Name: Isabella Lores-Chavez and Charles Kang
Date and Time:
2016.10.24, 1:40 pm
Location: LabSubject: Grinding madder root and soaking
To make red madder lake, we are following the recipe found in Kirby (as are the rest of the groups in the lab).
The first step in making madder lake pigments is to grind the madder root. We measured out and weighed 6 g of madder and used two different mortars and pestles. The porcelain mortar and pestle was less effective at breaking up the madder root than the stone mortar and pestle. We used two main techniques: crushing with the pestle and twisting the pestle into the madder root to grind it. While grinding the madder, we could smell the smokey, earthy scent of the organic material. Some of the roots were tough and difficult to break up. We spent a total of about 15 minutes grinding the root.
When we had a mixture of powder and broken up roots, we transferred our madder to a piece of polyester netting. With all the ground madder nestled in the center of the polyester netting, we bound it up like a tea bag and tied it with a piece of string. We then prepared a 180 mL of distilled in a 250 mL beaker and placed the polyester netting bag in the water. We pushed it into the water with our fingers to make sure that the bag was really soaking up the water, and watched as red tints began to color the water.
We left the beaker with the polyester netting bag soaking overnight, with a parafilm covering to prevent any debris from falling into it.
Name: Isabella Lores-Chavez and Charles Kang
Date and Time:
2016.10.27, 1:00-3:00 pm
Location: LabSubject: Heating and adding potash alum + potassium carbonate (potash)
During the next phase of making red madder lake, after soaking it overnight, we heated the madder and added potash alum and potassium carbonate to it.
First, we removed the parafilm from the glass beaker and prepared to set it on a hotplate. We found out from the postdocs that the madder solution we were using was actually not the same one as the one we had prepared on 10/24. Another student had needed to use the solution first in the lab, the previous day, so Professor Smith had ground more madder for us, put the ground madder in a polyester bag, and soaked it in a glass beaker overnight. Professor Smith had indicated that the madder was not entirely finely ground, something for us to be aware of as it could potentially change our results.
We had a thermometer ready to note the temperature of the liquid on the hotplate constantly; we left it sitting in the solution, resting it against the polyester bag to avoid directly touching the hot bottom of the beaker with the thermometer (which would give us a slightly inaccurate read on the temperature of the solution). We turned the temperature up on the hotplate, perhaps a little too eagerly: for a few minutes, the temperature climbed very slowly, then suddenly climbed up to 80 degrees Celsius, 10 degrees higher than what we were aiming for. To counteract this, we took the beaker off of the hotplate for a few minutes, keeping the thermometer in the solution to ascertain when the temperature lowered to 70 degrees Celsius. As we waited for it to cool, we also turned the hotplate temperature back down to a very low setting. Meanwhile, however, we took note of when the solution had first hit 80 degrees Celsius and started timing 30 minutes of extraction from that moment. We put the beaker back on the hotplate, keeping a close watch on the thermometer and adjusting the settings of the hot plate only slightly to keep the temperature as close to 70 degrees Celsius as possible. This step certainly made us aware of how much of this process would have depended on experience and intuition in the early modern period, without the availability of precise temperature-measuring devices like thermometers. We found it conceivable that a practitioner performing this dye extraction process would heat the solution at around this temperature, but with no real way to know that he or she was keeping the solution exactly at 70 degrees Celsius.
While the dye was extracting, we measured out and weighed 3 grams of potash alum and 1.2 grams of potash on a scale. Once we had been extracting dye at approximately 70 degrees Celsius for 30 minutes, we removed the beaker from the hotplate and set it on the counter, then removed the polyester bag from the solution. Charles wrung the liquid out of the bag using a spook and fork, compressing it to ensure that as much as liquid as possible remained in the beaker, then set the bag aside on a ceramic plate.
We decided not to filter the hot solution before adding the potash alum to it, to see if this might alter the results (particularly the color) compared to the work of our classmates, who were filtering before adding the potash alum. We then added 3 grams of potash alum to the solution and put the beaker back onto the hotplate, to heat the solution to 80 degrees Celsius. During the course of both heating processes, the dyestuff solution emitted a distinct smokey fragrance, earthy and almost smelling of tobacco.
While the solution was being heated, we prepared a solution of 1.2 grams of potash and 120 mL of water in a 600 mL glass beaker. Once the dyestuff solution was at 80 degrees Celsius, we removed it from the hotplate and set it on the counter. We then began to add the dyestuff solution to the alkaline solution (of distilled water and potash) slowly, while stirring constantly with a chopstick. We watched as the dyestuff solution reacted with the alkaline solution, creating a red foam filled with bubbles on the surface of the substance. We kept stirring to help the reaction along. The goal was to get the substance to the point where a reaction was no longer occurring, meaning that bubbles would no longer form on the foam.
Once it seemed that the bubbling had stopped and the solution was no longer undergoing a chemical reaction, we tested the pH. Because we mixed an alkaline solution with an acidic solution, we expected the new solution to have a pH of about 6. We tested the solution first with a basic pH strip, which indicated a pH of about 7. We stirred the solution a bit more and tested it again with a pH strip, this time getting a read of about 8.
We decided to try a more precise pH strip to get a more accurate read of the pH, since we did expect it to be a bit more neutral than at a pH of 8. We used 4-color pH strips and this time got a clear read of 7.
Satisfied with this read, we covered the glass beaker with a parafilm and left it to settle overnight.
Name: Isabella Lores-Chavez and Charles Kang
Date and Time:
2016.10.28, 11:45 am-1:45 pm
Location: LabSubject: Filtering red madder pigment
The next stage of making red madder lake involved filtering and washing the pigment.
First, we set up a filtering system: we placed a paper coffee filter in a funnel, and set the funnel over a glass mason jar. We removed the parafilm from our glass beaker containing the neutralized dyestuff solution and gradually poured the solution directly into the funnel. We then waited as the liquid filtered through the coffee filter paper, leaving behind blood-red pigment on the filter paper. At first, the liquid poured quickly through the
This process was extremely lengthy, much more so than we expected. The liquid filtered through the coffee filter and funnel very, very slowly, probably because the accumulation of pigment was significant. So much red matter (madder?) sat on the filter paper that the liquid had very little porous material through which to pass. It dripped into the mason jar drop by drop for almost an hour and a half. We periodically used a chopstick to move the pigment particles around and create spaces for the liquid to pass through, but even this didn't help the filtrate drip into the mason jar much faster.
Finally, at around 1:25 pm, we determined that enough of the filtrate has passed through the filter to move on to the next step: washing. We threw out the red filtrate and re-set the filter and funnel on the glass mason jar. We then poured distilled water into the funnel, enough to cover all red particles. As the filtrate of this wash slowly began to drip into the mason jar, we saw that it was relatively clear, with only a tinge of red. With Joel's consultation, we determined that this filtrate was clear enough to suffice as a wash for the pigment. We covered the funnel with plastic wrap and left the labeled mason jar and funnel sitting on the counter, expecting the wash to be completed by the time we returned to the lab on Monday.
Name: Isabella Lores-Chavez and Charles Kang
Date and Time:
2016.10.31, 12:40-2:00 pm
Location: LabSubject: Painting out red madder lake
After leaving the red madder pigment washing and drying over the course of the weekend, we returned to the lab on Monday to paint it out with egg white and egg yolk. As a class, we collectively determined that we should paint out using egg and not oil because all the red madder pigments were still too damp to mix with oil.
For a full account of painting out with egg whites and egg yolks, please see Charles Kang's field notes. All our paint samples were a very dark red, a kind of maroon, almost brown. Our most beautiful paint sample, with pigment properly ground into the medium, came from mixing the red madder lake with egg white and egg yolk. It resulted in the smoothest paint, relatively easy to manipulate and set down, and with the slickest surface qualities.
