studio made messier by a lot of bottles of water.

The basic experimental premise is very simple. Keep all the other variables steady (or known at least) and have the water as the main variable. Measure as much as I can about each water sample, to have some idea on what it contains, but then keep the dyestuff, the method, the fibre, the mordanting.. all of that to be the same so that differences can be safely assumed to be because of the water.

Which dyestuff to choose was an easy one. Madder is delightfully reactive to changes in water hardness, and pH and generally is a bit of a fussy goose, so it’s perfect for this. I got a nice big container of R. tinctorium, so that all 60 samples can be taken from the same batch of powder. Natural dyes are variable in and of themselves, from one batch to the next. The growing conditions, the soil, how the plant was handled and the dyestuff extracted all can affect the dye that I’ll be using, so at the very least, this one container should be relatively homogenous, even if multiple batches of madder went into it.

Fibre was also a no brainer choice. I’ve worked up small skeins of 100% wool yarn, all of which has been mordanted at 10% wof with alum. Basic, easy, nothing fancy going on here. Wool and alum. Done and done. The skeins aren’t quite perfectly consistent, they range from about 5 and a half grams to about 7 and a half grams, but I’m willing to be ‘close enough’ on that one.

Grocery bins are eternally handy.

I’ve had very good luck with using a water bath to keep my temperatures very consistent, as of course madder is also sensitive to what temperature it’s dyed at. Basically a large tub of water is heated with an immersion heater (sous vide gadget, I do love you and not just for steaks), and each dye bath lives in its own glass jar within that tub of water. I used this method for one of my earlier madder experiments and it worked a treat. I will have to work in batches, as I can’t fit all 60 at once, but good technique should keep that variable to a minimum.

Then it comes to the water itself, and there’s lots of it. The plan is to grab the pH, the iron content and a general measure of hardness (Total Dissolved Solids) from each sample. This should give me a moderately good idea on what’s going on in the water itself. I will admit freely that it is not ideal that the water has now sat for a good six weeks before I’ve gotten to working with it. (Thank you holidays and general life challenges.) Stale water means that I’ve lost most of the volatile compounds that would have been in it, and any that were treated with chlorine (rather than chloramine), that’s absolutely gone. Some of the unfiltered water has sediment that has settled out while it’s sat, and while I do plan to give each a shake before I measure it, it’s not quite the same as fresh. Still, this is what I have, and the reality of collection means that there was always going to be some sitting time before I used it. So be it, we’ll manage.

So expect more on this project in the hopefully near future! I think I have all of the pieces in place now, so it’s just a question of getting to the doing part.

Alum experiment

The lovely folks over at Natural Dye Education FB group, mostly the group’s fearless leader from Mamie’s Schoolhouse, put forth a challenge after watching a talk at the Natural Dye conference in 2020/2021 about alum not being absorbed out of the water quite as much as we think, and so clearly we had to try it. If you want to read about the results from the whole group, she has a collective blog post about it.

The premise was to use 7 identical skeins of wool, and one pot of mordant water. That water held 7% wof (weight of dry fibre) of but a single skein. So the first skein of wool into the mordant bath got a full dose of alum. Then, without topping up any alum in that pot, the next six were mordanted (and labelled!) in succession. So, in theory, we would have no alum left.. somewhere in that chain. All 7 then went into a dyepot, all at the same time, such that they would get the same dye exposure and show up where the alum stopped. So the theory went. It was left up to the dyer on what dye they wanted to use, but alum and wool were consistent for all of us.

This is not spaghetti.

I used madder (because of course I did), and had dug up some bulky weight wool yarn out of the depths of the stash, each 55g. (Except for the 2 that I mismeasured and ended up 65g. whoops.) So because my skeins were (mostly) 55g, a mere 3.85g of alum went into that giant pot of water. I kept each skein at a simmer for about an hour, and then hauled it out hot and let it cool, unrinsed. Eventually there was a giant pile of damp wool.

Cleaned out pot and and fresh water and in went 100g of madder. I had a grand plan of containing it in a little cloth bag so I didn’t have to rinse out madder dust for days, but my bag wasn’t big enough once the madder started expanding on getting wet, so that was abandoned early and I resigned myself to a million rinses later. (Dear Future Me: When you do this again, let the skeins dry after you pull them out and then whap them on the deck railing a whole lot to get most of the madder out that way. You’ll be much happier, you’re welcome.) That sat on the stove at not quite a simmer, about 70 – 80C for a couple of hours.

Top: Most Alum Bottom: Least Alum (plus bonus silk skein)

In goes all 7 skeins at once, and those got to sit around at not quite a simmer (80 – 90C) for another couple of hours before the heat got turned off and everyone went to bed. The skeins in the dyepot, and me.. well.. in bed. Next morning, rinse (and rinse and rinse and rinse and rinse) and plot what else is going in that pot of still dark red dye liquour. The exciting thing here is that in spite of there being successively less and less alum on these skeins, my 7 skeins are functionally identical. Now, madder is a dye that will take without a mordant, but not usually quite this dark and strong, so clearly more experimenting is required. (Oh /darn/, I’ll have to do more dye work. Such a tragedy. 😉 )

Well! I have more of that stash wool, so I grabbed another 600g of it, got that mordanted up (10% ish) and in it went to the same dye bath as the last batch. The madder bath was on a roll! The first 300g were still pretty solid colours, but by the last 300g I was getting pretty pale pinks and I was not in the mood to slowly simmer it down enough to bother storing it, so I called it there. Currently the big bulky wool is telling me it would like to be a stripy big thick sweater, but we’ll see how long that lasts. I’m not very good at using up the bulky yarn in my life, although I better start using up more of my dyed yarn, or I’ll be overrun!

Exhaust baths