"take lye made from quicklime and white lead, mix and leave to soak and you will have a dark brown dye, and reiterating the same you will make black. Try other colours with the lye made of lime"

Name: Sophie Pitman, Naomi Rosenkranz, Jenny Boulboullé
Date and Time: 4/5/2015, 2pm

2016.April.5, 2:00pm

Location: Chandler 260
Subject: Making lye from quicklime
"take lye made from quicklime and white lead, mix and leave to soak and you will have a dark brown dye, and reiterating the same you will make black. Try other colours with the lye made of lime"

The manuscript mentions quicklime 9 times, but does not give a recipe to make 'lye made from quicklime'. Therefore, I used a modern recipe found online,

How to make Lye using Quick Lime (Calcium Hydroxide) Calcium hydrixide is a chemical compound known more commonly as slaked lime. It is formed when calcium oxide is mixed with water. Put 3 pounds of washing soda, 3 pounds of slaked lime, and 12 quarts of water into a large pot. Boil for 20 minutes. Wait for the contents to cook, and when cold, pour off the liquid part which is your lye.

This recipe was also followed by Yi and Kok in their preliminary dye experiments, (unusually they chose this lye, which is not the usual recipe used by dyers - which would involve wood ash rather than quicklime), so I followed their proportions.
This was their workflow:

Name: Yuan Yi, Cindy Kok Date and Time: 2015. Nov. 16, 12:57 PM Location: Chandler 260 Subject: Making Lye for Dyeing with Saffron We consulted a modern recipe for making lye from this site: __http://www.countryfarm-lifestyles.com/make-lye.html#.VkK30rerSUk__ Measured 2 beakers of 500 ml of water. Measured 60g washing soda x2. Measured 60 g quicklime x2. Placed each beaker on a burner around 1:10pm. Began boiling around 1:15pm. 1:18 adjusted boiler on right to 2 to see difference in boiling. 1:20 adjusted boiler on right to 3, boiler on left to 2. 1:24 roiling boil on right side, turned down to 2. Continued to adjust boilers to keep them gently boil. Smells faintly like baking bread? burnt toast? Turned off at 1:35 pm.

My questions:

I need to make lye from quicklime for this black dye experiment, but I had certain questions to address in this initial experiment - namely, why make this lye from quicklime when it is the less common recipe (and more dangerous) way to make lye? The more usual way, and far easier, is to just pour water over wood ash. What struck me when I discovered that quicklime was being made in the lab by calcining oyster shells was that it made material sense for the author/practitioner to experiment with materials that he was already working with in the workshop. That the lab had this leftover material from former experiments, and I was able to use, gave me new insight about what materials were at hand to the author/practitioner. I suspect that this experiment does not work with wood ash lye - and I intend to experiment with lye made with wood ash later on. For now, I will follow the recipe as best I can, and will test with such controls later on.

Thoughts:

I found myself both excited and anxious in this experiment. For the first time I was in the lab leading an experiment, rather than working on skill-building exercises where the postdocs and other students had a clear idea of process and outcome, and could discuss ideas together. This time Naomi, Jenny and I were asking a lot of questions, but had few answers - and they were looking to me as the annotator to lead the process. Having researched quicklime explosions, I was nervous of my materials - I have not used such materials before, how would they react? Would it work? I was also really excited to be making something, to be getting started on the experiment. Already the recipe was forcing me to think hard about materials, and what 'lye made from quicklime' was - the author/practitioner doesn't give a recipe for it, so it must be something he already knew how to make and/or was commonly made.

My workflow:

Following the SDS and research about quicklime online, I decided to follow this procedure in the fume cupboard, to avoid fast exothermic reaction when water interacted with the quicklime.

• A note on materials:
• The Quicklime was already in the lab stores - and I believe was made from oyster shells from the lab (although the tub of quicklime was not labelled with this information - I was told this by Naomi and Jenny).
• Process:
• Set up hotplate in fume cupboard
• Poured 500ml of distilled water into each 1000ml beaker
• Poured 60g of sodium carbonate into each glass beaker of water, under the fume hood
• Measure 60g of quicklime in each of the 2 beakers, under the fume hood, stirring and gradually placing the quicklime little by little
• Placed beakers on hotplate at 14:50, on minimum heat
• After 2 mins, have a milky appearance
• Stirred at 14:56
• Turned up to 3 at 15:12 - still not boiling
• Turned down to 2 at 15:15 to contain boiling
• Turned up to 3 at 15:31 as not boiled yet
• At 15:33 boiling
• Turn off at 15:43, no smell (as I did my experiment in fume hood)
• Left the lye to cool overnight, covered, in the fume hood.

Click the arrows below to view a slideshow of this process

Name: Sophie Pitman and Naomi Rosenkranz

Date and Time: 4/6/2016

2016.April.6, 10:30am

Location: Chandler 260
Subject: Adding leads to the lye
"take lye made from quicklime and white lead, mix and leave to soak and you will have a dark brown dye, and reiterating the same you will make black. Try other colours with the lye made of lime"


My questions:

Although this recipe has been translated as 'white lead', I wonder what the author/practitioner means by the French term he uses - 'litharge'. I decided to experiment with three possible materials - all of which can be termed 'litharge' - white lead, red lead, and yellow lead. Would any of these make a black dye when combined with quicklime? How much should I use? There are no quantities, proportions or indications of time in this recipe - how long should I 'mix' and 'leave to soak'? Am I to soak the lead and lye together or does 'soak' indicate I should add whatever I want to dye? What is this recipe a dye for? I am assuming textile, but how do I know? Will I be able to find out? I was also curious as to whether my lye was effective - was this recipe going to work, and if not - was I already setting myself up for failure by using a self-made lye? I asked Naomi to order some commercially made lye (one made of quicklime, and another of wood ash) so that I can test with them to compare with the lye I have made.

Thoughts:

If working with quicklime had made me nervous, working with lead was even more daunting. I found myself constantly tweaking my lab coat and gloves to ensure no skin was exposed, and becoming increasingly conscious of any itches or the need to touch my face (which I was unable to do for nearly an hour). Naomi's presence in the lab was essential - as a safety check, someone to bounce ideas off, and someone to take photographs as I handled the leads in the fume hood. I was hoping for immediate results, when the lead/lye mixes did not turn immediately black, I worried that I was doing something wrong. What had I missed? Was the lye not strong enough? Maybe I didn't boil it enough? Was I using the right substances for 'litharge'? Were my proportions off? I didn't doubt the recipe so much as myself. I feel so amateur at all of this, I think the hardest thing to overcome so far is my own confidence in doing experiments. As someone who has not set foot in a lab for well over a decade, when the last time I thought deeply about chemicals was in my mid-teenage years, I lack confidence in this area - I know I shouldn't, but I do. Although I am increasingly convinced that the arts/sciences divide is unhelpful and artificial both in historical terms and in contemporary life, for so long I have self-defined as someone who works in the humanities and so science labs were out-of-bounds spaces. Also, making dye in a lab seemed incongruous. The only experience I have had with dyeing takes place in kitchens, sheds, artists workshops or gardens - with natural ingredients. The lab coat, gloves, fume hood environment, handling dangerous materials like lead and quicklime, made me feel far away from textiles and dyeing.

• A note on materials:
• I used Kremer pigments for the white lead (aka cremnitz white), red lead (aka minium), yellow lead (aka litharge, massicot)

• Process:

• Laid out all the materials - glass beaker for lye, 3 scoops (1 for each lead), the tubs of white lead, red lead, and yellow lead, the tub of lye, distilled water, six plastic pots with lids - prelabelled, a scale (covered in plastic to enable easy clean-up) - on newspaper, in the fume hood.
• My aim was to make 6 pots: white lead with lye, white lead with distilled water (a control), red lead with lye, red lead with distilled water (a control), yellow lead with lye, and yellow lead with distilled water (a control) each with the ratio 100ml liquid to 1g of lead - I chose this ratio based on the container size, and decided that if this did not yield successful results, I could adapt the ratio in later experiments. The MS recipe has no indication of quantity.
• As we were working with lead, safety was paramount - we worked with the fume hood as closed as possible, and sealed our lab coats to our gloves with elastic bands.
• I decanted 100ml of lye (trying to keep the top liquid separated from the sediment) into a glass beaker, and poured this into the plastic pot labelled 'White Lead and Lye'
• Then I measured out 1g of white lead (this was incredibly hard in the fume hood, as the scale was extremely sensitive and the airflow and plastic wrap both caused the scale to fluctuate).
• I scooped small amounts of the white lead into the pot, anticipating some colour change - would this be when the liquid became black?
• There was no colour change, the lead was incredibly hard to stir into the lye and didn't easily dissolve, although with stirring did start to dissolve a bit. Much of the powder balled up into chunks that had to be broken with the stirring utensil.
• 
• Then I added white lead to the water (the control pot) and it was even harder to stir in - it formed a filmy substance that resisted being dissolved in the water.
• I covered both containers with lids and cleaned off the scale to avoid cross-contamination of the leads.
• I repeated the measurements (100ml of lye/water with 1g of lead) with the red lead, adding small amounts of the lead bit by bit and stirring.
• The red lead has a bright, almost florescent orange, tone - it dissolved more easily than the white lead had done - and turned both the lye and the water the same tone as the lead powder - i.e. bright orange - still no evidence that this was a black dye!
• 
• I repeated the measurements (100ml of lye/water with 1g of lead) with the yellow lead, adding small amounts of the lead bit by bit and stirring.
• The yellow lead lost some of its brightness in both the lye and water - becoming a pale and murky yellow.
• 
• By 1pm, I had finished the experiment, and lined up the pots in a row against a white paper background - the only visible color change occured between the lye and white lead, which was turning a pinkish brown - could this be the dye? The lead in lye solution seemed to be separating more than the lead in water - the sediment at the bottom of the pots is more visible (as you can see in the image below).
• 
• Click the arrows below to view a slideshow of this process
• 

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Name: Sophie
Date and Time:

2016.April.8, 11:45am

Location: Chandler 260
Subject: Checking on lead in the lye, and leaving some uncovered
"take lye made from quicklime and white lead, mix and leave to soak and you will have a dark brown dye, and reiterating the same you will make black. Try other colours with the lye made of lime"


My questions:
What does the recipe mean by 'leave to soak' and for how long? I wondered whether perhaps the lack of color change was due to me leaving the mixture covered, so can I try leaving some exposed to air?

Thoughts:
I am already starting to feel more confident with my experiment, and being in charge in the lab. Maybe this is just from spending more time here, or from knowing that I can try and test my ideas and learn from their outcomes. Over the weekend, having left the mixtures open, I kept wishing I could take a look.

Process:

• I checked on the leads in lye and water, and photographed them to measure any change. The red and yellow lead mixtures did not seem to have changed much, except for some separation of sediment in the bottom of the container with a translucent liquid on top. The white lead in water was still a bright white, but the white lead in lye was distinctive - it was a darker pink/brown than two days before. This led me to believe that it was the most promising candidate for the black dye - perhaps white lead is the correct translation of the French 'litharge' in the black dye recipe on f38v of the MS.
• As the MS recipe does not mention whether the lye and lead mixture should be left "to soak" with a cover, I decided that I should try to leave some uncovered, to see if the addition of oxygen, or some evaporation, made the solutions look more like a black dye.
• This proved problematic - lead is dangerous, especially in solid form, and should not be inhaled. Therefore I decided to decant a small amount (less than half) of the lye/lead mixes (white, red, yellow) into open containers and leave them open in the fume hood. However, I knew that it was likely that all liquid would evaporate over the weekend, while the lab was closed. Still, I hoped that the solids left behind would indicate any color change.
• Click the arrows below to view a slideshow of the lead/lye and lead/water mixes after 2 days "left to soak" and the lead/lye pots uncovered in the fume hood

Name: Sophie Pitman
Date and Time:

2016.April.10, 12:00pm

Location: Chandler 260
Subject: Testing the lye, trying with some textiles
"take lye made from quicklime and white lead, mix and leave to soak and you will have a dark brown dye, and reiterating the same you will make black. Try other colours with the lye made of lime"

My questions and thoughts:
I am still wondering whether my lye is strong enough, so I want to test it. Over the weekend I have been thinking a lot about what 'leave to soak' means, and I am increasingly convinced that it implies that whatever is being dyed needs to be in the mixture. Would this change the colour of the dye? Have I been wrongly assuming that the liquid will be dark brown/black by itself? Do I need to add a substance to get a black tone? I have been assuming that what is being dyed is wool - I know from my own work on textiles in early modern Europe, and from talking with Giorgio Riello earlier this semester when he visited the lab, that this would have been the most commonly used textile. Not only were sheep flocks common in France (as in much of Europe) and wool readily available, it was relatively easy to dye. Cotton was incredibly rare in clothing in this period (becoming more common although expensive after increasing trade with India in the early 17thC), silk was expensive and rare, likely imported through Italy (although the author/practitioner mentions the cultivation of silkworms and is singles it out as a textile elsewhere in the MS). Linen would have been worn close to the skin - it was seen as the most healthy textile for undergarments as it could be washed and bleached easily - but it was not a common textile for making outer garments, and so would often not have been dyed. Moreover, linen was valued as something that could be easily bleached. Wool, a warm, ubiquitous and easily dyeable textile, seemed to be the most likely textile for dyeing (if, indeed, this recipe is to dye a textile - something I hope to address in my annotation). Also, in the context of other recipes, wool looks like the most likely candidate.

Following up after Friday's experiment to leave the lead/lye mixes exposed to air:

• As expected, much liquid in the uncovered lead/lye mixes left in the fume hood over the weekend had dissolved. I was disappointed to find that none of the uncovered lead/lye mixes had turned black, but the white lead/lye uncovered mx was certainly more grey black than the covered lead in water control or the lye and white lead covered. The yellow lye/lead uncovered was a darker yellow than the control and the covered lye mix. The red lead uncovered was a little darker, but had not changed much.

For images see this slideshow:



As the only distinctive color change towards brown/black (both in the covered and uncovered samples) had been in the white lead/lye mixture, I decided to test my fibers/textiles using this.

• A note on materials:
• We don't have any wool in the lab, and I was surprised that Yi and Kok did not test on wools in their dye experiments . In the absence of wool, I decided to test on my hair, as both are made of keratin, and are chemically similarso would make for a good comparison. Moreover, as I discovered in researching other similar recipes, the quicklime/lead mix was used in the nineteenth-century for hair dye, so hair seemed an appropriate substance to test. I will source wool and try in another experiment.
• I used the linen, cotton and silk that were in the lab, already sourced by Yi and Kok.

Process:

• 12pm - To test the lye, I decided to see whether I could dissolve a feather in it (as recommended by the website from which I took the lye recipe) I also dropped it onto some pH paper and it was very alkali (dark blue).
• 1pm - An hour later, the feather had not dissolved completely, but had started to break up.
• I cut small squares (c.1cm x 1cm) of cotton, linen and silk, and took 2-3 strands of my own hair (which is red/blonde) and placed them in individually labelled pots. I did this twice - so that each textile could be tested with the white lead/lye solution and with lye by itself.
• 1.17pm - Using a pipette, I squirted a few drops of white lead/lye mixture into each of the pots. The linen instantly started to go brown/black - something was happening! The cotton and silk both turned the pink/brown/beige of the white lead/lye mixture. The hair was hard to see.
• 1.21pm - The linen in white lead/lye was a darker brown/black
• 1.41pm - the hair in white lead/lye had turned black!
• 3pm - I decided to 'reiterate the same' and interpreted this element of the recipe as doing a second application of dye (I was using such small amounts so was not dunking textile or fiber into dye, but rather squirting the dye onto the textile or fiber)
• 3.20pm - The silk and cotton were just the pink/brown of the mixture, but the linen and hair were black in the lead/lye dye. The control pots of textile/fiber plus lye were all unchanged except for the linen, which looked a darker brown (was this because the linen is darker to begin with and when wet looks darker?)

For a slideshow of this process, click the arrows below:


Name: Sophie Pitman
Date and Time:

2016.April.12, 1:00pm

Location: Sophie's Apartment, 58th Street
Subject: Scouring Wool

I decided, after some encouraging results with hair, that I had to try dyeing wool. I sourced some 100% pure wool from the Lion Brand - it is a compromise as it is American wool from American sheep (rather than French wool from an historic breed) but is supposed to be good for hand dyeing.


To dye wool, it must be cleaned first. I followed the simple instructions from Wild Colours website, which explains that "Scouring is much more than washing; when you scour you remove grease and oils from the fibre as well as dirt."

• 1pm - Heated water in a kettle, and used about half a saucepan of boiling water to half a saucepan of cool water - the water should be approximately 50-60*c
• I added a generous squirt (c. walnut size) of natural dish soap to the pan of water.
• I snipped a little wool to retain a sample of the unwashed wool. The rest I plunged into the hot water, taking care not to aggravate the fibers (which would start felting the wool, easy to do when felting just requires hot water, some soap and lots of manipulation).
• The dry wool smelt faintly farm-like, but when I plunged it into the water, my whole bathroom - even apartment - smelt like a farmyard. My hands retained this smell for at least 2 days...
• After about 7.5 hours, the water had cooled and I wrung out the water from the wool, rinsing it in cold water to get rid of the soap.
• 9pm - I then hung the wool to dry overnight
• 9am on April 12 - The next morning it was slightly damp at the bottom, but dry enough to use. It didn't look different to the unwashed wool, but judging from the smell and brown tinge of the water, I had managed to get rid of a lot of oil and fats that were in the wool by scouring.

Process


For a slideshow of this process, click the arrows below:



Name: Sophie Pitman, Jenny Boulboullé

Date and Time:

2016.April.13, 9:30am

Location: Chandler 260
Subject: Testing lead/lye mixes with wool
"take lye made from quicklime and white lead, mix and leave to soak and you will have a dark brown dye, and reiterating the same you will make black. Try other colours with the lye made of lime"

The first thing I did upon returning to the lab 2 days later was to check on the white lead/lye and textile/hair samples that I had made on Monday.

• The linen and lye control had shrivelled into a hard pale brown ball
• The linen and white lead/lye, which had looked brown/black 2 days before, was bright white, powdery and very hard - so not a successful black dye on linen!
• The silk and lye control remained white
• The silk and white lead/lye still had a pale pink/brown/beige colour of the white lead/lye mixture.
• The cotton and lye control remained white
• The cotton and white lead/lye still had a pale pink/brown/beige colour of the white lead/lye mixture.
• The hair and lye control was even paler blonde than the original hair colour
• The hair and white lead/lye remained black!

For a slideshow of the samples 2 days later, click on the arrows below:


My questions and thoughts:
It seems that this recipe for black dye only works on hair, as after two days the linen had been bleached white. This leads me to think that the recipe is for some kind of chemical reaction that takes place with something that is in or on hair - keratin? So I expected that the white lead/lye mix would work on wool. I thought that I would also try to see if red lead (aka minium) and yellow lead (aka massicot, litharge) would also work with the wool.

• 10.30 - In the fume hood, I set up the lye and red lead, lye and yellow lead, and lye and white lead mixes. I prepared small plastic pots with labels and a c.4 inch piece of washed wool in each pot. I also prepared a control pot (just lye) and decided to try the wool and white lead both covered and uncovered to see whether oxygen was necessary for the reaction to take place.
• 10.35 - I used a pipette to squirt a few drops of red lead/lye on some wool. It immediately soaked up the bright red/orange colour.
• 10.40 - I used a pipette to squirt a few drops of yellow lead/lye on some wool. It immediately soaked up the bright yellow colour.
• 10.42 - I used a syringe (as the mix was too thick to take up with a pipette) to squirt a few drops of white lead/lye on some wool, in two different pots. It immediately soaked up the pale pink/brown colour.
• 10.43 - I used a pipette to squirt drops of lye onto wool for the control. The wool became a pale yellow.
• By 10.45 the lead/lye mixes were already turning darker. I left the wools 'to soak' for 15 minutes
• At 11am I 'reiterated' the process of adding the lead/lye mixes to the wools by squirting a few drops onto each piece of wool.

For a slideshow of the adding lead/lye to wools click on the arrows below:


Outcome:

Even before the 'reiteration', the three wool samples dyed with lead (red, white, and yellow) were already turning dark brown/black while the lye control had not changed color. After the reiteration, all three lead/lye mixes had turned the wool samples dark brown/black. I left a sample of each covered in plastic pots.


Name: Jenny Boulboullé

Date and Time:

2016.April.15, 5.45pm

Location: Chandler 260
Subject: Checking on wool samples dyed with lead/lye
"take lye made from quicklime and white lead, mix and leave to soak and you will have a dark brown dye, and reiterating the same you will make black. Try other colours with the lye made of lime"


Jenny was in the lab with another group and offered to check on my wool samples for me. The photo she sent me was a disaster - the wool had completely dissolved in the pots, all that was left in each sample was a black liquid (the red lead sample still had some bright orange liquid too, mixed into the black). Even the wool control sample, left in lye, was gone.



Name: Sophie Pitman, Donna Bilak

Date and Time:

2016.May.2, 1.00pm

Location: Chandler 260
Subject: Repeating the lead/lye dye experiment, and then washing/removing wool to avoid disintegration
"take lye made from quicklime and white lead, mix and leave to soak and you will have a dark brown dye, and reiterating the same you will make black. Try other colours with the lye made of lime"

Thoughts:

I had been a bit anxious that the washing process would remove a lot of the black color, but during my research for the annotation, had discovered that the black color was actually a permanent result of a chemical reaction that occurred within the core structure of the hair (or in this case, wool) itself - creating a lead sulphide that was black in color. Therefore I anticipated that the color would not 'wash out' as such, but perhaps I would halt the color change process midway?

Process:

After the last experiment, where the wool was successfully dyed black but then disintegrated, I decided to repeat the process but then add a finishing step. Was it sufficient to just remove the wool from the pot with the lead/lye dye or would I have to wash? To find out, I decided to dye two samples of wool with each lead/lye mix (red, yellow and white) and then remove one sample from the dye pot and leave, and wash the other sample in three pots of tap water.

Having been surprised by how quickly the color change occurred before, I decided to film the process this time around - Donna helped me with this, and like Naomi had been first time around, was an invaluable right-hand helper - taking dozens of photographs with her phone, taping up my sleeves, and talking through processes with me.

I repeated the dye process I had used on 2016.April.13 (see above for my field notes) and then about 5-10 minutes after the 'reiteration,' when the wool was black, I used chopsticks to take the wool out of the dye mix and into a clean pot. These samples I labelled 'wool removed from lead/lye mix, unwashed'. With the other samples, I decided to dunk the wool into water, swirl it a little (only for a couple of seconds) and then transfer to another clean bath, repeat, and wash a third time. I then took the washed sample and placed it into a clean dry pot, labelled with the word 'washed'.


For a slideshow of the process, click the arrows below:
(*nb, the final photograph with dissolved wool was the outcome of my previous experiment, and what prompted me to experiment with removing the wool from the dye mix and washing)

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ASPECTS TO KEEP IN MIND WHEN MAKING FIELD NOTES

• note time
• note (changing) conditions in the room
• note temperature of ingredients to be processed (e.g. cold from fridge, room temperature etc.)
• document materials, equipment, and processes in writing and with photographs
• notes on ingredients and equipment (where did you get them? issues of authenticity)
• note precisely the scales and temperatures you used (please indicate how you interpreted imprecise recipe instruction)
• see also our informal template for recipe reconstructions
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