Table of Contents
Shibori is an overarching Japanese word for various methods of resist dyeing; there is no English equivalent.
Resist dyeing is a technique for dyeing fabric with designs or patterns that is common through many cultures across the world – there’s the western tie-dye made popular in 1960s USA, batik in many African and Asian cultures, and screen printing, among others. The basic premise in all of the different types of resist dyeing is that there are many ways to ‘block off’ parts of the cloth in order to keep it from taking up the colour of the dye (in other words – sections of the cloth resist the dye).
It is believed that the different resist dyed methods made their way to Japan from China prior to the 700s CE – the earliest extant examples of resist-dyed fabric were included in an inventory of gifts made in 756 CE to the Hōryū-ji temple (Wada p. 11).
Since then the numerous techniques have become staples of the traditional art of Japan, and while they all have their own names, they are also all encompassed under the singular term: shibori.
Below is a video on shibori methods. Apologies, but due to technical issues with one of the clips there is no footage of stitched shibori. However, two fantastic resources are listed in my citations section should you be interested.
Wax, or paste, resist dyeing is very common around the world – known specifically as batik in Indonesia, Malaysia, and India among other places – and is where wax or a paste is applied to the cloth in order to keep dye from reaching those sections. Once the fabric is dyed, the wax/paste can be washed away, and the process repeated if desired. This can be used in conjunction with stencils to create more complicated designs, or with stamps to cover large areas more effectively. Certain patterns can dictate what area the batik is from, or what the fabric’s purpose is and some patterns are reserved for very specific occasions.
Ikat (known as kasuri in Japan), is the process of employing resist dyeing on the yarn before it is dyed and subsequently woven into fabric. It is common in several cultures around the world, including many places in Asia, Africa, and South/Central America.
Ikat dyed fabric is characteristically ‘blurry’ since the design is developed when dyeing the yarn and then the weavers have the challenge of matching up the yarn on the loom in order to produce the pattern through the weave. Double ikat is when both the warp and the weft are resist dyed to produce a design and is incredibly challenging for all the artists involved.
The best way to see how ikat is done is by watching it. The following video was recorded over three months and then time lapsed, but it shows the entire process, from warping to weaving. The artist chose to paint the dye on, which is not the traditional method, but still works.
Arashi shibori was developed in the 1880s and therefore isn’t within the SCA period; however, it is my favourite method as the patterns are gorgeous. There are other forms of shibori that use a pole to protect parts of the fabric from the dye, and while they all have specific names, they can, along with arashi, be generally called bōmaki (literally pole-wound).
The word arashi can be translated as storm and the resulting patterns reflect that.
Fabric is folded (if needed) and draped around a pole (any sort works, PVC is common in North America). Thread is then wound around and the fabric is compressed tightly together. (Photo credit Liz Kelly, retrieved from https://commonfold.wordpress.com/2013/08/08/arashi/)
While artists are able to incorporate their own creativity, there are a few specific things to note:
- The fabric should not overlap when wrapped, but can be wrapped straight onto the pole or at a diagonal to spiral around the pole
- Fewer folds/thinner fabric tends to work better both with how it allows the dye to permeate and how easy it is to compress
- The dye vat you are using must be able to reach the top of the fabric once its compressed onto the pole, unless you are specifically looking for an uneven dye or to dye the fabric multiple colours.
Once dyed and dried, you can remove the fabric from the pole and open it to see the pattern. The fabric should then be rinsed and hung to dry before it’s done. (Image retrieved from http://momijistudio.blogspot.com/2014/05/arashi-shibori.html)
The final goal of this research and my research into indigo dye is to craft a Japanese kosode in a period style. Even though my persona isn’t Japanese, I felt as though this was a good project to show both of these areas of interest.
A kosode is a simple Japanese garment that was originally an undergarment and eventually evolved into the modern kimono. The word translates to “small sleeve” and refers to the small opening of the sleeve, different from the big, open sleeves of the layers that were worn over it in the Heian period (794-1172 CE).
- White silk fabric – woven in a more traditional loom width of 14.5″
- White silk single ply thread – white because I plan on dyeing it as well to hand sew the final result
My source for figuring out a kosode pattern is the website of an SCA Laurel – Saionji no Hana – at wodefordhall.com, as she has done an immense amount of research into SCA period Japanese garments and has presented the information in an easy-to-understand way. I am well aware that I have a lot more to learn and research regarding kosode construction specifically; however, for the moment it is mostly a vehicle for the rest of my research into shibori and indigo dye.
Since I knew I wanted to use particular shibori techniques and dye the fabric, I chose to measure and cut the fabric first to make sure I had all of the pieces and could see how they would work together so that I could plan my pattern.
I followed the website’s instructions to figure out my base panel width, which turned out to be 14″ – just shy of the width of the fabric I wanted to use, which mostly means that my seam allowances will be fairly narrow. However, since I’m planning on hand sewing the final result, hopefully it won’t be much of an issue. That base panel width allowed me to figure out and cut the rest of the fabric I required. (Image taken from wodefordhall.com)
In addition, as I am not particularly Japanese-sized, it is likely that the final product will not fit me precisely – however, I am limited in the amount of fabric I have.
Before cutting my silk, I did a mock up in 15″ kimono cotton purchased from Maiwa in order to make sure I understood how the pieces went together and to see whether my base panel width would work for my body type. I plan to use that mock up as a test for the rest of the project up to, and including, sewing it together.
For a full garment, I wanted to choose a technique that was historical, able to be documented, and quick to learn, even if it would take practice to perfect. In researching shibori techniques and history, I found that bound shibori – specifically ne-maki or base-wound shibori – is one of the oldest techniques, is pictured in a fan sutra painting from twelfth century Japan, and, while repetitive, is not as simple as it looks.
This technique ends up as a white ring on indigo cloth and is made by wrapping the thread tightly around a portion of cloth several times, keeping the thread tight and close together. The thread is tied off with a kamosage knot (a friction knot), and the next portion of fabric is drawn up, so that as much as is possible the thread remains unbroken and travels from point to point. This allows for a finishing technique at the end where the fabric is simply tugged and all of the knots come loose and free the cloth. (Image taken from Wada p. 56).
Wada, Yoshiko Iwamoto, Mary Kellogg Rice, and Jane Barton. Shibori: the Inventive Art of Japanese Shaped Resist Dyeing: Tradition, Techniques, Innovation. New York, NY: Kodansha USA, 2011.
Callender, Jane. Stitched Shibori: Technique, Innovation, Pattern, Design. Tunbridge Wells, Kent: Search Press, 2017.
Below is a project I completed a couple years ago about indigo dye. It’s interesting to see how I’ve progressed in building indigo dye vats over time.
A Comparison of Indigo Dye Vats
Indigo blue is one of the most challenging and, in my opinion, rewarding, colours to dye. Not only is the historical method of making this dye difficult, but the chemistry behind the indigo plant is a fascinating look into the mystery of nature and the creativity of humanity.
While my original vision was to complete several dye vats using both indigo powder and indigo plant matter, due to some hiccoughs with growing my own plants I was forced to scale back the project and focus on comparing a modern chemical vat with a historical fermentation vat. This still provided a worthy challenge and plenty of opportunity for experimentation with different fiber types. You can find the full, unedited version of my documentation at the end of the section.
Indigofera Tinctoria (True Indigo)
Found originally in India, Indigofera tinctoria prefers tropical climates and can also be found in China, Indonesia, and parts of Northern South America. (Image from Wild Colour by Jenny Dean (1999)).
Early English buyers focused their attention on western Indian (Gujarat mainly), which Marco Polo described in his Travels:
They have also abundance of very fine indigo. This is made of a certain herb which is gathered, and [after the roots have been removed] is put into great vessels upon which they pour water and then leave it till the whole of the plant is decomposed. They then put this liquid in the sun, which is tremendously hot there, so that it boils and coagulates, and becomes such as we see it. [They then divide it into pieces of four ounces each, and in that form it is exported to our parts.]Marco Polo, The Book of Ser Marco Polo, the Venetian, concerning the Kingdoms and Marvels of the East, trans. Henry Yule, vol. 2 (London: John Murray, 1871), 312.
Due to the fact that the indigo pre-cursor, indican, is contained solely in the leaf of the plant, and that only a small amount is obtained from each leaf, the processing and making of indigo dye was one of the most expensive form of dyeing in the medieval world.
I attempted to grow and harvest my own Indigofera tinctoria, but despite several different seed batches from several different suppliers, it refused to even sprout. Perhaps I overwatered it, or the soil was unfavourable. Either way I was unable to obtain a crop this year. Next year I will try to sprout the seeds first in wet paper towel before planting.
Persicaria Tinctoria (Japanese Indigo)
Also known as Polygonum tinctoria, dyer’s knotweed, or tadeai, this variety of indigo is common in Eastern Europe and Asia, particularly the Tokushima prefecture of Japan, where there are still studios that dye using historical methods. The plant matter can be used fresh, dried, or fermented and made into sukumo or aidama to be used at a later date.
I was more successful in my attempts to grow Persicaria tinctoria than Indigofera tinctoria, as the plant seems to be more forgiving, but still require more leaf production in the future to attempt a dye-vat made solely of plant matter. From what I was able to harvest this year, I have begun the process to make sukumo on a very small scale.
Isatis Tinctoria (Woad)
Woad is what was common in Europe before the Europeans discovered Indigofera tinctoria. However, even though it finds the growing conditions in Europe more favourable than true indigo, Isatis tinctoria contains the indigo pre-cursor isatan B as opposed to indican and in much weaker concentrations. It was a common cosmetic, particularly for the Celts and was used as a textile dye by the Anglo-Saxons and Vikings.
I did not attempt to grow my own crop of woad at this time, as I was more focused on true and Japanese indigo, but it would make for an interesting comparison in the future.
Indican is found in many other plants, such as Indigofera suffruticosa, common in the tropical and subtropical areas of the Americas from the southern United States all the way down to Argentina. There is also Indigofera bracteolata from West Africa, Marsdenia tinctoria which is common in subtropical regions like Nepal, Thailand, Burma, and Indonesia, or the other varieties in Japan such as Mercurialis leiocarpa and Strobilanthes cusia. Finally, there is the synthetic indigo that was developed in 1897 and is still produced and used today.
Indigo Dyeing Methods
According to a blog post by Maiwa Handprints Ltd., there are three things you need for an indigo vat: indigo, a base, and a reducing agent. The indigo can come from either the living/actual plant or as a powdered extract. However, in order to utilize the indigo properly, since it is not water-soluble, there needs to be a reducing agent that diminishes the oxygen in the solution, which thereby encourages the indigo to dissolve. A base turns the solution alkaline (as opposed to acidic) and allows the reducing agent to work.
A fermentation vat is an older form of indigo vat in which the “dye-stuff was made soluble in water with the help of micro-organisms [sic] and alkaline substances…[t]he bacteria, whose metabolism produced the required reduction, were often assisted with some food-stuff that enhanced their effect, such as sugar, honey, molasses, etc.” When using fresh or dried indigo leaves, the leaves themselves contain sugar, though more is often added to promote the fermentation (however, if you add too much you risk the fermentation getting out of hand). When dyeing from an indigo powder, the fermentation can come from a variety of sources including: fruit, madder, or even stale urine. In order for the fermentation to work, it needs to be kept at a consistent temperature of about 40° C. This keeps the microorganisms alive and working to reduce the oxygen within the vat.
A historically very common form of fermentation vat was the urine vat. It has been in use for thousands of years and even Pliny the Elder describes dyeing fabric Tyrian purple in much the same way, as “the liquid is mixed with water and human urine in equal parts, one-half only of the proportion of dye being used for the same quantity of wool.” Urine has a tendency to be acidic (with a Ph of around 6), but can be alkaline if the proper foods have been eaten. When urine is allowed to stand for some time, it develops the micro-organisms whose “metabolism produces the ammonia which is a necessary reducing-agent.” This does take some time, and some recipes for an indigo vat will specify that the urine must be quite old. In later works, even more specifications were noted, such as that the urine must come from men, or as in Cajsa Warg’s work in 1762 which states to “take urine, preferably of those who drink strong drinks.” However, the pros of this type of vat (simple ingredients that are easy to collect), may be outweighed by the cons (smell, and the need to collect urine and keep it for up to several months), depending on the individual. I, personally, chose a different method of fermentation.
There are several opportunities to use modern substitutions in the pursuit of an indigo vat if a pure fermentation bath proves too time-consuming or finicky to work with. For the most part, these are chemicals that have been discovered to work as a base or a reducing agent that are not found in nature or were not used historically. These are compounds such as sodium dithionite or thiourea dioxide, both effective reducing agents, or calcium hydroxide (calx) which is used as a base.
It is also helpful to test the alkalinity of the solution with a digital Ph reader to make sure your vat is on the correct path. Historically, the alkalinity could have been tested by feel, as the more alkaline a solution, the more ‘slippery’ it feels.
Modern Dye Vat
For the first dyebath, I chose to replicate a more modern, chemical vat, while still using natural indigo powder. For the recipe, I followed the one provided by Maiwa, from whom I purchased the indigo powder. The base is calx (calcium hydroxide) and the reducing agent is thiourea dioxide.
- Calx (calcium hydroxide)
- Thiourea Dioxide
- Indigo Powder
- Rainwater/Distilled water
First the fibers must be scoured to remove any grease, wax, pectic substances or oil. This will help the dye to infuse the fiber evenly. For wool and silk (protein fibers) you can use a gentle soap in warm water, leaving it overnight, and being careful not to agitate the wool so much that it felts. For linen and cotton (cellulose fibers) this is best done with a pot of hot (simmering) water and washing soda, agitated gently and left for at least an hour. The water will turn a yellow-brown, and you can repeat this process as many times as you feel is necessary or until the water remains clear. I only needed to scour the cotton and linen, as the wool and silk I had were sold ‘ready for dyeing.’ When the vat was ready, the fibers were put in already damp to provide consistency.
Next, Maiwa recommends mixing a stock solution:
- Fill a quart size wide mouth mason jar with hot water. Dissolve 1 to 1.5 teaspoons of lye.
- Add 2 – 4 teaspoons finely ground natural indigo and stir for 2 minutes.
- Add 1 teaspoon of thiourea dioxide or 2 teaspoons of sodium hydrosulfite and stir for about a minute.
If reduction of the indigo starts properly, the colour of the surface of the liquid should change to a purplish violet with at coppery sheen. Place a lid on the jar and set aside in a warm room (or place in a pan of warm water) for about 60 minutes. The solution will change from an opaque blue to a translucent brown-yellow as it reduces. Check the stock solution to see if it is ready by dribbling some solution on the side of a white cup. Note the change from clear yellow to opaque blue as the indigo is reintroduced to the oxygen in the air. At this point the stock solution may be used or kept up to a week. If kept longer the solution may need to be revived. Heat gently to about 50°C (120°F) and add some more reducing agent (thiourea or hydrosulfite) and stir well.
Then it’s time to prepare the vat itself:
- Put 5 gallons of hot water 110-140°F (45 – 60°C), in a plastic pail or garbage can.
- Add 1/8 teaspoon of lye into the water and stir until dissolved. This makes the vat slightly alkaline so that the reduced indigo from the stock solution does not re oxidize when added.
- Add 1/2 teaspoon of detergent. This will help the indigo penetrate the fiber and will break up oxidized indigo on the surface of the vat.
- Add 1 teaspoon of thiourea dioxide or 2 teaspoons of sodium hydrosulfite and stir gently until dissolved. Cover the vat and allow it to reduce for about 15 minutes. 5. Carefully lower the jar of stock solution into the vat and pour out the contents (avoid pouring from above as this adds oxygen). Use all the stock solution for cotton or half for the same weight of wool. 6. Stir gently and allow 30-60 minutes for the vat to turn yellowish green.
Finally, the scoured fibers can be added to the dyebath. They will be submerged and agitated slightly in order to facilitate dyeing as evenly as possible. Then the fiber is left for an amount of time, in this case I opted to let the fiber dye for 10 minutes. For a much lighter shade, the dyeing time can be drastically reduced, with an immediate rinse upon removing the fiber from the dyebath.
The product is then removed from the dyebath carefully, in order to prevent oxidizing the bath more than necessary, and any excess liquid is squeezed out (preferably while still submerged). The fibers are allowed to oxidize for 30 minutes and can be dyed again if required. The only fiber I put into the vat for a second time was the cotton, as it required more time and more dye to reach a shade similar to the wool, silk, and linen.
When the dyeing process is finished, the product is left to oxidize and dry for 24 hours. If a darker shade is desired, the process may be repeated (without the need to scour the fibers again) as many times as necessary. Once happy with the results, the fibers are washed and rinsed.
The main challenge with a chemical indigo vat is the proportions. By following a recipe developed by experts in the field, I was able to easily create the conditions needed for the indigo to work properly, but to guess at the proportions would be difficult. Once the vat was showing the ideal conditions, it was easier to adjust it to maintain those conditions. It was also difficult to start from a stock solution and transfer to a vat, as I was working in a space that was smaller than I would have liked
The dyed fibers were all very consistent in colour, and brighter than I anticipated, though the cotton needed a second dye to reach that same level.
Historical Dye Vat
For the second dyebath, I chose to attempt a fermentation vat made with natural indigo powder. For the base, I used soda ash; for the reducing agent, I used a combination of madder and wheat bran; and I made sure to use collected rainwater, topped up with distilled water when I needed more.
- Wheat Bran
- Soda Ash
- Indigo Powder
- Rainwater/Distilled water
For this vat, I applied a slightly less scientific, but a more historically accurate method. Instead of following an exact recipe, I used a recipe as more of a guideline and as a place to start, adding more ingredients as required. Fermentation vats are, by their very nature, fluid and difficult to maintain and therefore a recipe cannot be considered a way to achieve a perfect vat each and every time. As such, I am unsure of exactly how much of each ingredient I used in the end.
First the fibers (cotton and linen) were scoured as per the method in Dye Vat One. The wool and silk were purchased ready for dyeing and did not need to be scoured. Again, the fibers were damp when they were added to the vat.
Then I followed a recipe from Sandberg’s Indigo Textiles that appears to be a translation from a book from 1759:
– with which you can dye blue
wool, linen and cotton
from: An honest and reliable dye-book 1759
Take a wooden vessel large enough for 8 jugs of water; then take a copper-kettle, into this pour 7 jugs of water and 8 weights of coarse madder, a stoup of bran, 1 pound of grey potash, allow the kettle to come to a boil and let it boil for a quarter of an hour, then pour it into the firkin in which the dye shall be, lay something over it so that it keeps warm; take 4 weights of Indigo in a small pot with a quarter of a gallon of water, 4 weights of potash, allow it to boil for half an hour, while it is boiling pound gently on the bottom of the pan with a pestle so that the indigo becomes as fine as powder, when it is boiled, take the pan off the fire and allow it to cool somewhat, and also pound evenly so that the indigo becomes truly small, then pour from the firkin what is clear and with the pestle pound the thickness on the bottom of the pan until it becomes quite fine: then pour all into the firkin and rinse the pan clean, and stir well the content of the firkin and allow it to stand 12 hours, then stir again, and so continue until 24 hours have passed, then the dye is ready to dye.
NB All woollen yarn that is to be dyed blue must first be washed in warm water and dyed wet. But linen yarn is dyed dry. All cotton yarn is boiled for half an hour in pure water and dyed wet.
1 jug = 2.6 litres
1 weight = 13.3 g
1 stoup = 1.3 litres
1 pound = 425 g
1 bucket = 49 litres
I used that recipe in conjunction with the following, similar one from a website that allowed me to substitute some of the ingredients and measurements:
- 4 oz. ground Indigo
- 2 oz. ground Madder
- 2 oz. wheat bran (buy at any health food store)
- 12 oz. washing soda (“soda ash”)
Combine these ingredients in about a three gallon pot of warm water. Always add these amounts in proportion. A larger vat can be made, for example with: 1 lb. ground indigo, 1/2 lb ground madder, 1/2 lb ground bran and 3 lbs washing soda in about a 10 gallon plastic tub. However, I advise starting small, till you are comfortable with the process. The size of the pot is determined by the amount of fibre you need to dye at one time. A three gallon pot is good for yarn skeins of 4 to 6 oz., while a 10 gallon or larger tub will be needed for yards of fabric.
WARMTH: It is necessary to keep the vat warm, but not hot, around 100 – 110° Fahrenheit. It is the same temperature for raising bread or making yogurt. It should feel pleasantly warm to the hand.
To keep it warm, a light bulb in a reflector can be put under the vat, with a blanket over it to keep in the heat. (See illustration, next page.) In a warm climate no additional heat is needed, but be sure the vat is out of direct sun so it does not overheat.
TIME is very important. It takes time for the vat to ferment and it does no good to try to rush the process. The first time, it takes about a week for the vat to ferment and be ready to dye. With “renewals” the time needed is a bit less, four or five days.
In the end, my measurements were likely not the same as stated here. I started with the ingredients and measurements in the second recipe (as I was working on a smaller scale), and then tested the Ph of the solution and adjusted as necessary. Once the indigo was added, it became easy to tell whether the vat was ready simply by immersing something (a length of yarn, or a finger) to see if the dye would stick to it. This particular vat never attained the look of the chemical vat, but it seemed to work fine all the same.
Once the vat was set, I dyed each of the fibers for approximately 10 minutes, same as with the chemical vat, and then I let them oxidize. The cotton, again, was the only fiber that needed a second 10 minutes in the vat to obtain the same colouring. They were then left to dry.
There were several challenges with the fermentation vat – namely, getting the fermentation started. As I live alone and did not wish to risk burning my house down, I was unable to maintain a situation where the vat could remain at a high enough temperature to keep the fermentation process active, despite trying many different methods. As such, I did end up needing to jump-start the fermentation by adding a small amount of a chemical reducing agent (thiourea dioxide). This quickly set the vat in order and allowed me to proceed with dyeing the fiber.
The results of this vat were interesting. The colour was a much darker and duller blue than the chemical vat, possibly due to the addition of madder as a fermentation agent. Since the madder did not ferment as anticipated, it may be that the colour dissolved in the water and mixed with the indigo to obtain this different shade. In addition, when the yarn was withdrawn from the dyebath, it oxidized much faster than the indigo from the chemical vat. The final interesting difference was that the fermentation vat never took on the coppery sheen like it was ‘supposed’ to, yet it dyed perfectly well.
Indigo is complicated. From the basic chemistry behind indigo’s behaviour, to the intricacies of a fermentation vat, that is the crux of what I learned with this experiment: indigo is complicated. By comparing and contrasting two different indigo vats over four different types of fiber, we can see that there is quite a difference between a modern chemical vat and a (mostly) historical fermentation vat, not only in the results that were produced, but in how the vat behaved. Granted, some of those inconsistencies can be explained by a modern inability to perfectly recreate a medieval setting, but you would still expect some similarities in how the vats functioned.
In the future, I would also like to experiment with vats made with fresh or dried plant matter from the indigo-producing plants, or even to include woad as a contrast to the true indigo I used here. The foundation for obtaining indigo straight from the plant matter is the same as from indigo powder, but it would be interesting to see if and how the results are different.
 Gösta Sandberg, Indigo Textiles Technique and History (Asheville, NC: Lark Books, 1989), 19.
 Ibid. 22.
 Leggett, 19.
 John Marshall, Singing the Blues (Covelo, CA: Saint Titus Press, 2018), 12.
 In Japanese – Ibid.
 Ibid. 9.
 Ibid. 9 – the moist version of aidama.
 Marshall, 9. – dried cake made from composted material.
 Indigo and Woad, PDF, Vancouver: Maiwa Handprints.
 A body of a Celtic chieftain was discovered to have preserved tattooed skin and dates to approximately 500 BCE – John Edmonds, The History of Woad and the Medieval Woad Vat(Little Chalfont: J. Edmonds, 2006), 12.
 Ibid. 14.
 Marshall, 11.
 Ibid. 12.
 Ibid. 13.
 The natural dyes store in Granville Island, Vancouver BC, considered experts in the field.
 “Natural Dyes – About The Organic Indigo Vat,” The MAIWA BLOG, accessed September 06, 2018, http://maiwahandprints.blogspot.com/2013/08/natural-dyes-about-organic-indigo-vat.html.
 For a more in-depth discussion of the chemistry behind indigo vat dyeing, see Appendix A.
 Sandberg, 40.
 Pliny the Elder, Natural History, Book 9, Chapter 64.
 Sandberg, 139.
 Rosetti (1548) Plictho – Recipe 43 reads (English translation): “The more the urine is old, the better.”
 Sandberg, 139.
 English translation from Sandberg, 171.
 Due to the fact that bases react with the fatty acids in your skin – this is how soap is made (“The Observable Properties of Acids and Bases,” ChemTeam, accessed September 06, 2018, https://www.chemteam.info/AcidBase/Acid-Base-Properties.html.).
 The following instructions are from Indigo and Woad, PDF, Vancouver: Maiwa Handprints.
 Sandberg, 170.
 “Indigo Natural Fermentation Vat,” Aurora Silk, accessed September 10, 2018, http://www.aurorasilk.com/tutorials/how_to_natural_indigo_dye_vat.html.
The Chemistry of Indigo
While indigo’s chemistry is known and utilized today, it is unknown whether dyers in pre-17th century Europe and Asia knew exactly why indigo acted the way it does. It is more likely they learned how a dye vat was ‘supposed’ to look, feel, or smell, passing traditions down for hundreds of years after many trials and mistakes were made. However, as the science behind it is fascinating, and explains why dyeing with indigo can be difficult, I opted to include it here.
Indigo begins as a molecule known as ‘indican’ (in Indigofera tinctoria and Persicaria tinctoria, but the indigo precursor in woad is isatan B); however, it is actually the molecule ‘indoxyl’ that is able to penetrate the fiber within the indigo vat. When the indoxyl is exposed to oxygen outside of the vat, whether or not it is attached to a fiber, it forms bonds and becomes indigo.
Below are the skeletal formulae of these molecules. Skeletal formulae are common in organic chemistry and look quite bare as they simply show the carbon ‘skeleton’ without the requisite hydrogen atoms attached. However, they enable us to briefly glance at multiple molecular structures and see how they are similar. I have also included each molecule’s molecular structure.
Indican (C14H17NO6) is what is called a glucoside, or a glucose molecule that is bound to another molecule, in this case, indoxyl.
Isatan B (C14H15NO6) is also a glucoside, just with a slightly different molecular composition. It has the exact same indoxyl molecule attached to a different sugar molecule.
When starting with fresh indigo or woad leaves, obtaining indoxyl is easy: just remove the glucose molecule. This is done through a process called hydrolysis, and can be done naturally or chemically. While there are a variety of ways to achieve this chemically, it can be done organically in a fermentation vat, where the yeasts from the fermentation will eat the sugar molecules, leaving behind the indoxyl dissolved in water. Then the indoxyl can be used to dye fibers or precipitated out to form powdered indigo.
Once indigo is in its powdered form, it is stable and can be traded or shipped, but it is no longer water-soluble. The indigo must be converted back into a water-soluble form in order to use it as a dye.
This is where the dyeing process can get tricky. In order to achieve this reduction, an alkaline vat and a reducing agent are needed. The reducing agent provides electrons that are able to bond with the excess oxygen to form alcohols, which are water-soluble. This also leads to an excess of hydrogen ions. When there is an excess of these ions in a solution, that solution is said to be acidic. By providing an alkaline solution to begin with, one that has an excess of OH ions, the solution will balance out through the production of sodium salts and water.
For example (using urine):
(12 C16H10N2O2(s) + (C6H12O6(aq)) + 9H2O(l) + (CH4N2O(aq)) = (12 C16H10N2(OH)2(aq)) + (7 CO2(g)) + (2 NH4+) + (2 OH–)
Indigo (solid), plus glucose (aqueous), plus water (liquid), plus urea (aqueous) equals leuco-indigo (aqueous) plus carbon dioxide (gas) plus ammonium hydroxide (the NH4+ + OH–)
To break it down into its component parts:
C6H12O6(aq) + 6 H2O(l) = 6 CO2(g) + 24 H+ + 24 e–
Glucose is oxidized into carbon dioxide and hydrogen ions with free electrons
12 C16H10N2O2(s) + 2 H+ + 2 e– = 12 C16H10N2(OH)2(aq)
Indigo takes some of those hydrogen ions and free electrons and becomes leuco-indigo
CH4N2O(aq) + H2O(l) = CO2(g) + 2 NH3(g)
Urea plus water is converted by the bacteria into carbon dioxide and ammonia
2 NH3(g) + 2 H2O(l) = 2 NH4+(aq) + 2 OH–(aq)
Ammonia is soluble in water and deprotonates a small amount of the water to obtain ammonium and hydroxide
While the above equation is balanced, it is not perfect, as the amount of ammonia that converts into ammonium (NH4+) and hydroxide (OH–) depends on the Ph of the solution, which is also dependent on how much ammonium (acidic) versus hydroxide (alkaline) there is. If another alkaline ingredient, such as sodium hydroxide or washing soda, were used, the by-products of that reaction would be different. Not only that, but fermentation itself can create by-products that alter the equation. So this particular version is not as important as the basic idea behind the equation: that combining these ingredients causes a chemical reaction to occur, and that due to this reaction, hydroxide and hydrogen ions will form and solid indigo will be changed to leuco-indigo.
Eventually, the reducing agent gets used up and the sugar gets turned into an acid, therefore no longer reducing the oxygen in the vat and changing the overall Ph back towards neutral and halting the fermentation. This is part of why it is so difficult and exacting to create and maintain a fermentation indigo vat, and why it is so impressive that peoples from pre-17th century societies figured it out. Everything needs to remain in balance so that the correct chemical reactions can occur.
 “Indigo: Recreating Pharaoh’s Dye,” Science in School, accessed September 06, 2018, https://www.scienceinschool.org/2012/issue24/indigo.
 Glucosides are subsets of glycosides. A glycoside is a molecule in which a sugar is bound to another functional group via a glycosidic bond. A glucoside is when that sugar is specifically glucose.
 K. G. Gilbert et al., “Qualitative Analysis of Indigo Precursors from Woad by HPLC and HPLC-MS,” Phytochemical Analysis 11, no. 1 (2000): 18, doi:10.1002/(sici)1099-1565(200001/02)11:13.0.co;2-x.
 The chemical breakdown of a compound due to reaction with water.
 To create a solid from a solution.
 “Indigo-a-go-go: Better Dyeing through Chemistry,” Sheep Cabana, accessed September 06, 2018, http://www.sheepcabana.com/?p=1180.
 “Indigo-a-go-go: Better Dyeing through Chemistry,” Sheep Cabana, accessed September 06, 2018, http://www.sheepcabana.com/?p=1180.
 H+ ions, or simply just the hydrogen nucleus with no electron.
 OH– or hydroxide, an oxygen and hydrogen atom held together by a covalent bond that carries a negative electric charge.
 AKA indigo white – for the fact that it is colourless in an alkaline solution.
 The chemical in indigo that produces the blue colour.
 A reddish-orange crystalline compound made by oxidzing indigo.
 A chemical compound most often produced as a byproduct of bacterial metabolism.
 “Unit – Chemistry of Textiles: Dyeing Fibres,” accessed September 06, 2018, http://wwwchem.uwimona.edu.jm/courses/CHEM2402/Textiles/Dyeing_FibresJ.html.
 Extrapolated from “Chapter 12: Dyes,” Caveman Chemistry : Hands-on Projects in Chemical Technology, 12.2, accessed September 06, 2018, https://www.cavemanchemistry.com/cavebook/chdye2.html.
 The removal (transfer) of a proton.
Here is the unedited documentation that accompanied the above project. The full works cited list is included.
Below is a project I completed several years ago regarding the creation of lemon balm tinctures. It was one of my first forays into alchemy and solidified my love and fascination with the subject.
Alchemy is often equated with the fantastical “search for the Philosopher’s Stone.” As Hutin says: alchemy is “commonly held to be the art of the transmutation of metals, a medieval pseudoscience whose object was to produce gold” (9). In actuality, alchemy was a complex precursor to modern chemistry that practitioners thought about and studied in many different ways: from what Hutin defines as Practical Alchemy, or the “direct application of theoretical alchemy” (14); to Mystical Alchemy, which was more spiritual in nature; to what was known as the Ars Magna, or Royal Art, which became popular in the 15th and 16th centuries, and combined the other two practices.
Alchemy is complicated. It requires a vast knowledge of a variety of subjects and a lot of study. It is very difficult to break alchemy down into its component parts and not simply leave the student far more confused than they were at the outset. Therefore, although alchemy consists of several theories, this section will focus on two of them: the three principles, and the seven stages, as well as the ideas behind Spagyrics.
The Three Principles
The three principles include ‘Sulphur,’ ‘Mercury,’ and ‘Salt,’ which, confusingly, are not the compounds we know today by those names, but are instead representative of certain qualities of matter. Sulphur refers to the ‘active properties’ (such as combustibility) and is often considered masculine. Mercury refers to the ‘passive properties’ (such as malleability, or volatility) and is considered feminine. Salt is the means of union between the two. In the case of these experiments, the potassium carbonate is the Salt, due to its presence as the middle step; the alcohol is the Mercury, due to its volatility and the fact that it is extracted by the process of distillation; and the lemon balm is the Sulphur due to its combustibility and the fact that it contains the essential oil of the plant.
The Seven Stages
Beyond this, there are seven widely accepted stages that an alchemical work (whether physical or spiritual) goes through. These are:
- Calcination: “Reduction by fire of substances, usually minerals, to powder or ash; subjection to roasting heat; the word also covered other processes, such as the addition of corrosive substances; pulverising of substances by fire to remove the moisture uniting the parts…pulverising over a fire” (101)
- Dissolution: “Separation into parts of constituent elements, disintegration, decomposition” (107)
- Separation: “Dividing into members, division of the pure from the impure” (111)
- Conjunction: “Mixture or union of elements or substances figured as marriage, copulation, uniting of male and female or brother and sister or king and queen sometimes to form an androgyne; the moment of conception” (105)
- Fermentation: “An idea of the process of transmutation…figured as leavening bread with yeast, gold is the ferment of the elixir, without which the philosophers’ medicine cannot be perfected…” (108)
- Distillation: “…three main kinds: by ascension, descension, or filtration; the rising of vapours of a liquid in its own container such as an alembic or a process in a descensory, but in both cases the purpose is purification” (107)
- Coagulation: “Conversion of liquid to solid; solidification, either by crystallization or by the cooling of a fused substance; reduction of liquid substances to a solid mass by deprivation of their vapours” (105)
These stages do not have to be physically obvious – i.e. the changes could take place on the spiritual plane rather than the physical one, depending on the alchemical work being produced.
Spagyrics is a very specific kind of alchemical methodology. The word comes from the Ancient Greek words σπάω spao “I collect” and ἀγείρω ageiro “I extract” and it tends to refer to a plant tincture that includes the ash of the calcined plant (in other words, potassium carbonate or potash). According to Hauck, “In spagyrics, the plant is dried, ground up, or pressed to concentrate its essences, which are then separated and brought back together in a more purified and potent form. The object of spagyrics is to isolate the living essences of the plant and preserve them for later use while at the same time getting rid of the useless or impure parts” (175). However, spagyric compounds take time. These compounds must meet very specific conditions to say that it is spagyric and they take much longer to make than normal chemical compounds, because “spagyric preparations must be made during certain alignments of the planets that are determined by the signatures of the plant itself” (Hauck 176).
 All definitions taken from Roberts 1995
 Evaporation (Roberts 101)
 A method of distillation or fusion in which fire is applied on top of the vessel and the liquid product or essence flows down into the receiver below (Roberts 107)
 Straining a thing through a woollen cloth or paper (Roberts 108)
 Chemical furnace in which liquid falls downward from the gross matter (Roberts 107)
 Craig p. 730
 See additional documentation for more information about Alchemical Astrology and plant signatures
Lemon Balm Tincture
Alchemy is, at its core, a combination of both science and mysticism. From those who wish to experiment and find ways to create something new, to those who believe the spiritual journal of alchemy is more important, including all of those in between, there are a multitude of ways to practice and experience alchemy.
Today I submit a look into the process of alchemical experimentation, specifically with regards to the creation of the Primum Ens Melissae or the ‘First Entity’ of the herb today known as lemon balm.
In order to fully explore the process of alchemical experimentation, I created five tinctures using slightly different materials and methods in order to examine the outcomes of each. The reason for the number of experiments is due to the various combinations of materials that need to be tested.
Four of these involved mixing and matching fresh versus dried lemon balm, and using potash versus a plain tincture, but the method will be identical. The last one will be based on a recipe for the Primum Ens Melissae attributed to Paracelsus, which involves a different method.
During the creation of these tinctures, I also participated in the common practice of using spagyrics as described above to invoke the mystical, or spiritual, side of alchemy.
Alchemy was only for the initiated. It was cloaked in secrets, codes, and riddles, making it virtually impossible for anyone to decipher notes or conversations unless they had been inducted into the order.
However, alchemical experimentation could be performed by anyone who thought they understood what they were doing, but unfortunately many of those people were hacks and con men who were incapable of producing anything of worth. There were, of course, also those people who published books and were widely respected in their time and beyond, and those who made great strides in the fields of chemistry and medicine, without whom our own scientific fields would be vastly different.
This particular experiment is based on a modern recipe (in order to have a starting point – due to the secretive nature of period alchemists they didn’t really have ‘recipes’). In order to develop a tincture that would have been used in period as a remedy for various ailments (what ailments were treated often depended on which planet was associated with the plant). While the recipe itself (the one used for the first four experiments) may be modern, the process of experimenting with different materials and different methods was period. The fifth experiment, the Primum Ens Melissae, is based on a recipe that is ostensibly from Paracelsus, a Swiss alchemist who lived in the first half of the 16th century. However, the source it comes from (Hartmann) fails to cites its own sources properly. This is unfortunate, but it is the closest thing to an ‘alchemical recipe’ that I have been able to procure, which is why this is a process piece on the method of experimentation, rather than an accurate reproduction.
Western alchemy itself (as opposed to Chinese or Indian alchemy) has existed for hundreds of years, generally thought to have begun in Egypt, and spread through the Islamic world to Europe after the Roman empire fell. The earliest writings that still exist after the burning of the Library of Alexandria in 292 CE are from sometime around 300-500 CE. It picked up in Medieval Europe in the 1100s when Arabic books were translated into Latin and lasted until it was mostly replaced with more modern sciences in the 18th century.
I decided to undertake this experimental process piece, because the complexity, secrecy, and methodology of alchemy intrigue me. Alchemy is one of the cornerstones of modern science, without it, discoveries would not have been made and chemistry would be centuries behind where it is now.
 Definition: a medicine made by dissolving a drug in alcohol.
 A potassium-primary compound such as potassium carbonate. Can also be potassium hydroxide (caustic), or potassium sulfate or a number of other compounds.
My hypothesis for this experiment is that fresh lemon balm works better than dried, potash can assist the process when used correctly, and that the more period recipe for the Primum Ens Melissae will be the most successful in terms of appearance (and not actual medicinal qualities).
Included in the footnotes are possibilities for what part of each method corresponds to each of the Seven Stages detailed in Appendix 1.
Experiments One to Four
The methods used for Experiments One through Four were nearly identical
- Begin the experiment on a Thursday, between 3:26 AM, and 6:51 AM, preferably during the first hour after Sunrise, as this is the time of day, and week, when Jupiter rules.
- Prepare the menstruum
- Return the Celestial Fire (animate the Mercury) by slowly pouring the alcohol into an open glass while heating the glass gently with the warmth of your palms; gently swirl the alcohol to agitate it
- Meditate or pray for the secrets of Melissa Officinalis to be revealed to you, and that a sacred place be created in your heart and lab
- Take half an ounce (14.1g) of dried Melissa Officinalis (Lemon Balm) OR 6.5g of fresh Melissa
- Crush the Melissa by hand at first, then by mortar and pestle as you focus on the idea of releasing the divine essence of the herb
- Put herb into a clean glass jar
At this point Experiments One and Two continue thusly:
- With focused intent pour alcohol over the herb until it is saturated (but no more than 2/3rds full)
- If using a metal lid, cover it with a barrier (like plastic wrap) so the solution does not come into contact with metal
- Seal the jar, wrap it, and place it in a warm place
- Shake the jar every day for 14 days, returning it to its warm, dark place
- After 14 days, leave it undisturbed for an additional 21 days
- Filter out the tincture and place in another glass jar
While Experiments Three and Four continue this way:
- Take the dissolved potash, pour it over the herb with focused intent
- Then pour alcohol over the potash saturated liquid, again with focused intent, until the jar is 2/3rds full
- If using a metal lid, cover it with a barrier (like plastic wrap) so the solution does not come into contact with metal
- Seal the jar, wrap it, and place it in a warm place
- Shake the jar every day for 14 days, returning it to its warm, dark place
- After 14 days, leave it undisturbed for an additional 21 days
- If the potash is highly concentrated enough, and the alcohol is of a high enough proof, the parts should be separated. Therefore extract the alcohol using a syringe. If the parts have not separated, the experiment is a failure.
Experiment One – Dried Lemon Balm
As the first experiment, this appeared to work fairly well. Over the first 14 days, the solution started out with a reddish-brown tinge that contained some green, but gradually became a darker brown. It remained cloudy and would produce a slight foam when shaken. Eventually, shaking the mixture produced no change, and at the end of 14 days, it was left alone in a warm, dark space for an additional 21 days.
After the final 21 days, the lemon balm was removed by filtering the solution through cheesecloth, leaving behind a dark brown liquid.
Experiment Two – Fresh Lemon Balm
This experiment also appeared to work fairly well. The fresh lemon balm produced more of a green solution over the first few days, but as time progressed the solution began to turn reddish-brown as the leaves died and decomposed. It was a clearer solution than Experiment One, and foamed less when shaken. After 14 days, it was left alone in a warm, dark space for an additional 21 days.
After the final 21 days, the lemon balm was removed by filtering the solution through cheesecloth, leaving behind a reddish brown liquid that was more transparent than the results of Experiment One.
Experiment Three – Dried Lemon Balm and Potash
This particular experiment began rather poorly. Due to the fact that potash and high proof alcohol do not mix, agitating the solution led to initial clumping of the lemon balm and it did not seem as though it would work.
After the full experiment period (14 days of agitation, 21 days being left alone) the solution was filtered and turned out very similar to Experiment One. That is, a dark liquid was left behind. Except for the fact that it had a surprising green tinge to it. It was so green it was nearly black. Of course, unless the alcohol is siphoned off, the tincture is too alkaline for consumption. Once the alcohol and the potash was left to rest, it appeared to separate, but the colour was so uniform it was impossible to tell. Therefore I did not separate the alcohol off.
Experiment Four – Fresh Lemon Balm and Potash
Much like Experiment Three, this experiment began poorly, though luckily fresh lemon balm is not as prone to clumping as dried.
After the full experiment period, the solution was filtered and turned out, as expected, similar to Experiment Two with the result being a slightly more reddish-brown liquid. However, once again it had an emerald green tinge to it in certain lights.
Again the solution needed to separate before the alcohol could be siphoned off to create a consumable tincture. This time, there was enough of a colour difference to siphon off the alcohol (alcohol was green, potash stayed reddish-brown).
Experiment Five – Primum Ens Melissae
This method is taken from Hartmann, which appears to have been quoted verbatim from Paracelsus, but with no actual citation:
“The Primum Ens Melissae is prepared in the following manner: – Take half a pound of pure carbonate of potash and expose it to the air until it is dissolved (by attracting water from the atmosphere). Filter the fluid, and put as many fresh leaves of the plant Melissa into it as it will hold, so that the fluid will cover the leaves. Let it stand in a well-closed glass, and in a moderately warm place, for twenty-four hours. The fluid may then be removed from the leaves, and the latter thrown away. On top of this fluid absolute alcohol is poured, so that it will cover the former to the height of one or two inches, and it is left to remain for one or two days, or until the alcohol becomes of an intensely green colour. This alcohol is then to be taken away and preserved, and fresh alcohol is put upon the alkaline fluid, and the operation is repeated until all the colouring matter is absorbed by the alcohol. This alcoholic fluid is now to be distilled, and the alcohol evaporated until it becomes of the thickness of a syrup, which is the Primum Ens Melissae; but the alcohol that has been distilled away and the liquid potash may be used again. The liquid potash must be of great concentration and the alcohol of great strength, else they would become mixed, and the experiment would not succeed” (300-301)
This method differs substantially from Experiments One through Four in that it is a much shorter time frame, and there is no agitation of the solution. This should lead to a lighter colour as the plant matter will ferment less, and should also lead to a clear separation between the potash and the alcohol.
This experiment did not turn out as planned. The potash leached the nutrients, and the colour, from the fresh lemon balm fine once the leaves were macerated, leaving behind a more yellow-ish tint than expected. Once the leaves were removed and the alcohol added, the solution remained separated.
However, the alcohol did not take on the colouring from the potash as expected. Instead, the solution remained separated as clear alcohol on top and yellow-tinged potash at the bottom. I am unsure whether the fact that the alcohol is denatured is the cause of this, or whether something else went awry in the experiment. More experimentation is obviously required after some more research.
 See Appendix 2 for more information about the Scientific Method
 In order to have a starting point, since period alchemical sources are often incredibly secretive and difficult to discern, the basics of this recipe were taken from a modern source, The Complete Idiot’s Guide to Alchemy, and supplemented by my own alchemical research.
 For more information about alcohol and the requirements for this experiment, please see Appendix 5
 For more information about Melissa Officinalis, please see Appendix 3
 Could be considered Calcination: pulverising the substance, though not over fire
 Could also be considered Calcination: addition of corrosive substance; also Conjunction
 Dissolution, Fermentation
 Distillation and Separation
 The creation of the potash would be the Calcination. For more information about the process of creating potash, please see Appendix 6
 Dissolution and Conjunction
 Due to the fact that the alcohol used was denatured, the tincture is already unsafe for consumption; however, in the interest of completion, this fact was ignored.
 Dissolution; additional Fermentation
Here I’ve included my full documentation for the lemon balm tincture experiment, which includes appendices that elaborate on important alchemical ideas above and beyond what I’ve already mentioned. The full works cited list for the above information is also included.
Sanguis Leonis (Blood of the Lion)
A more current project that I am attempting is the creation of a substance, an oil, known as Sanguis Leonis.
I first came across “Blood of the Lion” in a primer for modern, practical alchemy – hardly the most historical source – but the idea intrigued me. The primer did – in theory – take the idea from George Ripley, a known alchemist from the 1400s, but as it is not an academic publication there is a distinct lack of in-text citations, and so it was difficult to ascertain exactly where I could locate corroborating information. I’ve always been up for a research challenge, however, so I decided to see if it would lead me anywhere.
The initial information I had was as follows:
After isolation and purification, the metal acetate is subjected to a dry distillation. That is, the crystals themselves are distilled slowly at first, then gradually increasing to about 400° to 700°C. The products of this distillation are a volatile spirit (a Philosophical Mercury), an oil (the Sulfur of the metal, called the Lion’s Blood), a watery phlegm and a solid residue (often called the Black Lion) from which is obtained the Salt.Bartlett, Robert Allen. Real Alchemy: a Primer of Practical Alchemy. Lake Worth, FL: Ibis Press, 2009. p.84
Around 1450, the English alchemist George Ripley called this distillate the Blessed Liquor or Menstruum Foetens and describes it as containing three substances:
1. The Aqua Ardens – which burns like wine spirits.
2. A thick white water called Lac Virginum or virgin’s milk
3. A blood-red oil called Sanguis Leonis or Blood of the Lion
While I have not yet completed my research into this, and also have not compiled enough for any sort of documentation, I will be focusing on my own findings in this section. As mentioned several times, alchemy is often up to interpretation and my own research has led me to cross-check multiple sources (primary, secondary, and tertiary), I’ve run into various roadblocks such as different languages and lack of access to sources, and while my overall interest hasn’t waned, modern responsibilities have sometimes caused me to lose focus making me return again and again and try to remember what I have already figured out.
Current Data and Conclusions
I have not yet managed to locate an exact primary source, though Ripley wrote extensively on a concept known as the Greene Lyon. Most secondary sources agree that the Greene Lyon is a chemical solution, other authors sometimes use that term for iron sulphate; however, Ripley refers to it in conjunction with ‘Venus’ in his alchemical poetry, which is the planet associated with copper, which several academics have determined means Ripley is referring to copper acetate.
The seyd Menstrue ys, (I say to the in councellOf Congelation – The Sixth Gate (The Compound of Alchymie by George Ripley)
The blod of our Grene Lyon, and not of Vytrioll,
Dame Venus can the tweth of thys the tell,
At thy begynnyng to councell of yf thou her call:
Thys secret ys hyd by Phylosophers grete and small;
Whych blode drawen owte of the seyd Lyon,
For lac of Hete had not perfyt Dygestyon.
While I’m still in the process of determining exactly what needs to happen, I have come to several conclusions:
- I need to make something called the Radical Vinegar (essentially concentrated acetic acid imbued with the essence of copper)
- This involves distilling red wine vinegar until it is concentrated
- As household vinegar is normally about 5-6% acetic acid, this will likely involve several distillations. Distillations can be completed either by heat or by freezing, I opted for freezing as it required less of my active attention.
- After the vinegar is distilled, I take copper wire and burn it to begin to break it down and then I combine it with the distilled vinegar and heat it (I think), to attempt to form deep green crystals of copper acetate (Green Lion)
- Then distill the copper acetate again to get Radical Vinegar
- This involves distilling red wine vinegar until it is concentrated
- I then choose a mineral or metal ore and distill it with the Radical Vinegar
- I should get several results:
- Volatile spirit (possibly dangerous and explosive)
- Oil (Sanguis Leonis)
- Watery phlegm (Lac Virginum I think)
- Solid residue (Black Lion, also known as the alchemical Salt)
- I should get several results:
Although I definitely want to do more research before starting the second part, particularly if there’s a chance of it being dangerous, I figured I could start with the Radical Vinegar, as the initial distillation had to begin before anything else.
As mentioned, I opted for a frozen distillation method. Because acetic acid has a different freezing point than water, at low concentrations it will melt first, allowing for separation. Because I am using red wine vinegar, it’s easier to see when most of the acetic acid has separated.
I bought the red wine vinegar and separated it into spare pop bottles I had to make freezing it easier. Once they had frozen solid, I would suspend them in a funnel I had set up on top of another bottle in order to let the acetic acid drip out. Once mostly clear ice remained, I would do it again with another bottle. You can see in the image here that the acetic acid is beginning to separate from that top section as it all melts and makes its way into the second bottle.
One of the interesting, yet unfortunate, things about distilling acetic acid, is that there is a point where the concentration is high enough where the melting order switches. Acetic acid on its own has a higher freezing point than water – about 16.6 degrees Celsius – but when it forms a solution with water, the concentration levels can cause a freezing point depression and allow for a process called fractional freezing. However, when the concentration became high enough, the solution would no longer freeze solid as seen in the video below.
Additionally, after three distillations, it was very obvious that I was concentrating the acetic acid – accidentally breathing some in or getting it on your skin will cause irritation.* Beyond that, however, was the proof when I set a bottle of concentrated vinegar next to a newly purchased one from the store:
I would still like to try distilling it even further as my (less than accurate) math puts me at maybe 15% acetic acid, but I need to do some more research into fractional freezing methods to figure out how to accomplish this.
I’m still very interested in trying to complete this project, and if anyone has any suggestions or a background in chemistry that would like to assist/collaborate, I would definitely be interested in hearing from you.
*Ask me how I know!
The following item is a research paper I wrote on the linguistics of the rhyme scheme in the song “Three Ravens” as written down by Thomas Ravenscroft. I opted to upload it as a PDF in order to retain the layout and footnotes and to keep from cluttering the exhibit page. You can download it below. If there are issues with downloading, or with PDFs, please let me know and I will endeavour to get you a copy another way.
Additionally, I approached this topic from the perspective of a linguist as opposed to a performer or bard, and focused more on the research through primary and secondary sources, as well as the actual process of interpreting pronunciation. Therefore, there is a lot of terminology that the paper covers prior to the main discussion in order to allow all readers a somewhat even footing.
As a note: I am aware of the Shakespeare in Original Pronunciation movement and linguist David Crystal’s work in this area, and I do cite him in the paper; however, I discovered his contributions after the majority of my own research had been completed.
Thank you to everyone who took the time to look through my work, I hope you enjoyed it and I really appreciate your time.
If you would like to leave any comments, questions, or suggestions, please feel free to do so below, or schedule a one-on-one Zoom conference with me. I’ll also happily talk to people through other means at other times if you’d like to contact me separately.