On Saturday April 6, 2013 I made four different inks. On April 13, 2013 I entered each of those inks into the South Oaken Arts and Sciences Fair along with the write up documentation of what I did, how I did it and background information. The entry took first place.
In this post you will find the seven (7) pages of documentation for the entry and the accompanying 6 pages of appendixes. If you are one of the followers of my blog, some of this information will be known to you, though how it all ties together will be more certain. Some of the information will be entirely new. I hope you enjoy this lay person’s approach to medieval Iron Gall Ink making.
PLEASE COMMENT OR ASK QUESTIONS, as it helps me to become better at my ink making and my other scribal endeavors as well.
Copyright 2013, David Roland. All rights reserved. Permission to use in part or whole is granted to any participant of the Society for Creative Anachronism as long as proper source citation and attribution is given to me and this documentation. If you wish a copy of the documentation in a word document form please feel free to contact me.
Oak Gall Inks
“What an astonishing thing a book is. It’s a flat object made from a tree with flexible parts which are imprinted with funny dark squiggles. But one glance at it and you’re inside the mind of another person, maybe somebody dead for a thousand years. Across the millennia an author is speaking clearly and silently inside your head directly to you. Writing is perhaps the greatest of human inventions, binding people together who never knew each other, citizens of different epochs. Books break the shackles of time. Books are proof that humans are capable of working magic.” ~ Carl Sagan
Join me for a moment in a thought experiment. Think of all the court scrolls you have seen. All the books you have read. All medieval manuscripts in the world. Have that picture in your mind? Now in your mind erase every last bit of ink from them all. Did your heart stop just a bit? Such is the importance of ink. The loss of all that knowledge would be devastating.
For thousands of years ink of one kind or another has been used to pass on knowledge. Stored knowledge is what lets us know about the past. The different ways to make ink to store knowledge is an ongoing and historical masterpiece of creativity. Even today we have different inks for ink jet printer, laser printers, magazines, newspapers, books, ball point pens, fountain pens and much, much more.
What was the ink that was most widely used and important in the western world for the longest period of time? “Iron gall ink is arguably the most important ink in Western history. It was known by the Romans and became widely used after the late Middle Ages.” Ink is an amazing liquid that has the almost magical ability to store and transfer the most ephemeral of all things, thoughts.
For this entry I made 4 different iron gall inks that could have been made inside the SCA time period. I used distilled water, Aleppo oak galls, copperas, raw vinegar, logwood and gum arabic as my ingredient list.
– Ink 1 is made of distilled water, oak gall extract, copperas and gum arabic
– Ink 2 is made of distilled water, oak gall extract, raw vinegar, copperas and gum arabic
– Ink 3 is made of distilled water, oak gall extract, copperas, logwood and gum arabic
– Ink 4 is made of distilled water, oak gall extract, raw vinegar, copperas, logwood and gum arabic
Materials and Components
Distilled water is purified by steaming the water and collecting the condensed water vapor. In period recipes we see that the directions call for the use of rain water, clear running water and in general description of the purest water one might be able to obtain. Well water was not always trustworthy due to various chemical that might exist in it.
I used distilled water to simulate pure water in period.
Aleppo oak galls are known by a variety of names and were known and used since ancient Greek times.
“The most important of the insect galls is the Aleppo gall. Also known as Turkey gall, Levant gall, gall-nut, gall of commerce and ink marble, they have a spherical shape, are hard and brittle, about the size of a wild hickory nut, and appear on the stems and branches of Quercus aegilops, Q. infectoria, Q. pendiculata and other oaks. The gall is produced by a wasp of the family Cynipidae (Cynips tinctoria), which is found in eastern Europe and the Near East, including portions of Greece, Hungary, Iraq and Turkey. This gall has been of commercial importance since the time of Ancient Greece and has been used for a variety of purposes [Fagan, 1918; Felt, 1940″].
One can extract tannic acid and gallic acid from Aleppo oak galls. Aleppo oak galls are 65% tannic acid and 2% gallic acid along with other ingredients.
Copperas is a bluish green crystal used over and over in various period recipes. Ferrous Sulfate Heptahydrate is Fe(II) SO4 + 7 H2O is a greenish crystal form. I used this form of copperas in my ink as it is the period form.
Copperas, much like today, was commercially and industrially made. The Tankerton Copperas Works, a late 16th and early 17th century English copperas manufacturing site, was discovered in 1995. This highly capitalized industrial manufacture of copperas is called by some “The Forgotten Chemical Revolution” that was the beginning of the Industrial Revolution. It was also collected in mines and worked in places such as in Goslar, Germany.
“Vitriol was obtained from different mines and obtained by various techniques. In Goslar, Germany, a large concentration of natural vitriol supplied much of Middle Europe. Fluid was collected in large iron pans as it trickled out of the rock in mine shafts. Crystallized salts would form after the water had evaporated. The fluid was also collected in barrels, and vitriol crystals developed on a rope hung into the barrel as the fluid evaporated. To increase the iron sulfate content, scrap iron was added to the solution. Iron sulfate could also be obtained as a by product from alum manufacturing. The primary contaminant in this salt solution would be aluminum.”
Gum arabic is also called chaar gund, gum acacia, meska, or char goond. It is the sap from the Acaccia Senegal tree. The purpose of gum arabic is as a thickener and binder for the ink. For those scientifically minded see Appendix A Figure B.
Gum arabic is found in many period recipes as the binder to hold the ink solution to the writing surface. Other binders that could have been used were fish glue and glair with perhaps a touch of honey. These binders seem to be too hard and inflexible even with the honey additive. When Gum arabic became available through trade routes to the middle east it quickly became the favored binder for ink. In period recipes you will see it called gum, gum arabicke, gomme and other such phonetic derivatives.
Raw vinegar is also an ingredient found in some ink recipes. Modern vinegar is made up of pasteurized and purified acetic acid and water. In period there wasn’t a process of pasteurization and thus was raw vinegar. Pasteurization kills microbes including the yeasts that made the vinegar and molds that may be present as well.
I haven’t tested to see what differences using raw verses pasteurized vinegar would make for the ink. However, raw vinegar is far more period than the modern vinegars would be. Research has shown that adding vinegar during the boiling process can help pull out more of the acids in the oak galls. “Boiling crushed or ground galls in water (wine, beer, etc.) extracted most of the gallotannic acid and gallic acid from the galls. Addition of an acid (vinegar, hydrochloric acid) also serves to increase the percentage of the gallic acid.”
I obtained the raw vinegar from a merchant at a farmer’s market.
Logwood is a coloring additive to the ink and is found in a few recipes that I have come across. When logwood comes in contact with iron it turns black. Logically this seems like it would be a good additive to put in iron gall ink. As it turns out even in period it was known to cause the ink to fade. Fugitive inks and pigments are ones that are not colorfast and are said to be fugacious in character. The use of logwood in ink was banned in period in some places. “In 1581 the Parliament prohibited its use ‘because the colours produced from it were of a fugacious character.'” Even in modern times, testing has shown that the use of logwood in iron gall inks creates an inferior ink to pure iron gall inks. “It was shown that no gall and logwood ink was equal to the pure gall ink in so far as durability in the writings was concerned. All such inks were exhibited which, though durable before the addition of logwood, faded rapidly after logwood was added to them.”
Another problem with logwood is that it remains soluble in water after drying. Iron gall pigment on the other hand does not. So, adding logwood makes it easier to remove the ink without being detected, making forgery of documents much easier. So, why use it?
Iron gall ink doesn’t always turn completely black until it comes in contact with the oxygen. This process of oxidation can be slow but it makes the ink very permanent. If the ink goes on in a translucent manner, knowing exactly where to put your next pen stroke can be problematic. The additive of logwood causes the ink to be black in the bottle before the oxidation process occurs. This process can make writing much easier. So, it makes some sense to add the logwood if you don’t care if the writing will fade or you aren’t worried about forgery.
“Nobody makes the same tomato soup.”
The recipes I followed are ones of my making based off of my research of many period recipes for iron gall ink. The components can all be found in iron gall recipes from inside the SCA time period. I synthesized what I knew of those recipes and put them together in a logical way that could have been used in period but I have never seen in any of the recipes. I created four recipes for iron gall ink in this fashion that are intended to test each ink in a comparative manner to each of the other inks.
I boiled three ounces Aleppo oak galls for 20 minutes in two separate pots each. In the first pot I only had water. In the second pot I added the raw vinegar. Many recipes call for the water and (if present) vinegar to be boiled. As the pots were heating up I used a mortar and pestle and broke the oak galls.
While the galls were boiling I retrieved 4 baby food glass jars and labeled them. In jars 3 and 4 I put ¼ teaspoon of logwood into the bottom.
After boiling the oak galls for 20 minutes I strained out the large pieces of oak galls using linen fabric. I then added 1.5 oz of copperas to each pot and stirred. This caused a chemical reaction turning the solution black.
In jars 1 and 3 I put roughly 4 fluid oz of ink from the water only pot. In jars 2 and 4 I put roughly 4 fluid oz of ink from the water and vinegar pot. I then added a tsp of gum arabic to each jar.
The recipes I followed are ones of my making based off of my research of many period recipes for iron gall ink. The components would all be found in various iron gall recipes from inside the SCA time period.
This process seems simple enough but the order of operations is very important and being creative about the process helps. Previous experiments of mine have shown that putting in the logwood before the copperas interacts with the oak gall extract will create a weak colored ink and causes and unknown precipitate to occur. Adding in gum arabic during the boiling process literally gums up the works and seems to slow the chemical reactions between the oak gall extract and the copperas and the logwood. Adding in the vinegar after boiling the oak galls seems to defeat the purpose of the vinegar being there to help extract even more tannic and gallic acid from the oak galls.
Each ink was then tested on sheep parchment, deer parchment and Bristol vellum paper. Each had its own section labeled with the number on the bottle. For the parchments each ink was tested on the flesh and the hair sides. The different surfaces were used as a way to observe if one ink recipe was superior on any given surface and if any ink recipe was superior an all the surfaces.
I cured and cut 4 goose quills, one for each distinct bottle of ink. I marked the quill with the number of the bottle it was paired with. After placing the writing surface on a 45 degree angle scribal desk, I used the quills to write a series of test marks on the writing surface. The human eye can be easily fooled by the forms in letters making one perceive something as darker or lighter than it may actually be. The purpose of the test marks was to use pen strokes that are used in writing calligraphy but not to distract the comparison of the ink color by actually using calligraphy.
Each writing surface being quartered this created 20 distinct data points for the project. Each comparable to the other data points creating potentially 400 cross references.
I am very happy with the results of this project. I created four separate ink recipes each of which could have been found in period, using only materials that could have been used in period putting them together in my own creative fashion. Each ink writes very well and could stand on its own for use in any period scribal project. Having created an easy to use visual reference for 20 data points shows each ink has its own visual properties that are in fact somewhat dependent on the surface they are written upon.
INK MAKING APPENDIX A
Table 9.3 Chemical content of the Aleppo gall
|Ellagic acid and luteo-gallic acid||2.0|
|Chlorophyll and volatile oil||0.7|
|Brown extractive matter||2.5|
|Gallate and Oxalate of lime|
Source: Food and Agriculture Organization of the United Nations (FAO) Corporate Document Repository. http://www.fao.org/docrep/005/y4351e/y4351e0d.htm “Non-wood forest products from temperate broad-leaved trees” Chapter 9.
Gum arabic is “believed to be a branched polymer of galactose, rhamnose, arabinose, and glucuronic acid as the calcium, magnesium, and potassium salts with a mol. wt. of approx. 250,000”
Tea Tannins vs Tannic Acid
There seems to be much confusion about Tea Tannins and Tannic Acid; they are NOT the same. Tannic Acid is found in, for example, Oak leaves and, originally, was extracted to perform the task of tanning leather. Tea Tannins will not tan leather.
The formula for Tannic Acid (Acidum Tannicum) is: C14 H10 O9
The formula for Tea Tannins is: C20 H20 O9
“Logwood, employed more extensively for “added” color than any other color compound, was introduced into Europe by the Spaniards, A. D. 1502. In England it does not appear to have been much used until about 1575.
In 1581 the Parliament prohibited its use “because the colours produced from it were of a fugacious character.” Its use was legalized in 1673 by an act, the preamble of which reads, “The ingenious industry of modern times hath taught the dyers of England the art of fixing, the colours made of logwood, alias blackwood, so as that, by experience, they are found as lasting as the colours made with any sort of dyeing wood whatever.”
It is obtained principally from the Campeachy tree, which grows in the West Indies andSouth America. The practical utility of logwood as the base for an ink was a discovery of Runge in 1848, who found that a dilute solution of its coloring matter, to which had been added a small quantity of neutral chromate of potassium, produced a deep black liquid which apparently remained clear and did not deposit any sediment. This composition became very popular on account of its cheapness and dark purple color. It is of a fugitive character, though, and has passed almost entirely out of commercial use.”
Forty Centuries of Ink by David N. Carvalho. Pg 88
“From their high price, however, and that of galls generally, sumach, logwood, and even oak bark are too frequently substituted in the manufacture of inks, but it need scarcely be said always injuriously.”
Forty Centuries of Ink by David N. Carvalho. Pg 90
Period Iron Gall Ink Recipes
A Booke of Secrets showing diverse ways to make ink – 1596
To make Inke to write vpon paper.
Take halfe a pint of water, a pint wanting a quarter of wine, and as much vineger, which being mixed together make a quart & a quarter of a pint more, then take six ounces of gauls beaten into small pouder, and sifted through a siue, put this pouder into a pot by it selfe, and poure halfe the water, wine, and vineger into it, take likewise foure ounces of victriall, and beat it into pouder, and put it also in a pot by it selfe, whereinto put a quarter of the wine, water, & vineger that remaineth, and to the other quarter, put foure ounces of gum Arabike beaten to pouder, that done, couer the three pots close, and let them stand three or foure daies together, stirring them euery day three or foure times, on the first day set the pot with gaules on the fire, and when it begins to seeth, stir it about till it be throughly warme, then straine it through a cloath into another pot, and mixe it with the other two pots, stirring them well together, and being couered, then let it stand three daies, till thou meanest to vse it, on the fourth day, when it is setled, poure it out, and it wil be good inke. If there remaine any dregs behind, poure some raine water (that hath stand long in a tub or vessell) into it, for the older the water is, the better it is, and keepe that vntill you make more inke, so it is better then clean water.To make Inke for parchment. Make it in all points like to the inke aforesaid, only take a pint of water, & of vineger and wine a pint more, that is of each halfe a pint.
Another sort of Inke.
Take a quart of cleare water, and put it in a glasse, put into it thirteene ounces beaten victriall, let it stand three daies, and stir it three or foure times euery day, then take thirteene ounces of beaten gaules, and put them into a new earthen pot that is wel leaded, poure into them a quart of cleane water, that done, set it on the fire, and let it seeth till it consumeth about a finger deepe, but suffer it not to seeth so fast that it seeth ouer the pots brim, then strain it through a wollen cloath, into another pot, that is leaded, poure into the cloath a cup full of good vineger, and strain it through likewise, that done, if there remaineth any thing in the cloath, cast it away, then put into the matter, foure or fiue ounces of beaten gum and stir them well together, then againe straine them through a cleane wollen cloath, and poure into it a cup full of good vineger, and straine it through the cloath, and let it stand till it be coole, then put it into a straightnecked glasse, stop both the glasses well, till you haue occasion to vse them, then take of each water a little quantitie, and mix them together, so haue you good inke.
Another of the same sort, but easie to make.
Take the beaten gauls, and put them in the water doe the like with the victriall in a pot by it self let those two waters stand, and when you haue cause to vse inke, poure out of each pot a like quantitie, and it will be blacke, then put into it a little beaten gum, & it will bee good inke.
Take a quart of strong wine, put it into a new pot, and set it on a soft fire till it be hote, but let it not seeth, then put into it foure ounces of gauls, two ounces and a halfe of gum Arabike, and two ounces of victriall, al beaten into smal pouder, and sifted through a siue, stirre it with a wooden sticke, and it will be good inke.Another.
Take an ounce of beaten gaule, three or foure ounces of gum Arabicke, put them together in a pot with raine water, and when the gum is almost consumed, strain it through a cloath, and put into it almost halfe a cup of victriall beaten to pouder.
Take a pint of beere, put into it an ounce of gaules beaten to pouder, let it seeth till it seeme somewhat red, then put to it three quarters of an ounce of greene victriall, in small pouder, and let it seeth againe, when you take it off the fire, cast into it three quarters of an ounce of gum, and a small peece of alum, both in pouder, and stir them all together till it be cold.
Take two handfulls of gauls, cut each gaule either into three or four peeces, poure into them a pint of beere or wine, (which you wil) then let it stand eight houres, straine it from the gaules, and put victriall therein, and to the victriall a third part of gum, set it on the fire to warm, but let it not seeth, and it will bee good inke: and of those gaules you may make inke foure or fiue times more.
A Book Containing Divers Sorts of Hands, by
John de Beau Chesne and M. John Baildon, and published in 1571.
“To make common yncke of Wyne take a quart,
Two ounces of gomme, let that be a parte,
Five ounces of galles, of copres take three,
Long standing dooth make it better to be;
If wyne ye do want, rayne water is best,
And as much stuffe as above at the least:
If yncke be to thick, put vinegar in,
For water dooth make the colour more dimme.
In hast for a shift when ye have a great nead,
Take woll, or wollen to stand you in steede;
which burnt in the fire the powder bette small
With vinegre, or water make yncke with all.
If yncke ye desire to keep long in store
Put bay salte therein, and it will not hoare.
Of that common yncke be not to your minde
Some lampblack thereto with gomme water grinde”
PROBABLY XIIth CENTURY
Chapter 38. Ink
When you are going to make ink, cut some pieces of [haw]thorn wood in April or in May, before they grow blossoms or leaves. Make little bundles of them and let them lie in the shade for two, three, or four weeks, until they are dried out a little. Then you should have wooden mallets with which you should pound the thorn on another hard piece of wood, until you have completely removed the bark.
Put this immediately into a barrel full of water. Fill two, three, four, or five barrels with bark and water and so let them stand for eight days, until the water absorbs all the sap of the bark into itself. Next, pour this water into a very clean pan or cauldron, put fire under it and boil it. From time to time also put some of the bark itself into the pan so that, if any sap has remained in it, it will be boiled out. After boiling it a little, take out the bark and again put more in. After this is done, boil the remaining water down to a third, take it out of that pan and put it into a smaller one. Boil it until it grows black and is beginning to thicken, being absolutely careful not to add any water except that which is mixed with sap. When you see it begin to thicken, add a third part of pure wine, put it into two or three new pots, and continue boiling it until you see that it forms a sort of skin on top.
Then take the pots off the fire and put them in the sun until the black ink purges itself from the red dregs. Next, take some small, carefully sewn parchment bags with bladders inside, pour the pure ink into them, and hang them in the sun until [the ink] is completely dry. Whenever you want, take some of the dry material, temper it with wine over the fire, add a little green vitriol and write. If it happens through carelessness that the ink is not black enough, take a piece of iron a finger thick, put it into the fire, let it get red-hot, and immediately throw it into the ink.
Incaustum etiam facturus incide tibi ligna spinarum, in Aprili siue in Maio prius quam producant flores aut folia, et congregans inde fasciculos sine iacere in umbra duabus hebdomadibus uel tribus aut quatuor, donec aliquantulum exsiccentur.
Deinde habeas malleos ligneos, cum quibus super aliud lignum durum contundas ipsas spinas, donec corticem omnino euellas, quem statim mittes in dolium aqua plenum; cumque duo dolia uel tries seu quatuor aut quinque cortice et aqua repleueris, sine sic stare per octo dies, donec aqua omnem corticis sucum in se emordeat. Post haec mitte ipsam aquam in cacabum mundissimum uel in lebetem, et supposito igne coque; interdum etiam immitte de ipso cortice in cacabum, ut si quid suci in eo remansit, excoquatur; quam cum modice coxeris, eice, aliumque rursus immitte. Quo facto coque residuam aquam usque ad tertiam partem sicque eiciens de ipso cacabo mitte in minorem et tamdiu coque, donec nigrescat atque incipiat densescere, hoc omnino cauens ne aliquod addas aquae, excepta illa quae suco mixta est; cumque uideris eam densescere, adde uini puri tertiam partem, et mittens in ollas nouas duas uel tres, tamdiu coque, donec uideas quod in supremo quasi cutem trahat.
Deinde tollens ipsas ollas ab igne, pone ad solem, donec se nigrum incaustum a rubea faece purificet. Postea tolle folliculos ex pergameno diligenter consutos ac uesicas, et infundens purum incaustum suspende ad solem, donec omnino siccetur; cumque siccum fuerit, tolle inde quotiens uolueris et tempera cum uino super carbones, et addens modicum atramenti scribe. Quod si contigerit per negligentiam, ut non satis nigrum sit incaustum, accipe ferrum grossitudine unius digiti, et ponens in ignem sine candescere, moxque in incaustum proice.
This recipe was taken from Theophilus, On Divers Arts. Theoremost Medieval Treatise on Painting, Glassmaking and Metalwork, Translated from the Latin with Introduction and Notes by John G. Hawthorne and Cyril Stanley Smith, Dover Publications Inc., New York, 1979, p. 42.
The Latin version was taken from Monique Zerdoun Bat-Yehouda, Les encres noires au Moyen Âge (jusqu’à 1600), Éditions du CNRS, Paris, 1983, p. 156.
Medieval Manuscripts some Ink and Pigment Recipes
This booklet of ink and pigment recipes was compiled by the Special Collections Conservation Unit of the Preservation Department of Yale University Library.
Allen, Tim. The Forgotten Chemical Revolution. British Archaeology. Aug. 2002 <http://www.archaeologyuk.org/ba/ba66/feat2.shtml>.
Carvalho, D. N. Forty centuries of ink: a chronological narrative concerning ink and its backgrounds. New York: The Bank Law Publishing Co., 1904. Project Gutenburg EText. October, 1998 [Etext #1483]
“CHAPTER 9.” FAO: Food and Agriculture Organization of the United Nations, for a world without hunger. N.p., n.d. Web. 8 Apr. 2013. <http://www.fao.org/docrep/005/y4351e/y4350>.
De Beau Chesne, John, and M. John Baildon. A Book Containing Divers Sorts of Hands. 1571. Print.
De Hamel, Christopher. Medieval Craftsman Scribes and Illuminators. 1992. Toronto, Buffalo: Trustees of the BritishMuseum, University of Toronto, 2009. Print.
Iron Gall Ink Website. <http://www.irongallink.org/>.
Lindquist, Evan. Old Ink Recipes. <http://www.evanlindquist.com/oldinkrecipes.html>.
Special Collections Conservation Unit of the Preservation Department of YaleUniversity Library. Medieval Manuscripts some Ink and Pigment Recipes.
The Iron Gall Ink Corrosion Website <http://www.knaw.nl/ecpa/ink/>. [13-09-1999 16:46:52]
The Tea Man.19 Feb 2011. <http://www.teatalk.com/science/tannin.htm>.
White, Edward. A Book of Secrets, showing diverse ways to make and prepare all sorts of ink and colors. Trans. W.P London. Adam Islip, 1596. Print.
 See Appendix B Period Iron Gall Ink Recipes
 Food and Agriculture Organization of the United Nations (FAO) Corporate Document Repository. http://www.fao.org/docrep/005/y4351e/y4351e0d.htm “Non-wood forest products from temperate broad-leaved trees” Chapter 9
 SEE FIGURE A in APPENDIX A
 See Appendix B Period Iron Gall Ink Recipes
 Carvalho, D. N.. “Forty centuries of ink: a chronological narrative concerning ink and its backgrounds..” New York: The Bank Law Publishing Co ;, 1904. Project Guttenburg EText. October, 1998 [Etext #1483] pg 88
 Ibid Pg 68
 The Iron Gall Ink Corrosion Website http://www.knaw.nl/ecpa/ink/ [13-09-199916:46:52] “An introduction to the interpretation of historical ink recipes” Ad Stijnman, The Netherlands Institute of Cultural Heritage (ICN), Amsterdam
 See Appendix B Period Iron Gall Ink Recipes