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Evan Lindquist, Artist-Printmaker
Artist Laureate for the State of Arkansas, 2013-2017

Old Ink Notes

Sources of Information
Information about ink formulas, chemistry, and history of Western and Asian ink: Jack C. Thompson. Manuscript Inks. Portland, Oregon. The Caber Press. 1996. It includes an appendix on Oriental ink sticks by Claes G. Lindblad. Scroll down on this page to see "Dry and crystalline forms of ferrous sulfate", a valuable excerpt from Jack's book. If you plan to make ink, read this first.
http://www.teleport.com/~tcl/mi.htm
The Iron Gall Ink Corrosion Website. Covers all aspects of iron gall ink corrosion. Topical pages include: Introduction, Iron Gall Ink, Ink Corrosion, Collection Management, Research, Conservation, Events, Literature, Links, Discussion List, Site Map, Credits, Ink Corrosion Horror Show. New research and up-to-date information will be posted.
http://www.knaw.nl/ecpa/ink/index.html  
Claes G. Lindblad's pages on inks and colors for designers and calligraphers.
http://www.algonet.se/~claesg/index.htm
Conservation OnLine. Resources for conservation professionals. CoOL, a project of the Preservation Department of Stanford University Libraries, is a full text library of conservation information, a wide spectrum of topics on conservation of library, archives and museum materials. (New link created 6/2/2001)
http://palimpsest.stanford.edu/
AIC--American Institute for Conservation of Historic and Artistic Works. Resources Center, Education Grants, Scholarships, Specialty groups, Find a conservator.
http://www.conservation-us.org
Canadian Bookbinders and Book Artists Guild has great links and information (Binding, Papermaking, Calligraphy, Letterpress / Typography, Wood Engraving, Paper Decorating, Conservation, Workshops, Exhibitions)
http://www.cbbag.ca/
Make iron-gall ink from acorns? Larry Vienneau has posted a video on YouTube to demonstrate the process.
http://www.youtube.com/watch?v=zV0l3KbnYAo
The Household Cyclopedia has a page on inks and other pages on art materials and methods
http://www.publicbookshelf.com/public_html/The_Household_Cyclopedia_of_General_Information/
"Where can I get ingredients to make ink?"
I receive this question often. Check this link.
http://www.sinopia.com
If you know of other reputable sources that can provide most of the materials listed in these pages, please share the information. I will be pleased to post their contact information here.

How is old ink used?
Follow these links to find comprehensive information about calligraphy, penmanship, and pen nibs. To learn more about Ornamental Penmanship, you will find online scanned pages of complete, rare old manuals and tutorials for Spencerian, Copperplate, Engrossers Text and other styles with broad pen and pointed pen.

History of pens and penmanship, oblique penholders, pointed pen work styles and methods, Ornamental Penmanship, Copperplate, Spencerian
Dr. Joe Vitolo's Zanerian.com
International Association of Master Penmen, Engrossers, and Teachers of Handwriting.
IAMPETH
Steel pen nibs and related items. BLAM design supplies new and vintage steel pen nibs. BLAM design is a site about Lettering, Comics, Handwriting, Vintage Pens and Calligraphy.
Hans Presto's Vintage Pen Nibs
To prevent ink from molding, add a few bruised cloves, or a little oil of cloves. An old practice, no longer recommended, was to add a few drops of creosote to prohibit the formation of mold. Creosote is now considered to be a hazardous substance.
E.W. Bloser's Ink
E.W. Bloser, was owner of the Zaner-Bloser Co. in Columbus, Ohio. He described his ink in two paragraphs of a typewritten letter to Daniel W. Hoff, Meadville, Pennsylvania, April 28, 1913. His description follows:
"In signing my letters I usually use Zanerian India Ink, although I sometimes use some of our Zanerian School Ink. However, I think that I used India Ink in signing most of the letters I sent you. There is really very little India Ink in it, the main part being water. I put in the inkwell a little India Ink and then add a little water, stirring it quite a good deal. I then add a few drops of Arnold’s Writing Fluid* until the ink comes to the point of separation. The India Ink is made largely of carbon and the Arnold’s Writing Fluid is antagonistic to it and will not mix well. For that reason very little of the Writing Fluid should be added at a time, although enough should be added from time to time to bring it to the point of separation. That is, to the place where the ink becomes full of specks, the solids separating from the water. If the ink stands for some little time the water comes to the top and the solids go to the bottom. It should then be thoroughly stirred and probably a little more water put in on top without stirring it. Of course, this should be done from time to time as the ink is used. It doesn’t require much time. The older the ink gets, the better it comes and a little water can be added now and then. It is astonishing how little ink there really is in the inkwell after it has been used for several months. I got hold of this idea accidentally some years ago by unintentionally mixing the two antagonistic inks and then experimenting with this ink. If it is done just right, there is probably no better ink for fine ornamental writing. A very fine line can be secured by loading the shades. They are black enough to make the proper contrast.
"I enclose herewith a little writing executed by our Mr. Knowles. You will notice on the light lines that the ink is to the point of separation, as is shown by the tendency to skip a little, and if more Writing Fluid were put in, the ink would be spoiled. Stirring is one of the necessary things in order to get the best results with it, since in this way the antagonistic elements seem to be sufficiently united to work properly."
* Arnold's Writing Fluid was described as a mixture of sulphate of indigo and gallotannate ink. More information on page 3, Old Ink Recipes.
For a brief history of writing ink, see:
Art Maier, "Ink Ink Ink, Part I", Pen World magazine, summer 1988, pp 12-15, 29
Preparation of Iron Gallotannate and Gallate Inks
When water is called for, distilled water is best, with rainwater the second choice. There are places where the water of streams and wells is so hard, because of the calcium carbonate dissolved in it, that a substantial part of the acid in iron gallotannate and gallate inks will be neutralized if natural water is used for making them. ...
To make a liter of one of the gallotannate inks, dissolve the gallic and tannic acids in about 600 ml of water at about 50 degrees Celsius (122 degrees Fahrenheit). For convenience, this can be done in a 1-liter measuring flask set in a vessel of warm water. ...
Swirl the flask frequently to hasten the dissolving of the acids. Then add the requisite amount of hydrochloric acid, and the crystals of ferrous sulphate. ... allow to cool. Meantime dissolve the dye in a separate portion of 250 ml of water. Filter the solution directly into the measuring flask. Rinse the vessel in which the dye was dissolved with two or three small portions of water, not more than 100 ml in all, and pour each portion through the filter paper to wash as much of the dye as possible into the flask. ... When the solution in the flask is at the correct temperature, the carbolic acid can be added, and finally enough water to make total volume 1 liter. The ink must now be mixed very thoroughly by inverting the stoppered flask a dozen or more times. ...
From Circular of the National Bureau of Standards C413, "INKS"
U.S. Department of Commerce, Issued December 28, 1936
By C. E. Waters
Equipment for Making Ink The manufacturer of inks will have proper equipment, but whoever makes small batches at home must put up with makeshifts, unless he has some chemical glassware for preparing the solutions, a measuring cylinder or two, and moderately sensitive scales with small weights. If ordinary bottles must be used, and the solutions have to be heated, there are two safe ways to go about it. One is to set the bottle in a deep vessel containing cold, or at most lukewarm, water, and then to pour in hot water slowly, and not against the side of the bottle. Another way is to set the bottle in water as before, but to put under it a piece of wire netting or a spiral of heavy wire to keep the bottle from touching the bottom of the vessel. It can then be heated over a low gas flame or on a stove. The idea in either case is not to heat the outside of the bottle too quickly while its contents are cold, because the expansion due to the heat may so strain the glass that it will break. The materials will dissolve more quickly if the bottle is swirled or shaken frequently so as to stir up the relatively concentrated solution at the bottom. So far as possible avoid the use of metal vessels for making ink....
From Circular of the National Bureau of Standards C413, "INKS"
U.S. Department of Commerce, Issued December 28, 1936
By C. E. Waters
Modern ingredients. "Modern writing ink is made by combining tannic, gallic, and dilute hydrochloric acids with an iron salt, phenol, and a blue or black dye.... Iron gallotannate writing inks have been in use since the twelfth century.... Their permanence, however, is not usually considered great enough for general artistic use, especially where there is continual exposure to daylight; permanence for use in records and documents, which are ordinarily kept filed away in darkness and in which considerable fading or color change could occur without seriously impairing legibility, is another matter."
Ralph Mayer, The Artist's Handbook, [New York: The Viking Press, 1981], p 535-536
History. "Ink for writing and drawing was invented in China and Egypt at about the same time; according to various researches, the date in each country is generally believed to be not much before 2500 B.C. These inks were of the same type as our modern drawing ink -- mixtures of carbon and binders. The Romans called their carbon ink atramentum. Later they also used sepia. The earliest record of the material we now know as writing ink, as it has been made and used from medieval times down to the present, is in the writings of Theophilus, who described an iron-nutgall ink. Pliny, however, about ten centuries before this, knew that paper treated with copperas could be blackened with an infusion of nutgalls."
Ralph Mayer, The Artist's Handbook, [New York: The Viking Press, 1981], p 536
If ink has a tendency to bleed or run when applied to paper, try adding more gum Arabic to the ink. Experiment to find the right amount. If you add too much gum, the ink will remain wet or sticky. Most papers available today were made for purposes other than receiving liquid ink.

A Forest of Ink
"Logwood trees from the forests of Central America and the West Indies furnish the principal ingredient in Logwood Inks. These trees rarely exceed forty feet in height and are ready for felling when about ten years old. After the bark and sap-wood of the trees have been removed, the dark brown colored wood remaining is cut up into chips and exported to this country. The chips are put into vats with other necessary ingredients and go through a process very much resembling the steeping of tea in order to extract the coloring matter. This coloring can be seen by holding these chips up to the light and noting the purplish black appearance.

"The best species of logwood trees are grown in Jamaica, so it is Jamaica chips that go into our Logwood Inks, of which the most important and best known is Carter's Black Letter in ten-cent bottles. Logwood Inks write a purplish black and dry black, and are in general use in schools and for other purposes where absolute permanency is not required. If you want to distinguish this class of inks from the aniline and iron-gall classes, test with dilute muriatic acid and the logwood inks will assume a bright red tint."

Carter's Ink Company advertising brochure, The story Your Ink Bottle Tells, 1919

A River of Ink.

"Travelers in northern Africa have observed a curiosity of nature -- a river of ink. The water is black, yet the streams which feed it are clear.

"Chemical analysis and examination revealed the cause of this strange phenomenon. One of the streams which empties its water into the river is strongly impregnated with iron from the soil through which it flows. Another stream carries tannin from a peat swamp. It is the chemical combination of the iron, tannin and oxygen of the air that turns the water black. This chemical reaction forms the basis of the third and most important class of inks, known as iron-gall inks. These are the inks of real permanence and are represented by Carter's Writing Fluid and Carter's Fountain Pen Ink.

"Iron-Gall Ink was first made in the twelfth century, but it was not until the re-establishment of learning in the fifteenth century that it came into common use.

"The most important factor in the making of this ink is gall nuts, certain species of which are found in China, India, Japan and even in some oak and willow trees in America. The gall nut which will produce the greatest amount of tannic acid and unite in the most perfect chemical solution is the one desired for making ink, and this gall nut known as the Aleppo gall is found in far off Syria, Asia Minor. These nuts are hard, spherical bodies, about the size of our acorn.

"A peculiar kind of insect, Mrs. Cynips Tinctoria, similar to our horsefly, bores into the small twigs of oak trees and then lays eggs in the wound. A little lump is the result.... The egg grows with the gall and is soon converted into a larva which feeds on the surrounding vegetable matter and forms a cavity in the centre of the lump. Eventually the lava [sic] becomes a fly and escapes by eating its way out, if the gall remains long enough unpicked. In such cases, a small round hole in the side of the nut shows the path of escape. The best nuts for ink making are those that are picked when fully ripe but just before the escape of the insect, as these contain the largest amount of tannin.

"As the name implies, iron-gall inks are based on a liquid in which an iron salt is combined with tannin extracted from gall nuts. The iron salt is called copperas and comes in the form of beautiful green crystals.

"This liquid is practically colorless until acted upon by the oxygen in the air; that is, a pen dipped into such a fluid would make no visible mark on the paper. Most people, we find, like to see what they are writing as they write and so a blue aniline color is added. After the ink is exposed to the air, the iron-gall compound develops to an intensely black and permanent color, entirely superseding the original blue which ultimately fades away. This change in color is what causes it to be referred to commonly as a blue-black ink. The black remains clear and legible as long as the paper on which it is written lasts."

Carter's Ink Company advertising brochure, The story Your Ink Bottle Tells, 1919

Botanical information. "Tannin inks were first described in the eleventh century. Aleppo or nut galls have from the outset been the chief source of the tannin. These galls are formed on the twigs of the Aleppo oak (Quercus infectoria), as a response to the injuries caused by the egg-laying activities of an insect. The plant is a small shrub, 5 or 6 ft. in height, found throughout the Mediterranean region. The small spherical or pear-shaped galls are produced in great abundance and have an exceedingly high tannin content. In making ink, either the galls or an extract made from them are combined with ferrous sulphate; an agglutinant, such as gum arabic; and a coloring material, such as logwood. Similar galls produced on Rhus chinensis and other Chinese and Japanese species of sumac are sometimes used as substitutes for Aleppo galls, although they are much inferior.... Tannin inks are also made to some extent from other sources of tannin, such as logwood and chestnut. Logwood ink is especially noteworthy because it contains both tannin and a coloring agent as well."
Albert F. Hill, Economic Botany, [New York: McGraw-Hill], 1952
Writing Fluids. The very general use of steel pens has caused a corresponding demand for easy flowing inks, many of which have been of late years introduced under the title of "writing fluids," or "steel pen ink." These are mostly prepared from galls..., but a less quantity of gum is employed. The blue writing fluids, which either maintain their color or turn black by exposure, are prepared from the ferrocyanide of potassium (prussiate of potassa), or from indigo.
Dick's Encyclopedia of Practical Receipts and Processes, [no date] circa 1870
Permanence of Ink. The great difficulty with all iron inks is the precipitation which will take place, after a longer or shorter time, and which manufacturers have tried to obviate by substituting other materials. All inks, however, the basis of which is not tannate and gallate of iron, are not black immediately, and consequently not so agreeable to the eye when using them. The alizarine or rather indigo inks have a greenish, the chromium inks a reddish hue, and are not better adapted to withstand chemical agents than iron inks are.
Dick's Encyclopedia of Practical Receipts and Processes, [no date] circa 1870

Aging of Writing

... The fresh writing is blue, except in the rare case of the ink containing a black, instead of the usual blue, dye. In a few hours the writing becomes perceptibly darker, because the ferrous salt in the ink has begun to be oxidized to black ferric gallotannate. Under ordinary conditions of diffused daylight, the writing should attain its greatest intensity of color, a deep blue-black, in about a week. If the ink is unusually acid, the color develops more slowly. On the other hand, if the ink contains too little acid, or if the acid is neutralized by exposing the fresh writing to the fumes of ammonia, the blackening will be complete in a day or two.

The oxidation that causes the blackening does not cease abruptly when all the ferrous iron is converted into ferric iron, for the dye and the gallic and tannic acids are also subject to oxidation. In the course of time the dye will disappear. If this occurs before the two acids have been affected the writing will still be black, but no longer blue-black [if blue dye was employed]. This is normal for a well balanced ink, but if the ink maker depended more upon dye than upon iron gallotannate, the aging writing will never go through the true black stage, but that when all the dye is gone, a substantial part of the gallic and tannic acids will have gone with it, leaving writing with a brownish color. If the paper endures long enough, finally nothing will be left of the writing but rusty lines of ferric oxide. ...
From Circular of the National Bureau of Standards C413, "INKS"
U.S. Department of Commerce, Issued December 28, 1936
By C. E. Waters

Dry and crystalline forms of ferrous sulfate.

Jack C. Thompson writes: "It's very important that people making their own ink understand the difference between dry and crystalline ferrous sulfate, especially when trying to decipher an old recipe which may not stipulate the form."

Jack has generously given permission to copy the following information from pp 6-7 of his book, Manuscript Inks © 1996, The Caber Press, Portland, Oregon.

"Copperas is an interesting material. It is available today as a white, granular powder tinged green, or as green crystals. Copperas which I've manufactured occurs in the form of large green crystals. If the crystals are left exposed to the air they dry and turn into a gray-white, granular powder, with a green tint. Fresh copperas has the formula: FeSO4+7H2O; dehydrated (exsiccated; FeSO4+3H2O) copperas is approximately 35% lighter in weight.

"It has been a source of puzzlement to many scholars that, while the writing in some manuscripts has remained black and the parchment or paper sound, sometimes the ink has eaten through the support.

"It may be the case that the person making the ink used dehydrated copperas, by weight, in compounding a recipe where fresh (hydrous) copperas was intended, instead of reducing the weight of copperas by about thirty-five percent, thereby greatly increasing the amount of free sulfuric acid in the finished ink. There is sufficient variety in the proportions given in old ink recipes that some of them would produce a chemically aggresive ink, whichever form of copperas was used.

"There is at least one other, interesting, possibility. Parchment prepared from an animal skin which was dehaired in a lime bath retains some of the lime and this alkaline earth will neutralize some of the acid contained in the ink. If the skin was dehaired through the agency of water alone (and it is easy enough to do), there would nothing to neutralize the acid.

"Some recipes state that the copperas must be ground and sieved, suggesting (to me) that the recipe's writer was accustomed to using copperas in its dry form. Those recipes which only call for copperas to be added suggest that the copperas was in crystal form, for the crystals are fairly soft and soluble. The best reason for drying copperas is to ship it to market; shipping charges are based, in part, on weight and if some water is removed, the weight is less. There is sufficient excess water (and sulfuric acid) in crystal copperas to dissolve out and boil for some time when a sample is placed in a test tube over an alcohol lamp. If the heat is applied for a long enough time, the copperas changes into the pigment known as Indian Red; it is also known as jeweler's rouge.

"Another reason for drying it out, although it was not well understood at the time, is that copperas contains some free sulfuric acid, and the acid would soak into the packing and shipping materials causing them to break down.

"Any recipe which specifies filtering through wool indicates that the writer has observed that filtering through any other cloth will result in the eventual loss of the cloth through acid tendering; wool is naturally acid resistant."

When Post Cards came into use late in the 19th century, many people used Invisible Ink that could not be read until the receiver of the Post Card activated the ink to make it visible. There were many types of Invisible Inks used on Post Cards and secret correspondence, each activated in a special way.
But that's another story -- just one more part of the fascinating history of old inks.
 
This is the fourth of five pages of information about old ink.
The last page is an appendix about Testing, Dyes used in inks, and a Bibliography.