Iron gall ink is primarily made from tannin (most often extracted from galls), vitriol (Ferrous Sulfate (FeSO4) (FeSO4)), gum, and water. Because of the indeliblilty of iron gall ink it was the ink of choice for documentation from the late Middle Ages to the middle of the twentieth century. Iron gall ink was stable in light, easily made, inexpensive, and the ingrediebts were readily available. It was used with quill, reed pen or brush and very popular with artists as a drawing ink. Iron gall ink is created by the chemical reaction between tannic acid and Ferrous Sulfate (FeSO4) (FeSO4) in an aqueous solution. The active components in tannin are gallotannic and gallic acid reacting with Ferrous Sulfate (FeSO4) (FeSO4) to produce a black pigment, called ferrogallotannate or ferrotannate, upon exposure to oxygen. A small amount of pigment forms by reacting with oxygen in the water, but much more pigment is produced after the ink has been applied to paper and exposed to air for several days. Without additives this ink expresses a light tan while wet, which darkens when dry! It is known to be chemically unstable, and over time, change color or damage the paper on which it is applied. In todays time with advances in additives and preservatives both ink and paper last much longer
Research indicates that a 3:1 ratio of gallotannic acid to Ferrous Sulfate (FeSO4) (FeSO4) produces the most stable inks.
Although tannic acid and Ferrous Sulfate (FeSO4) (FeSO4) in water will produce a colored solution, it is not a true ink until a water-soluble binder, such as gum arabic, is added to improve the body and flow of the solution so it may be used with quill, reed or steel dip pens.
Iron gall ink is corrosive and not recommended for use in expensive fountain pens
Other ingredients can be added to strengthen or change the color of the ink, act as a preservative, or prevent it from freezing. A brief description of the source and function of each ingredient may inspire you to experiment with your own ink formulas.
gum arabic - is a water soluble golden-colored sap collected from Acacia trees native to North Africa. It may be purchased from art supply stores in the form of a liquid, a powder or as dried clumps or fragments. gum arabic acts as an emulsifier and keeps the black pigment suspended in the liquid - otherwise, it would settle to the bottom of the container over time. It also helps to thicken the ink, allowing it to flow more easily from the pen or brush onto the paper. More importantly, the gum holds the ink at the surface of the paper for a few extra seconds before sinking into the fibers. This influences the appearance and durability of marks made with the ink. The ink line is clearer and sharper than it would be without a binding agent, in part because the ink sinks less deeply into the paper fibers. However, too much gum arabic will cause the dried ink to become inflexible, and it can crack and flake off the surface. Click here for more information!
Tannic acid - is contained in the galls, bark, leaves, roots and fruits of various plants. The greatest concentration of gallotannic acid is found in galls; the bulbous growths formed on the leaves and twigs of trees in response to attack by parasites. galls are collected from oak, oak-apple and pistachio trees. Depending on the source, they can be amorphous in shape (Japanese and Chinese galls); large, smooth and globular (British and American oak galls); or small, round and spiky (Aleppo galls). Aleppo galls, collected from trees native to Turkey, contain the highest amount of gallotannate, and were used in trial preparations of the inks described below. A lower proportion of gallotannic acid may be extracted from the bark of various trees, including oak, chestnut, mountain ash and cherry. Various other sources for tannin include pomegranate rinds, horse chestnuts, hemlock and pine bark. However, the active tannins in these materials are different, and the ink will be less durable and have a green tone instead of the blue black color characteristic of high-quality iron gall ink. Essentially, there are three methods by which gallotannate is extracted from galls:
The fermentation process generally produces the richest, blackest inks. As the mold enzymatically digests the gallotannic acid, the solution is transformed to gallic acid. Gallic acid produces a purer black color in reaction with Ferrous Sulfate (FeSO4) (FeSO4), while gallotannic acid will produce a comparatively browner pigment. Should you want to make a gallic acid ink without investing the time, pure gallic acid can also be obtained from a chemical supplier.
The destructive mechanism of inks is a complex result of different chemical processes due to:
The chemical reactions between the inks and the carrier materials are especially influenced by the environment and storage conditions (temperature and humidity). Deterioration of paper by iron gall inks is a result of the action of inks and support containing iron and other transition metal ions such as copper or zinc. Damage to the support material goes through various stages:
Other degradation processes include the composition of:
The paper and parchment becomes brittle and friable as a result of age and the influence of the destructive inks, deteriorating its natural properties and eventually making it useless as an information medium.
A pigment is in its simplest form is a finely powdered mineral, colored earth, that is mechanically bound to a surface with a binder. Dyes on the other hand are chemically bound to a material generally with the use of a mordant (alum, chromium, copper, tin and iron.) This paper will focus on ground mineral pigments, binders and application methods.
Pigment Colors - The spectrum of natural earth colors can be found in most places of the world.
Natural Colors from the earth:
Processing - To convert a raw mineral into usable pigment is only a matter of grinding it into a very fine powder. Some times though, mineral pigments are very hard and have to be processed. This is done by grinding the mineral using a mortar and pestle (molcahjete) or simply a flat hand stone called a muller or mano, on a larger flat stationary stone (metate). The material being ground can be left dry or water can be added to help keep the fine particles from scattering as it is being processed. This is a tedious task, but knowing that not all of the mineral material need be perfectly ground to make it usable can help us to persevere.
One method of separating the finely ground pigment from the courser material is done using a process called settling. The powdered mineral is poured into a container of water. The water is then stirred to mix the ground pigment thoroughly through the water. The heavier particles of pigment will begin to settle to the bottom, while the lighter, finer particles remain suspended in the liquid. The amount of time given for the heavier particles to settle, will determine the consistency of the finished pigment; less settling time gives a courser pigment, more settling time results in a finer pigment. Usually, after less than a minute, the water with the lighter pigment particles is carefully poured off into another container and allowed to settle to the bottom. The fine pigment will settle to the bottom of this new container leaving the remaining water perfectly clear. Only now, should this clear water be carefully poured off and the remaining moisture in the wet pigment be allowed to evaporate away. The pigment that is left is fine and of uniform size. When it is completely dry, the finished pigment is then ready for use or storage.
The hazards of pigments may be classed in three broad categories:
The choice of pigments colors is a personal one, however, certain colors work well in tempera, some do not. Here is a list of more commonly used pigments.
Blue Ink -
Brown Ink - Digest powdered catechu, 4 parts, with water 60 parts, for some hours; filter, and add sufficient of a solution of bichromate of potassa, 1 part in 16 of water.
Crimson Ink - A beautiful crimson ink is made by mixing red ink No. 1 with the violet ink; about equal parts will answer. The parts given are those of weight, not measure. The mucilage of gum arabic prevents the fine particles of color falling to the bottom in the form of a sediment. Sugar gives to inks a glossy appearance, but very little of it should be used, as it is liable to make the ink sticky.
Gold Ink - Mosaic gold, 2 parts, gum arabic, 1 part, are rubbed up with water until reduced to a proper condition.
Ink of any colour may be made in the same manner, by substituting only a proper coloring ingredient to the aforementioned cinnabar, etc.
Silver Ink - Triturate in a mortar equal parts of silver foil and sulphate of potassa, until reduced to a fine powder; then wash out the salt, and mix the residue with a mucilage of equal parts of gum arabic and water.
Violet Ink - Eight parts of logwood and 64 parts of water; boil down to one-half, then strain and add 1 part of chloride of tin.
An exceeding good writing ink - Boil half a pound of India wood shavings in two quarts of good vinegar, to the reduction of one half. Take off the shavings, and substitute four ounces of gall nuts bruised, and put all into a strong bottle, which you expose in the sun for three or four days, shaking it during that time three or four times a day. Then add a dissolution of two ounces and half of gum-arabic in half a pint of either water or vinegar, Let the whole stand again in the sun for a week, shaking it several times every day, during that term; strain that liquor afterwards, and keep it for use.
Infuse 14 days with frequent agitation, or boil as directed in last receipt. This ink writes pale, but flows well from the pen, and soon turns black."
Black Ink #1- Campeachy logwood chips, 3 pounds; bruised galls, 9 pounds; boil in water, and to the mixed liquors add gum-arabic and green copperas (ferrous sulfate (FeSO4)), of each 4 pounds; to produce 16 1/2 gallons of ink. Quality very good, but inferior to the above [referring to Cooley's Superior Black Ink].
Black ink #2 - According to the most accurate experiments on the preparation of black ink, it appears that formula for the quantity of
Sulphate of iron should not exceed 1/3 part of that of the galls,
by which an excess of color matter, which is necessary for the durability of the black, is preserved in the liquid. Gum, by shielding the writing from the action of the air, tends to preserve the color, but if much is employed, the ink flows badly from quill pens, and scarcely at all from steel pens. The latter require a very limpid ink.
The addition of sugar increases the flowing property of ink, but makes it dry more slowly, and frequently passes into vinegar, when it acts injuriously on the pen. Vinegar, for a like reason, is not calculated for the fluid ingredient. The best blue galls should alone be employed in making ink. Sumach, logwood, and oak bark, are frequently substituted for galls in the preparation of common ink. When such is the case, only about one-sixth or one-seventh of their weight of copperas should be employed. [Inks so made possess little durability.*] (* The observation bracketed appears in an earlier work, Cooley's Cyclopaedia of Practical Receipts Third edition, London 1856)
Black Ink, Cooley's Superior - Bruised Aleppo nut-galls, 12 pounds; water, 6 gallons; boil in a copper vessel for 1 hour, adding water to make up for the portion lost by evaporation; strain and again boil the galls with water, 4 gallons, for 1/2 hour, strain off the liquor and boil a third time with water, 2 1/2 gallons, and strain; mix the several liquors, and while still hot add green copperas (ferrous sulfate (FeSO4)) (sulphate of iron) coarsely powdered, 4 pounds; gum-arabic bruised small, 3 1/2 pounds; agitate until dissolved, and when settled, strain through a hair sieve, and keep it in a bunged-up cask for use. This will produce 12 gallons, very fine and durable.
Black Steel Pen Ink - A black ink, not corroding steel pens, and neutral, may be prepared by digesting in an open vessel, 42 ounces coarsely-powdered nut-galls, 15 ounces gum senegal, 18 ounces sulphate of iron (free from copper), 3 drachms aqua ammonia, 24 ounces alcohol, and 18 quarts distilled or rain water. Continue the digestion until the fluid has assumed a deep black color.
Exchequer Ink - Bruised galls, 40 pounds; gum, 10 pounds; green sulphate of iron, 9 pounds; soft water, 45 gallons; macerate for 3 weeks, employing frequent agitation. This ink will endure for centuries.
Ferrous Sulphate Ink Powder, Iron Gallate Inks - Many formulas exist for making ink powder to produce writing fluid of good keeping quality, low acidity, and satisfactory permanence. Ink will keep longer without depositing sediment if it is made without tannic acid, but with an increased amount of gallic acid. It is possible to replace the usual hydrochloric or sulphuric acid by less than an equivalent quantity of a solid organic acid. ... The weight of ferrous sulphate called for, 15.0 grams, contains 3 grams of iron.
Dissolve ingredients in enough water (distilled is best) to make total volume of 1 liter. Variations in the type of dye and the amount of air in the bottle may cause formation of sediment. ...
Macerate in a clean corked bottle for 10 days, or even longer, with frequent agitation; then add
Mix well, and afterwards further add
Agitate occasionally for 2 or 3 days, when the ink may be decanted for use; but it is better if left to digest together for 2 or 3 weeks. When time is an object, the whole of the ingredients may be at once put into a bottle, and the latter agitated daily, until the ink is made; and boiling water instead of cold water may be employed. The above will make 1 quart of beautiful ink, writing pale at first, but soon turning intensely black. Dick's Encyclopedia of Practical Receipts and Processes, [no date] circa 1870
Glycerine Ink - Take copperas, 4 ounces; nut-galls, 12 ounces; logwood, 8 ounces; vinegar, 8 ounces; gum-arabic, 1 ounce; glycerine, 1/2 ounce; water, 48 ounces; all the solid substances are to be pulverized and boiled for an hour together; they are then set to cool, strained through a flannel bag, and after that filtered through a folded filter. A drop of oil of cloves is added, the whole well shaken and filled into bottles. This ink will copy well.
This makes a fine inexpensive homemade ink!
Method:
India Ink #2 - Let ivory or lampblack be mixed with a small portion of Prussian blue or indigo, for a blue-black, and let the same blacks be united with raw or burnt umber, bistre, vandyke or any other brown, instead of the blue, for a brownblack. These should be mixed together in a weak gumwater (perhaps matt-work would answer the purpose better), first levigating them very fine, in common water, on a marble slab. When dried to the consistence of a paste, let the glutinous matter be well mixed with them; that will be found sufficiently strong, which binds the composition so as to prevent rubbing off by the touch. Indian-ink drawings should be handled as lightly as possible. Too much gum in the composition will create an offensive gloss.
Ink Powder #1 - For an ink powder take
Pulverize and mix. This amount of ink powder will make 1 gallon of good black ink. Two or three powdered cloves should be mixed with each pound of powder, to prevent moulding.
Ink Powder #2 - Take equal parts of black rosin, burnt peach, or apricot stones, vitriol and gall nuts, and two of gum-arabic. Put the whole in powder, or in a cake, as you like best.
Ink Sticks | |
Chinese Ink Sticks | |
The characters on top of this Chinese ink stick means that the soot for it came from burning twigs or roots from a pine tree.
Pine soot ink has a blue-black hue and yields dead-matt writing on Western papers. Apart from looking for these characters, there is a good way to decide if an ink stick is made from pine soot by observing its bottom part (the one which you grind) will be dry, looks matte and dull. | |
This Chinese ink stick indicates that the soot has been obtained from burning vegetable oil.
Vegetable oil soot ink is shiny and has a brown-black hue. The bottom part of the stick (the one which you grind) will be dry, glossy and smooth. | |
Yellow Mountain Pine Soot This Chinese Ink Stick is made from pine soot. The top character means 'yellow' and the next one means 'mountain'. The ink obtained from it is somewhat coarse, but the ink behaves quite nicely. |
Everbright This Chinese Ink Stick, known as 'Thousand Autumns Light', is composed of vegetable oil soot. The characters for 'select soot' can be found on top, which indicates that it is of middle quality. |
Japanese Ink Sticks | |
Ink is made from the displaced soot obtained by burning organic substances which are mixed, along with other additives, to glue acting as a polymer base. The extreme heat and moisture of summer is not suitable for the production of ink. This means that ink must be made in the cooler part of the year from mid-October to the end April. The basic raw materials used in the production of ink are made from soot acquired by the burning of pine wood and sap, or vegetable oil. Although ink-making originated by using pine soot, vegetable oil is mainly used as of late. In the case of pine soot, red pine and it's sap are burned in a small stove placed in the centre of a small hut with sliding paper doors. Once burned, the soot which has been heavily deposited on the doors and ceiling are scraped off and collected. Oil soot, which is taken from the sesame, rape, camellia and paulownia trees, is favoured because of its price, quality and ease of burning. In addition, soot is improved by burning the mineral oil attained from petroleum oil. It has depth like oil soot but very small particles and a redness which gives it a different character. For the production of oil soot, a long tradition has followed by burning the oil in an earthenware bowl and later scraping the soot off the lid. But, because of low output, quality inconsistency and material waste an automatic unit was developed where a cylinder spins above the burning oil producing high quality soot. The adhesive glue is made from animal skin and bone which is boiled to produce a solid gelatin. By adding solid ink to the glue allows the soot particles to adhere producing an ink in which water can be added to create the necessary consistency for paper application. To melt the glue a heating method is used where water and glue are added together and steamed in a two level oven. The glue has a raw smell which is neutralized by adding plum flower and other fragrances. Once the glue is cooked, soot and glue are thoroughly mixed together. In Japan the weight mixture ratio is 10:6, soot to glue. However, the glue level is decreased and the viscosity is reduced in ink for fine letters. This mixture of soot, glue, and additives is put into a mixer and blended into a soft rice cake-like ball which is then kneaded by hand on a wooden board. After kneading, the ink ball is placed into a wooden pattern. Although there are many sizes of solid (dry) ink, in Japan 15 grams is called 1 cho and considered the standard. There are sizes ranging from 0.5 cho to 20 cho and many shapes, such as circles, square, etc. To make 1 cho of solid ink, a 26 gram ball is required which means the pattern must be much bigger than the finished product. A thoroughly kneaded ink ball is weighed, placed into a wooden pattern and pressed. The ink is then removed from the pattern. If the ink is left alone the surface will quickly dry and cracks will form. Because of this, the whole thing must by dried slowly by placing it into a box filled with damp charcoal. By constantly changing the damp charcoal the ink is dried over a 7-20 day period. Once fairly dry the ink is wrapped in rice husks and hung from the ceiling for 30-90 days to dry in the air. After drying any charcoal or debris that remain are quickly washed off with water. There are two types of surface finishes. One is a dull natural finish, and the other a buffed finish. The ink is stacked and dried for one month. Later the surface is prepared with letters or a picture and then packaged. |
Ink without gall-nuts, which will be equally good to wash drawings and plans, and strike very neat lines with the pen.
Iron-gall ink #2 "...Copperas is ferrous (or iron) sulphate, which is available from any drugstore as a dietary supplement. In its natural and impure state copperas has a green tinge, hence the incorrect association with copper. Tannin, or tannic acid ... is the brown substance found in the bark and leaves of trees. Medieval scribes had their own favorite sources, however:
Method: one part powdered gum arabic, two parts copperas, three parts crushed galls, and 30 parts water, all by volume...." Paul Werner, "Dragon's Blood and Ashes", Calligraphy Idea Exchange, volume 1, number 2
Boil the galls and logwood in 6 quarts water till reduced one-half; strain; add the other ingredients. Stir until dissolved. Clear and bottle. If it does not shine enough, add more gum; also a few cloves, to prevent mold. * [Note: The term "sugar candy" is not defined in the recipe. Dick's Encyclopedia, in a different location, entry 1368, describes five stages that result in different kinds of candy. Which type would have been used in this ink recipe about 1870? You be the judge.]
Jewish Scribe's Ink - This recipe was sent by Rabbi Yair Hoffman of Far Rockaway, New York, who obtained it from Rabbi Kilschevsky, a scribe in the Meah Shaarim section of Jerusalem. The recipe likely dates back to a time before the settlement was initiated by the students of Rabbi Elijah of Vilna in the early 1800's.
* The gum arabic gives it a rubber-like quality ensuring that the letters will not crack on the page. Care should be taken not to add too much gum arabic as this would allow the entire letter to slip off the parchment.
Making the ink-stone with which you may write without ink
Drawing Inks - Today most drawing inks are made from dyes. Inks such as India Ink and Chinese Ink are pigmented inks (made with pigments). They use gum arabic or Methylcellulose as the binder:
Gum arabic Recipe
For both types of drawing ink...
With either binder, the pigment paste and binder can be worked into a stiff dough, shaped, and allowed to dry. In order to be used as ink, simply wet the stick with water. This is known as Pearl Ink.
The oil loses by the boiling about 1/8 of its weight, and emits very offensive fumes. Several other additions are made to the oil during the boiling, such as crusts of bread, onions, and sometimes turpentine. These are kept secret by the preparers. The intention of them is more effectually to destroy part of the unctuous quality of oil, to give it more body, to enable it to adhere better to the wetted paper, and to spread on the types neatly and uniformly. Besides these additions, others are made by the printers, of which the most important is a little fine indigo in powder, to improve the beauty of the color.
Secret to revive old writings, which are almost defaced - Boil gall-nuts into wine; then steeping a sponge into that liquor, and passing it on the lines of the old writing, all the letters which were almost undecipherable will appear as fresh as newly done.
Shellac Ink, or Coathupe's Writing Fluid -
Shining ink #2 - Infuse for a day in a quart of good table beer half a pound of the blackest and most shiny gall nuts you can find. Add three ounces of gum-arabic, and half an ounce of brown sugar candy, with four ounces of green copperas (ferrous sulfate (FeSO4)). Then boil the whole in a glazed pipkin for about an hour, strain it through a cloth, and put in in the cellar to keep for use.
Standard for Government Writing Ink
(Federal
Specification, TT-I-563, Ink; Writing)
This formula was written originally to provide ink for use in post-office lobbies, where the conditions are devastating to pens. This standard ink is similar to some of the commercial writing inks. ...
Tannin ink for writing on celluloid
Dissolve the ferric chloride in a portion of the acetone and the tannin in the residue, and mix the solutions. Gardner D. Hiscox and Prof. T. O'Connor Sloane, Fortunes in Formulas, [New York: Books, Inc.], 1957