MAKING LAKE PIGMENT WITH MADDER: A HISTORICAL RECONSTRUCTION

The Making and Knowing Project, Columbia University
Last updated 2022-01-29 by NJR

As summarized in Activity Sheet: Making Lake Pigment with Madder, there are three historical recipe types for making lake pigment from madder. In Spring 2022, Naomi Rosenkranz and Charlotte Atkins undertook all three versions at once to make direct comparisons between them. Their field notes, working from the activity sheet, are presented below with extensive images of the process. They show the Making and Knowing Project’s method for reconstruction of the process of lake pigment making from madder roots in the M&K lab.

Refer to:

The recipes provided here are adapted from the ones provided in Jo Kirby et al, Natural Colorants for Dyeing and Lake Pigments: Practical Recipes and their Historical Sources (Archetype, London, 2014).

Modernized recipes, adapted for the laboratory (or kitchen)

From the late 14th century to the 17th century, madder lakes seem to be most commonly extracted from madder-dyed wool and not the roots (raw dyestuffs). Recipes from before (antiquity) and after (18th and 19th centuries) tend to extract from the roots directly. Thus, the modern recipes adapted here are from this later period.

There are three modernized versions of the historical recipes:

  1. “Standard” - [Code: ML-Std in Natural Colorants]

    1. Extract madder in water, then add alum, precipitation of pigment with potash

  2. “Standard Reversed” - [Code: ML-EBAl in Natural Colorants]

    1. Extract madder in water, then add potash, precipitation of pigment with alum

    2. Color is said to be a very slightly redder, less brown than Standard

  3. “Standard with Alum Extraction” - [Code: ML-Std in Natural Colorants]

    1. Extraction of madder in alum, precipitation of pigment with potash

    2. Color is said to be a brighter red than Standard

RECIPE 1: “Standard”

Materials and Equipment (Recipe 1)

  • Mortar & pestle
  • Hot plate
  • 2 Beakers (at least 600ml)
  • Pair of chopsticks or other stirring device
  • Thermometer
  • Funnel
  • Filter (such as a basket coffee filter) or filter paper
  • pH strips
  • 300ml Water - for madder
  • 50ml Water - for alum
  • Drawstring bag (muslin or polyester netting is best)
  • 10g Madder roots (the Making and Knowing Project typically sources this from Kremer Pigments, Kremer #37201-madder-roots)
  • 5g Alum (aluminum potassium sulfate, Kremer #64100-potash-alum)
  • 1.88g Potash (potassium carbonate, Kremer #64040-potash)

Procedure (Recipe 1)

  • Coarsely grind madder roots in mortar and pestle
  • Using a small utensil, add madder to the drawstring bag. Close the bag tightly, but make sure there is enough room in the bag for the madder to move around freely. Use multiple bags if necessary

Ground powder in bag on scale that reads 512g

Ground powder in bag on scale that reads 493g

Drawstring bag in beaker labeled Standard 1

  • Add 300ml water and bag of madder to 600ml beaker and leave to soak overnight
    • NOTE: soaking overnight can be skipped for time constraints, but the amount of colorant extracted will be affected, possibly changing the the final pigment

Madder bag soaking in beaker filled halfway with water and labeled Standard 1, beaker is on scale that reads 298.96g

  • After soaking overnight (if doing so), add alum and heat the madder+water+alum to 70°

Beaker labeled Standard 1 is on the stovetop, still has madder bag inside

Beaker labeled Standard 1 is on the stovetop, still has madder bag inside, thermometer shows temperature at 73 degrees F

  • Keep at this temperature for 30 minutes to extract the dye
  • Remove the drawstring bag, which can now be discarded

Hand removes bag from Standard 1 beaker

  • Add 5g alum to the solution and bring to 80°

Small cup containing white grainy substance is held near Standard 1 beaker

Standard 1 beaker on heat, small cup nearby is now empty

  • In the other 600ml beaker, dissolve 1.88g potash in 50ml water over heat

Beaker containing potash and water is on scale showing 52.08g

Two beakers on stovetop, left labeled Standard Potash and Water and right labeled Standard 1 and Alum

  • Pour the madder+alum solution into the potash solution VERY GRADUALLY and STIRRING CONSTANTLY
    • Do this slowly and incrementally, checking the pH of the solution after each addition until a pH of 6-7, there is no further effervescence, and precipitation of the lake pigment appears to be complete

Reddish liquid in one beaker is poured into another, the contents of which are also reddish

Beaker labeled Standard Potash and Water is full to around 125ml with red liquid and to around 550ml with pink foam

Video of a hand using a stick to vigorously stir the contents of the Standard Potash and Water beaker

Overhead shot of Standard Potash and Water beaker, which is full of reddish liquid and pinkish foam

Standard Potash and Water beaker full to about 325ml with reddish liquid and 500ml with pinkish foam

Used pH strip lying next to pH color chart, strip color not discernable

Used pH strip lying next to pH color chart and strip color mark, color mark is greenish and labeled 6-7

  • Allow the solution to settle for at least 15min (ideally overnight)

Overhead shot of Standard Potash and Water beaker with much less foam than in last picture

Standard Potash and Water beaker full to about 325ml with reddish liquid with hardly any pinkish foam atop

  • Pour solution through filter in a funnel

Funnel containing filter is positioned over an empty glass jar labeled Standard Madder Lake

Reddish contents of Standard Potash and Water beaker are poured into the funnel’s filter

Overhead shot of reddish liquid draining in filter

Reddish liquid drained through filter into Standard Madder Lake jar

Overhead shot of reddish liquid draining in filter, now less full

Reddish liquid drained through filter into Standard Madder Lake jar, now more full

  • Once the liquid has drained through, wash the pigment: discard the filtrate and place funnel+filter over a clean container. Pour 100ml of clean water through the filter. Repeat until the filtrate is clear

Reddish liquid drained through filter into Standard Madder Lake jar, now much more full

Overhead shot of dried and cracked pigment on filter

Overhead shot of hand holding WASH 1 sign next to wet pigment in wet filter

Hand holds WASH 1 sign next to glass jar filled with clear water, atop which are the funnel and the filter

Overhead shot of hand holding WASH 2 sign next to wet pigment in wet filter

Hand holds WASH 2 sign next to glass jar filled with clear water, atop which are the funnel and the filter

Overhead shot of dried reddish pigment in the aftermath of second wash

Standard Madder Lake jar is now more full of filtered water

  • Allow the pigment to dry on the filter (at least overnight), then scrape off and use

Filter is inside plastic bag labeled Standard Madder Lake

Dry filter containing reddish pigment

Zoomed-in photo of dry filter containing reddish pigment

Reddish pigment from filter is removed and now on paper

Leftover filter with pigment removed

Pigment in vial

RECIPE 2: “Standard Reversed”

Materials and Equipment (Recipe 2)

  • Mortar & pestle
  • Hot plate
  • 1 Beaker (at least 600ml)
  • 1 Beaker (at least 100ml)
  • Pair of chopsticks or other stirring device
  • Thermometer
  • Funnel
  • Filter (such as a basket coffee filter) or filter paper
  • pH strips
  • 300ml - Water for madder
  • 30ml - Water for alum
  • Drawstring bag (muslin or polyester netting is best)
  • 10g Madder roots (the Making and Knowing Project typically sources this from Kremer Pigments, Kremer #37201-madder-roots)
  • 5g Alum (aluminum potassium sulfate, Kremer #64100-potash-alum)
  • 1.88g Potash (potassium carbonate, Kremer #64040-potash)

Procedure (Recipe 2)

  • Coarsely grind madder roots in mortar and pestle
  • Using a small utensil, add madder to the drawstring bag. Close the bag tightly, but make sure there is enough room in the bag for the madder to move around freely. Use multiple bags if necessary

Ground powder in bag on scale that reads 506g

Ground powder in bag on scale that reads 511g

Drawstring bag in beaker labeled Standard 2

  • Add 300ml water and bag of madder to 600ml beaker and leave to soak overnight
    • NOTE: soaking overnight can be skipped for time constraints, but the amount of colorant extracted will be affected, possibly changing the the final pigment

Madder bag soaking in beaker filled halfway with water and labeled Standard Reversed 2, beaker is on scale that reads 304.47g

  • After soaking overnight (if doing so), heat the madder+water to 70°

Beaker labeled Standard Reversed 2 is on the stovetop, still has madder bag inside

  • Keep at this temperature for 30 minutes to extract the dye
  • Remove the drawstring bag, which can now be discarded

Hand removes bag from Standard Reversed 2 beaker

Standard Reversed 2 beaker is on stovetop, halfway full of reddish liquid and no drawstring bag

  • Add 1.88g potash to the solution and bring to 80°

Standard Reversed 2 and Potash beaker is on stovetop, is full to about 300ml with reddish liquid

Overhead shot of Standard Reversed 2 and Potash beaker, which contains reddish liquid and no foam

  • In the 100ml beaker, dissolve 5g alum in 30ml water over heat

Beaker labeled 2 Standard Reverse Alum and Water is on scale showing 35.55g

Two beakers on stovetop, left labeled 2 Standard Reverse Alum and Water and right labeled Standard Reversed 2 and Potash

  • Pour alum solution into the madder+potash solution VERY GRADUALLY and STIRRING CONSTANTLY
    • Do this slowly and incrementally until there is no further effervescence, and precipitation of the lake pigment appears to be complete. Check the pH of the solution, which should be about 6

Clear liquid in Alum beaker is poured into Standard Reversed 2 and Potash beaker, the contents of which are reddish

Beaker labeled Standard Reversed 2 and Potash is full to around 150ml with red liquid and to around 500ml with pink foam

Hand stirs Standard Reversed 2 and Potash beaker vigorously with stick

Beaker sits on cooling pad, contains mostly reddish liquid and some foam

Used pH strip labeled 5-6

  • Allow the solution to settle for at least 15min (ideally overnight)

Standard Reversed 2 and Potash beaker full to about 290ml with reddish liquid with hardly any pinkish foam atop

  • Pour solution through filter in a funnel

Funnel containing filter is positioned over an empty glass jar labeled 2 Standard Reversed Madder Lake

Reddish contents of Standard Reversed 2 and Potash beaker are poured into the funnel’s filter

Overhead shot of reddish liquid draining in filter

Reddish liquid drained through filter into 2 Standard Reversed Madder Lake jar, now more full

Overhead shot of reddish liquid draining in filter, now less full

  • Once the liquid has drained through, wash the pigment: discard the filtrate and place funnel+filter over a clean container. Pour 100ml of clean water through the filter. Repeat until the filtrate is clear

Reddish liquid drained through filter into 2 Standard Reversed Madder Lake jar, now much more full

Overhead shot of wet reddish pigment on filter

Overhead shot of hand holding WASH 1 sign next to wet pigment in wet filter, which contains some water

Hand holds WASH 1 sign next to glass jar containing a small amount of water, atop which are the funnel and the filter

Overhead shot of hand holding filter in water

WASH 1 label lies next to 2 Standard Reversed Madder Lake jar, which contains a large quantity of yellowish water

Overhead shot of dried reddish pigment in the aftermath of first wash

2 Standard Reversed Madder Lake jar is now more full of filtered water

Overhead shot of filter and funnel filled with water for second wash

WASH 2 sign lies next to 2 Standard Reversed Madder Lake jar, now contining clear water

  • Allow the pigment to dry on the filter (at least overnight), then scrape off and use

Dried 2 Standard Reversed Madder Lake filter dried after second wash

Dried 2 Standard Reversed Madder Lake filter dried after second wash, zoomed in

Dried 2 Standard Reversed Madder Lake removed from filter, small reddish chunks

Filter after reddish pigment chunks have been removed

Dried 2 Standard Reversed Madder Lake reddish pigment chunks in glass vial

RECIPE 3: “Standard with Alum Extraction”

Materials and Equipment (Recipe 3)

  • Mortar & pestle
  • Hot plate
  • 2 Beakers (at least 600ml)
  • Pair of chopsticks or other stirring device
  • Thermometer
  • Funnel
  • Filter (such as a basket coffee filter) or filter paper
  • pH strips
  • 300ml - Water for madder
  • 50ml - Water for potash
  • Drawstring bag (muslin or polyester netting is best)
  • 10g Madder roots (the Making and Knowing Project typically sources this from Kremer Pigments, Kremer #37201-madder-roots)
  • 5g Alum (aluminum potassium sulfate, Kremer #64100-potash-alum)
  • 1.88g Potash (potassium carbonate, Kremer #64040-potash)

Procedure (Recipe 3)

  • Coarsely grind madder roots in mortar and pestle
  • Using a small utensil, add madder to the drawstring bag. Close the bag tightly, but make sure there is enough room in the bag for the madder to move around freely. Use multiple bags if necessary

Ground powder in bag on scale that reads 501g

Ground powder in bag on scale that reads 509g

  • Add 300ml water and bag of madder to 600ml beaker and leave to soak overnight
    • NOTE: soaking overnight can be skipped for time constraints, but the amount of colorant extracted will be affected, possibly changing the the final pigment

Madder bag soaking in beaker filled halfway with water and labeled Standard Alum Extrc 3, beaker is on scale that reads 306.28g

  • After soaking overnight (if doing so), add 5g alum
  • Heat the madder+alum to 70°

Beaker labeled Standard Alum Extrc 3 is on the stovetop, still has madder bag inside

Overhead shot of beaker labeled Standard Alum Extrc 3 on the stovetop, still with madder bag inside

  • Keep at this temperature for 30 minutes to extract the dye

Beaker labeled Standard Alum Extrc 3 on the stovetop, still with madder bag inside and condensation along rim

Standard Alum Extrc 3 beaker is off the heat and on a cooling pad

  • Remove the drawstring bag, which can now be discarded

Hand removes drawstring bag from Standard Alum Extrc 3 beaker

Standard Alum Extrc 3 beaker after drawstring bag removal

  • In the other 600ml beaker, dissolve 1.88g potash in 50ml water over heat

Beaker containing potash and water is on scale showing 51.79g

  • Pour madder+alum solution into the potash solution VERY GRADUALLY and STIRRING CONSTANTLY
    • Do this slowly and incrementally until there is no further effervescence, and precipitation of the lake pigment appears to be complete. Check the pH of the solution, which should be about 6
    • Make sure both solutions are still hot (at least 70-80°) when combined because the dye may begin to precipitate out below this temperature

Reddish liquid in one beaker is poured into another, the contents of which are also reddish

Madder and alum have been completely poured into other beaker, which is full to about 350ml with reddish liquid and some foam

Beaker is full to 350ml with reddish liquid and some foam

Beaker 3 is stirred vigorously with a stick

Beaker 3 still full to 350ml with reddish liquid but with very little foam

Used pH strip lying next to pH color chart and strip color mark, color mark is greenish and labeled 7

  • Allow the solution to settle for at least 15min (ideally overnight)

Beaker 3, labeled Standard Alum Extrac Potash and Water, is still full to 350ml with reddish liquid but now has no foam

  • Pour solution through filter in a funnel

Funnel containing filter is positioned over an empty glass jar labeled Standard Alum Extracted Madder Lake

Overhead shot of reddish liquid draining in filter

Reddish liquid drained through filter into 3 Standard Alum Extracted Madder Lake jar

Overhead shot of reddish liquid draining in filter, now less full

Reddish liquid drained through filter into 3 Standard Alum Extracted Madder Lake jar, now more full

  • Once the liquid has drained through, wash the pigment: discard the filtrate and place funnel+filter over a clean container. Pour 100ml of clean water through the filter. Repeat until the filtrate is clear

Reddish liquid drained through filter into 3 Standard Alum Extracted Madder Lake jar, now much more full

Overhead shot of dried and cracked pigment on filter

Overhead shot of hand holding WASH 1 sign next to wet pigment in wet filter

Hand holds WASH 1 sign next to glass jar filled with clear water, atop which are the funnel and the filter

Overhead shot of hand holding WASH 2 sign next to wet pigment in wet filter

Hand holds WASH 2 sign next to glass jar filled with clear water, atop which are the funnel and the filter

  • Allow the pigment to dry on the filter (at least overnight), then scrape off and use

Dried 3 Standard Alum Extracted Madder Lake filter dried after second wash

Filter is inside plastic bag labeled 3 Standard Alum Extracted Madder Lake

Filter removed from bag, pigment is spilling out

Reddish pigment on paper

Open filter with pigment removed

Reddish pigment in clear vial

On the left lies a plastic bag labeled 3 Standard Alum Extracted Madder Lake Filter Paper containing emptied filter paper, on the right lies a clear vial filled with reddish pigment

A Visual Comparison of Recipes 1, 2, and 3

Heating solutions to extract dye

Three beakers on hotplates, each beaker halfway full of reddish liquid

Solutions after heating for half hour

Three beakers on hotplates, each beaker halfway full of reddish liquid that is now darker in color

Beakers after solutions have been combined and foam has settled

Three labeled beakers after foam has settled

Overhead shot of three labeled beakers after foam has settled

Solutions poured through filters

Three jars with funnels and filters, each draining reddish liquid into the jar below

Overhear shot of three jars with funnels and filters, each draining reddish liquid into the jar below

Three jars with funnels and filters, each containing reddish liquid

Same three jars and filters, now covered in clear wrap

Solutions three days later

Same three jars still covered, now much more full of reddish liquid

Overhead shot of three jars

Three jars now without clear wrap covering

Overhead shot of three jars

Pigments during wash

Three plastic-covered jars with funnels and filters, each jar contains clearish water

Overhead shot of plastic-covered funnels, each containing a used filter full of pigment

Recipes 1 and 3 are shown in wash #2, Recipe 2 is shown in wash #1

Lake Painting

22/04/2022

Comparison of pigments painted with gum arabic

25/04/2022

Comparison of pigments painted with gum arabic, colors have lightened slightly

An Alternative Method To Using Hotplates and Beakers

If you do not have access to hotplates and heat-safe glass beakers, an alternative method uses a water bath or bain-marie (see this cooking blog for more information about bain-maries).

Process

  • On your stove at home, prepare your solutions in mason jars (or other glass jars that can withstand prolonged heating such as pickling or jam jars).
  • Place the jars in a large cooking pot (the pot’s material doesn’t matter – can use steel, ceramic, etc.)
    • NOTE: be careful about using these pots to prepare foods after you have dyed with them if you are working with materials that are not food safe.
    • NOTE: the natural colorants can stain light-colored surfaces, so be careful if using ceramic or glass pots.
  • Fill the pot with enough water to come up past the solutions in your mason jars, being careful not to contaminate the solutions inside your jars
  • Heat the pot on your stove and follow the procedure for preparing lake pigments

Advantages and Notes

  • This is one way to prepare pigments at home without beakers or other shock-resistant containers
  • Beakers, Pyrex, and other borosilicate glass is specially formulated to withstand direct high heat (like when placed directly on a hot plate) as well as shocks or sudden changes in temperature (like placing a hot glass vessel with your bath onto a cold surface like a counter)
  • Regular glass, including mason jars, are not formulated in this way, and so it can be very dangerous (and messy) if used in the same way as beakers – direct high heat or sudden change can cause the glass to shatter
  • This method also allows for easier preparation without a thermometer
  • The temperature of your baths is determined by the temperature of the water in the pot
  • You will know the baths have approximately reached the desired temperature range of 80-100 °C when the water in the pot is beginning to simmer
  • Because water boils and begins to evaporate at 100 °C, your solutions will never exceed 100 °C, the temperature at which the colorants can begin to degrade. This is an easy way to prepare solutions without a thermometer and ensure you are not reaching high temperature levels
  • If the water in the pot begins to boil or simmer violently, your jars will start to shake and move around the pot. If this happens, it is a sign to turn your heat down