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Brígiða Vadesbana Copyright 2007-2010
Blue dyes from Plants
There is only one known source of natural blue dye used for clothing, a natural chemical called indigotin.1 Ancient and Medieval writings record a number of plants which will produce this blue colour; in fact, there are over 500 plants that can be used to make indigo dye.2
The most common source of indigo is from plants in the genus Indigofera, native to tropical climates, though not all indigofera contain indican, the indigo-precursor in Indigo-dyeing plants. Indigofera tinctoria, also known as Indigofera sumatrana, is the species most commonly used in Asia and India. Indigofera suffructiosa was used in Central and South America. Indigo is a member of the legume family and related to peas and beans. In Northern and Western Europe, being a temperate climate and unsuitable to grow indigo, dyers used woad (Isatis tinctoria), part of the mustard family, and distantly related to cabbages. Woad is native to southern Europe, but can be cultivated in more northern climates. Chinese and Japanese dyers, also living in a temperate climate, used dyer's knotweed (Polygonum tinctorum), also known as Chinese Indigo, belonging to the buckwheat family, a plant not native to Japan, but brought from China in the 5th or 6th century CE. These plants also produce indican, but in much smaller quantities.
Indigo dyeing in the Western world has been traced back to ancient civilizations in Mesopotamia, Egypt, Greece and Rome, including a garment found in Thebes dating to c. 2500 BCE3 and a cuniform tablet from the 7th century BCE, found near Babylon, describing a recipe for dyeing wool lapiscoloured by repeated dipping4. India, China, and Japan, have used indigo as a dye for centuries, creating elaborate patterned cloth through both dyeing and resist-printing. The oldest indigo dyeing centres are believed to be in India. In the Greco-Roman period, it was the primary exporter of indigo dyes to Southern Europe. Herodotus (writing around 450 B.C.) describes its use in the Mediterranean area. During the Crusades, indigo became one of the highly prized spices aquired in Cyprus, Alexandria and Baghdad, at the end of the trade routes from the India and the Far
Huxtable Emmett 3 Mattson 4 Scott
East. 5 Marco Polo talks about the production of the dyes in his Travels.6 But because these dyes had to travel through many lands on their way to Europe, suffering from heavy export duties in Persia, the Middle East, and Greece, indigo-derived blue dye was rare in Europe during the earlier part of the mediaeval period, and most blue in the rest of Europe was from woad, which was cultivated in northern Italy, southern France, and parts of England and Germany.7 In 1498, Vasco da Gama, a Portugese explorer discovered a sea route to India. This allowed for direct trade with indigo producers in India, reducing its cost, and increasing its availability. Indigo flooded into Europe through ports in England, Portugal and the Netherlands, and quickly over-took the use of woad due to its ability to produce clearer, brighter blues. Not unnaturally, those area which had made their fortunes from woad, sought to stem the destruction of their industry by imported indigo, and in 1598, both France and Germany banned the import of indigo, and dyers were forced to swear, at risk of death, not to use it.8 In Asia, blue dye has been used since the Zhou period in China (1045-771 BCE). Most often the source of the indigo dye is Dyer’s Knotweed (Chinese Indigo). In Japan, blue dye was used early on, but it was a native dye known as yama ai (Mountain indigo) that was used in a technique called ‘rubbed blue’, created by rubbing the leaves directly onto the fabric. Because this did not bond the dye to the fibres the colour faded quickly and ran when washed. When Chinese Indigo (known in Japan as tade ai) was first introduced in 5th or 6th century CE, it was used the same way as the Mountain Indigo had been, until vat dye technology was introduced as well. Blue is a popular colour in Japan because the colour is considered auspicious. It also hides dirt well, has some insect-repelling qualities and is one of the few natural dyes that dye cotton easily, an important consideration since silk was expensive and at some points forbidden to the common people. It is still popular today as a dye for the cotton summer robes called yukata. A raw indigo dyeing procedure, uses fresh leaves in the dye bath itself was developed, but the colours are not nearly as fast, and fermentation vats were preferred.9 Synthetic Indigo was first developed c. 1880 and quickly overtook naturally sourced indigo for dyeing as the synthetic indigo was cheaper, clearer and more consistant due to its lack of natural impurities. It does not adhere as well to fibres as natural indigo, however and will start to wear off sooner.
Producing the Dye
The indigo plant itself does not produce the blue dye. Indican, the indigo-precursor in the indigo plant and in dyer’s knotweed, which is a by-product of the plant’s metabolic process meant to resist insect attack10, is a colourless, glucose-based substance, and during the fermentation process that results in a usable dye, a bacterial enzyme created in the vat consumes the glucose, leaving indoxyl. The indigoprecursor in woad is isatan-B, which also hydrolyses in the fermentation process to form indoxyl, two molecules of which bond together with an oxygen molecule during oxidation to form indigotin. It is from this substance the dye powder is made. Chemically, the two dyes are identical. Any
Mattson Polo 7 Mattson 8 West 9 Wisniewski 10 Emmett
discrepancies in the dyes from different sources are a result of natural impurities in the dyes, and in the quality of the crop they were derived from, and the skill of the dye producer. 11 In India, the traditional method of producing blue dye from indigo plants is via giant fermentation vats.12 These vats, usually brick, lined with cement can be as much as 400 square feet, and are usually arranged in rows, with the bottom of each vat roughly even with the top of the next, connected by drains. Indigo is harvested starting at 4-5 months after sowing, and can be re-harvested at 3-4 month intervals. The plant produces usable leaves for 2-3 years, after which the plant may live but the dye produced is distinctly inferior.13 Bundles of freshly indigo plants are placed in the first vats, and water is poured over them. Sometimes logs or other weights are used to hold the plants down. The plants are steeped until fermentation has almost ceased, which can take up to a day and a half. During this process, the indican is hydrolysed into glucose and indoxyl, the glucose being consumed by the fermentation process. It has to be carefully timed, as over-fermentation can ruin the batch, so this is usually controlled by an experienced dye-maker. When the liquor is dark blue and sweet to the taste, the indoxyl has been extracted from the plant and is ready to be turned into indigotin. The liquid is then drained off into the next vat, where men standing in the vat agitate it with large paddles, to oxidize it, adding the oxygen bond to the indoxyl molecules and thereby creating indigotin. The colour changes from dark blue to a yellow-brown, and the indigotin begins to separate into flakes, which are then allowed to settle to the bottom. A drain set into the vat above the sediment level drains off the liquid to stop the fermentation process. Sometimes the resulting run off is drained into a third vat and allowed to settle again to maximize the yield of the crop. The remaining indigo pulp is heated to remove impurities, filtered through cloth and pressed to remove as much moisture as possible. The solid mass is then cut and dried, ready to be transported to the dyer.14 In Europe, woad dye was produced by fermentation as well, though the leaves were dried before fermentation. The young leaves of the woad plant were picked (once the leaves turn blue, it is too late to produce dye from them), crushed and hand-kneaded into balls, which were then dried and stored until the dyer needed to use them. When more dye had to be produced, the balls were ground into powder and piled up in layers in “couching” houses, where the layers were made wet and allowed to ferment for two weeks, causing the isatan-B (the sugar-bearing molecule) to break down into indigotin. Woad fermentation is particularly foul-smelling, as woad plants contain sulphurous chemicals, which may explain why Queen Elizabeth I famously ordered no woad dye to be produced within 5 miles of any of her homes. After the woad had been couched, it was formed into cakes and sent off to the dyers. Dyer’s knotweed was processed in a similar fashion to woad. After the rainy season was over, the firstcut began. The plants are cut and dried on both sides in the sun, then cut into smaller pieces. While this was happening, the farmers would continue tending the fields and a month later a second harvest occurs. The leaves, once dry, are placed in straw bags to preserve them until the fermentation process is begun.
Huxtable Maiwa, video documentary 13 Kew Gardens 14 Maiwa, video documentary
In the fall, an auspicious day is chosen to begin process of creating sukumo (the fermented leaves). The first-cut leaves are place in fermentation beds and mixed with water to a height of about a metre. Every five days, the fermenting leaves are sprayed and mixed, then sifted with wooden rakes until they regain their original height. The whole process is repeated up to thirteen times, with the second-cut leaves added during the fourth sifting process. By the twelfth or thirteenth sift the leaves are placed on a screen to help them ferment evenly. As it is important to keep the leaves warm while fermenting, the sukumo is kept covered by straw mats. At approximately 100 days after the fermentation begins, the sukumo is packaged up in straw bags in specific weights and sent on to the dyers.15
Using the Dye
(note: as Indigo and Woad at this stage are identical, these methods can be used for both) Traditional Fermentation Vats Indigotin is more properly called a pigment rather than a dye, as it is insoluble in water or alcohol, and does not dye the fabric, but lies on top of it. To dye with indigo, the indigotin must be reduced to a water-soluble substance, causing the indigotin to become leuco-indigo, or indigo-white, which appears a greenish-yellow in the vat. In the reduction process the reducing agent creates indigo white by causing the indigotin to lose the oxygen bond between the two indoxyl molecules.16 When the fabric is spread out in the air, the indigo-white reoxidizes, and returns to its insoluble blue form, remaining trapped in the matrix of the fibres. While different ingredients are used by different cultures, the essential process for starting and using a fermentation vat is the same. The vat must be alkaline, with a pH of approximately 10.5. This alkalinity may be produced with various substances: lye, stale urine (ammonia), soda ash, lime, potash or ammonium carbonate (baker’s ammonia or smelling salts). The reduction of the indigotin to indoxyl can use a number of different substances as well: stale urine (urea), bran, madder, sake, crushed cane sugar, Karo syrup, and dates. These substances caused the composting in the vat, creating bacteria, which produces hydrogen, and removes oxygen from the vat. Fermentation vats are tricky, as fermentation continues so long as there is food for the bacteria. Overfermentation is a problem, and will ruin the vat. The vat must also be kept relatively warm, though not necessarily as warm as when in use, so that the bacteria do not die off. Recipes for fermentation vats often suggest exhausting the dyestuff in the vat before closing the vat, if it is going to be left unused for any length of time. The initial fermentation takes about one week, reactivating it by adding new dyestuff and reducing agents will take 3-4 days. One of the most common ways to accomplish this reduction was to dissolve the indigotin in stale urine. This fermentation in urine usually takes about a week, during which the vat must be kept warm. The urine provides nutrients to the bacteria which reduces the indigotin, and also the ammonia which causes the vat to become alkaline. The process is complete when the solution is a greenish-yellow, and there is a copper or iridescent blue scum on the top. Using urine has disadvantages, not the least of which is the smell! The urine-vat is one of the smelliest fermentation methods. It does have some advantages, however. Urine is readily available to anyone, (everybody pees!), is milder on protein fibres, and is generally the only thing you need to add to the vat
besides the indigo.17 Poor fermentation can be fixed with additional sugars to feed the bacteria, and ammonia can be used to increase the alkalinity. The fabric or thread to be dyed is presoaked in water or urine, then gently lowered into the vat. Because introducing oxygen into the vat reverses the reduction, it is best to keep the fabric tightly bundled until underwater, and then opened. Fabric is left to soak for anywhere from 20 minutes to 24 hours, then pulled out carefully, squeezing the excess fluid off, gently and just under the surface of the dye solution, and brought out tightly squeezed. The fabric should then be spread out on a line or bush and allowed to air for about 20 minutes, before being reintroduced to the vat. The blue achieved by the dyer depended on the strength of the dye solution and the number of times the fabric is dipped into the vat. A single dip in the vat produces a pale blue, while repeated dips can produce a blue so deep it is almost black. In fact, some mediaeval blacks were produced by repeated indigo dips, combined with the use of tannins or iron mordants. In several dye centres lists of names for each shade of blue created at each additional dip were given specific names, some of which are still in use today, like ‘Royal Blue’ and ‘Navy Blue’. It was these repeated dips that made blue fabric so time-consuming, and therefore so expensive. Some Fermentation Vat Recipes: Recipe #1 8 ounces finely powdered indigo 4 ounces wheat bran 4 ounces madder 1 ½ pounds soda ash (washing soda) 4 gallons water Put ingredients in a large pot or bucket, and keep at 30˚ C, stirring well, but gently each day until liquid is yellow-green and has a blue-copper scum on top. Recipe #2 1 gallon urine (allowed to go stale) 1 ounce indigo, powdered, in a fine mesh bag Put mesh bag of indigo in vat with urine, and set vat in a warm place (in the sun, but protected from direct sunlight). Twice a day rub the bag between your fingers in the vat to help release powder from bag. When liquid turns greenish-yellow vat is ready to dye. Recipe #3 1 tablespoon yeast 1 cup warm water 1 rounded tablespoon sugar 2 level tablespoons indigo powder ½ cup non-sudsing ammonia Combine yeast, water and sugar in a container and let stand in a warm place 2 hours. Mix indigo with ammonia and let stand 2 hours. Add indigo mix to yeast mix in a half-gallon container, fill to top with
warm water and seal with a non-rigid seal (like saran wrap) and allow to stand several days. Vat is ready to when the liquid has turned yellow. Note: Some synthetic indigo dyes do not reduce properly in fermentation vats. It is recommended to always use natural indigo in fermentation vats. Chemical Vats Chemical vats are a modern adaptation of indigo vats. A typical chemical vat uses caustic soda (lye) as a reducing agent, and sodium sulphite, (e.g. Thio-Urea Dioxide), or sodium hydrosulfite to provide the alkalinity. The chemical vat has a few advantages over traditional fermentation vats, not the least of which is the smell! A chemical vat requires only a few hours to become active, and can be allowed to cool when not in use and left unused for a considerable length of time (my chemical vat was left approximately a year at one point). Warming and the addition of the reducing agent can easily reactivate it. Chemical vats can also be made much stronger than fermentation vats, allowing for much quicker build-up of colour. However, this speed, ease and olfactory relief come at the price of end results. Lye is extremely caustic and damaging to fibres, shrinking cellulose and eating protein fibres (and protein human skin cells). In the correct amounts needed for dyeing with indigo, it should neither shrink your cotton and linen, nor eat your wools and silks, though you do need to rinse them very thoroughly to prevent damage to the fibres. Another problem is that while the first few dips in a chemical vat do create a deeper blue each time, after only a few the differences between dips become much less noticeable, as the thio-urea is a discharging (bleaching) agent and discharges the indigo the vat previously deposited. A true, even, and deep blue is very difficult to achieve. A very strong dye solution may give you a dark blue, but result in a much less even, beautiful colour. Thio-Urea also makes over-dyeing difficult because it may discharge the previous colour. Always dye with the indigo first. Also, while a fermentation vat is used at its normal temperature, and thus is gentle on sensitive fibres like wool, the suitable temperature of a chemical vat for cellulose fibres is 90-100˚ F; the temperature for protein fibres is 120-130˚ F. As in fermentation vats, the fabric or thread to be dyed is presoaked in water, then gently lowered into the vat. Again, because introducing oxygen into the vat reverses the reduction, it is best to keep the fabric tightly bundled until underwater, and then opened. Fabric does not need to be left to soak for more than a few mintues. Pull out carefully, squeezing the excess fluid off, gently and as near to the surface of the dye solution as possible. The fabric should then be spread out on a line or bush and allowed to air for about 20 minutes, before being reintroduced to the vat.
Chemical Vat Recipes: Recipe #1
Stock Solution: 1-1/2 Tsp lye (caustic soda), dissolved in hot water Add 2-4 tsp finely ground indigo dye and stir for 2 minutes. Add 1 tsp thiourea dioxide and stir for 1 minute. Put a lid on the container, and place in a warm spot for 1 hour Solution should change from opaque blue to translucent yellow-brown. Preparing the Vat: Put 5 gallons of hot water in a plastic bucket Add 1/8 tsp of lye and stir until dissolved. Add 1 tsp thiourea dioxide and stir until dissolved Cover vat and allow it to reduce for 15 minutes Carefully lower jar of stock solution into vat and pour out contents. Stir gently and allow to reduce for 1 hour. Possible substitutions from the grocery store: Lye may be replaced with ‘washing soda’ (in the laundry detergent aisle, and Thiourea Dioxide can be replaced with Rit Colour Remover.
ALWAYS WEAR GLOVES!!! Fermentation vats contain bacterial agents, which may cause a reaction (and fermenting urine is just icky, even if it’s your own!). Chemical vats contain caustic chemicals, which will eat your skin (or at least the top layer of your fingernails-trust the voice of experience!). An apron is a very good idea. Always dye outside, or in a well-ventilated area, as the chemical vat in particular causes harmful vapours when heated (the fermentation vat just smells really bad). Remember, you can wear a vapour mask. You can’t put one on your cat. Trust me. Interesting Fact: Indican is a by-product of the indigo plant’s metabolic process meant to resist insect attack, which gives indigo-dyed fabric a mild insect-repelling quality!
Burnston, Sharon Ann. “Mood Indigo, the Old Sig Vat or Experiments in Blue-Dyeing the 18th Century Way” 2005. May 4, 2005. <http://www.sharonburnston.com/indigo.html>. Crowfoot, Elisabeth, Frances Pritchard and Kay Stanisland. Textiles and Clothing 1150-1450. The Boydell Press. Woodbridge. 2001. Emmett, Susie. “New life in an old dye” New Agriculturalist Online Issue 14: 00-2. Jan 20, 2007. <http://www.new-agri.co.uk/00-2/focuson/focuson3.html>. Gibson, Arthur C. “WOAD IS ME” Date Unknown. Plants and Civilization. Apr 28, 2005. http://www.botgard.ucla.edu/html/botanytextbooks/economicbotany/Isatis/ Mattson, Anne. “Indigo in the Early Modern World”. Date unknown. Jan 20, 2007. < http://bell.lib.umn.edu/Products/Indigo.html> Polo, Marco. The Travels: Description of the World. Trans. William Marsden, Thomas Wright. Konemann. Koln. 1996. Priest-Dorman, Carolyn. “Colors, Dyestuffs, and Mordants of the Viking Age: An Introduction” Apr. 24, 1999. May 4, 2005. <http://www.cs.vassar.edu/~capriest/vikdyes.html>. “Indigo: A World of Blue” Maiwa Handprints Ltd. Video Documentary. Date Unknown Maiwa Handprints Ltd. “Indigo: Natural or Synthetic” 2005. Maiwa Handprints Ltd. Feb 22, 2007. <http://www.maiwa.com/pdf/indigo_data.pdf> West, Jean M. “The Devil's Blue Dye: Indigo and Slavery”. Date Unknown. Slavery in America. Feb 22, 2007. < http://www.slaveryinamerica.org/history/hs_es_indigo.htm> Wisniewski, Mark. Dyeing to Dance. Hiroba International, Japan. 2004. Liles, J.N. The Art and Craft of Natural Dyeing: Traditional Recipes for Modern Use. University of Tennessee Press. 1990. http://invention.smithsonian.org/centerpieces/whole_cloth/u3tc/u3materials/natDye.html Kew Gardens. “Indigo” date unknown. Plant Cultures: Exploring Plants and People. Feb 22, 2007. <http://www.plantcultures.org.uk/plants/indigo_plant_profile.html>