Making Walnut And Butternut Inks

[Paddler]

In the summer of '09, the FPN had some threads with hints and snippets about walnut ink. Having a few black walnut trees in my yard, I looked on the Internet for more information, hoping to find a recipe. The information I found was mostly misinformation. All of it was conflicting and some was just patently wrong. I put the project on a back burner and began another project.

 

Then, around the end of October, I received a PM from someone who calls herself "wood". She said she had made some walnut ink and would like my opinion of it. A few days later, a sample came in the mail. I liked it a lot. Wood graciously gave me her recipe. I grabbed my coat and a rucksack and headed for the woods to try to find some walnuts the squirrels had overlooked. I was able to find eight old, black, half-rotted nuts and made a couple of ounces of ink from them. The experiments began. In January of 2010, my ink was completely used up. Wood sent me a whole pint of extract so I could continue my investigations. During the summer, one of my trees dropped a few immature nuts from time to time, so I could make ink more or less continuously and refine my recipe. The following is a description of my way of making ink from black walnuts (Juglans nigra) and from butternuts (Juglans cinerea).

 

The ink from both species has a brown color. The walnut ink is a warm brown. Butternut ink has a yellow component that makes the color look a bit mousy to me. It just doesn't "pop" the way walnut ink dies. The following writing sample was made on paper from a Mead Composition notebook. I chose this paper because it takes the inks well; it illustrates the shading the inks can make; it is inexpensive; and it is very widely available.

 

http://picasaweb.google.com/lh/photo/cNbB32_zIFyeZ9BJp53fyw?feat=directlink

 

The ink is fade resistant and water resistant. You can make it as light or as dark as you want it to be. You can make it yourself in about three days (most of that time is waiting). The nuts are usually free for the taking. The equipment needed is inexpensive. What's not to like? Two things:

 

1. The ink has no lubricity. Zilch. It feels like you are writing with plain water. The nib just drags along.

 

2. The ink reacts with iron. This wears out a steel dip pen nib much faster than other inks. After writing about 20 pages, a regular pointed nib has sharp edges and needs to be touched up on a stone.

 

First I want to dispel the misinformation I have read about black walnuts.

 

The center of the nut is the edible part called the "nutmeat". Surrounding the nutmeat is the "shell". In a mature nut, the shell is roughly spherical and deeply ridged. It is very hard. In an immature nut, the shell starts out soft (in June where I live) and gradually hardens (July), until in late August, it becomes very hard indeed. Surrounding the shell is a fibrous layer called the "husk". While the nut is on the tree, the husk is green. After the nut has fallen in late September, the husk gradually turns black. Ink is made from the husk at any stage.

 

Mature black walnuts range from the size of golf balls to baseballs. So, in the following recipe, the number of nuts that make an ounce of ink is extremely variable. The easiest way to obtain the husk material is to strew the nuts in your driveway and drive over them a few times. The shells are so hard, the weight of the car won't smash them.

 

Mature butternuts look like walnuts, only they are football shaped. The shell looks like a fat peach pit that is covered with sharp-pointed ridges. One end of the pit is flattened and narrowed to a stiletto-like blade. It would not be wise to drive over these with a car.

 

What you will need to make an ounce (+) of ink:

 

A supply of walnuts or butternuts, enough to make 1.5 cups (350 ml) of chopped husk material.

 

Rubber or vinyl gloves. The stain in the husks will color your skin brown. Only time will remove this stain. It takes about two weeks.

 

A sharp knife.

 

A cutting board. You are making ink here, not food. Don't use your kitchen cutting board or butcher block. The stain will never come out and who knows, it could be toxic.

 

A plastic tub or Pyrex dish, with lid, that will hold about three cups (700 ml).

 

About three cups (700 ml) of distilled water. Any water will work. Distilled water works best.

 

A wide-mouth jar that will hold about a pint (700 ml).

 

A large dispensing syringe or turkey baster.

 

A small (3 to 5 ml) dispensing syringe with a calibrated barrel. Used for measuring ink and additives.

 

A few paper towels.

 

A paper coffee filter.

 

A Pyrex cake or pie pan.

 

An oven or food dehydrator.

 

A two-ounce (60 ml) ink bottle.

 

A small quantity of high-proof ethyl alcohol. I use 151 proof rum. Wood uses 100 proof vodka. You want the alcohol to be as concentrated as possible so you don't have to add much as a preservative and thin your ink too much.

 

Procedure:

 

Remove the husk material from the nuts and chop it up, using the knife and cutting board. You want 1.5 cups of finely chopped husk. Put the husk material into the plastic or glass tub and just cover it with boiling distilled water. Put the cover on the tub and let stand for 24 hours.

 

Strain the liquid through a paper towel into the wide mouthed jar. Put the jar into your refrigerator. Label it!!!!! Return any husk material in the paper towel to the tub and cover with boiling distilled water again. Put the lid on and let stand for 24 hours. Strain the liquid into the jar with the first batch. Discard the spent husk material.

 

Push a wad of paper towel down into the nozzle end of the large syringe or baster. Cut two four-inch (10 cm) squares from the coffee filter and wrap them around wads of paper towel. Push them down the barrel of the syringe or baster and down against the first wad of paper. The paper towel material should hold the filter paper out against the barrel sides and make a good seal when it gets wet. Fill the barrel with the ink extract and squeeze it through the filter into another container.

 

The filtered extract is way too thin to make good ink. You must concentrate it. I pour the extract into saucers in my food dehydrator and set the heat to 135 degrees F. In a few hours, the ink is ready. If you don't have a dehydrator, you can use your oven. Set the temperature to 130 to 150 and use a glass cake or pie pan to evaporate water from the extract. If you used green husks, there is sugar in the extract. The sugar can caramelize or burn if the heat is too high. If that happens, you will have to filter the finished ink and you will lose a lot that way. Properly done, you will have a rather thick black puddle in the middle of a dry ring of solidified dye.

 

Put on your rubber glove and, with a finger, rub the liquid around on the dry ring to dissolve it into the liquid again. Test your ink with pen and paper. Keep evaporating until the ink is a little too dark for your liking. You will be adding alcohol to it later and that will thin it and make it lighter.

 

Use the calibrated syringe to transfer the ink to your inkbottle. Write down how much you have.

 

Now, you have to figure out how much preservative to add. I make my finished ink 10% ethanol by volume. Why? Because wood does it that way and hers lasts for years without spoiling. I have read that 5% is adequate. If so, that would be better, as the alcohol promotes feathering and bleeding. A low concentration, however, is taking a chance that Acetobacter will invade your ink and turn it to vinegar. It's your choice. Here is the equation:

 

AX = B(C+X)

 

Where:

A = alcohol proof divided by 200. This is the alcohol concentration of your booze expressed as a decimal.

 

B = the alcohol concentration, expressed as a decimal, in your finished ink.

 

C = the volume, in ml, of raw ink you are starting with.

 

X = the volume, in ml, of booze you must add to the raw ink.

 

Solve for X.

 

Example: I just made 32 ml of ink. How much 151 proof rum must I add to it to give me ink that is 10% alcohol?

 

A = 151 divided by 200 = .755

 

.755X = .1(32+X)

 

Multiply by 10 on both sides:

 

7.55X = 32+X

 

Subtract X from both sides:

 

6.55X = 32

 

X = 4.88 ml of rum

 

Additives:

 

You can make black ink from the brown version by reacting it with iron. You use clean, rust-free iron or steel for this. The result is something similar to iron gall ink. It gets darker as it dries.

 

Pour the ink into a shallow dish or saucer. Put on a rubber glove and take a wad of steel wool about the size of a cotton ball and dip it into the ink and squeeze it dry. Dip and squeeze repeatedly until the ink is as dark as you want it. It is important not to let the ink stagnate in the steel wool. If you don't keep it moving, the reaction forms a black pigment that will settle out. If there is enough of this pigment in the ink, it will bridge up in the nib slit and clog it. If you stop to test the ink with pen and paper and then want to make the ink still darker, rinse the steel wool out with distilled water and then continue the dip-squeeze routine. Be careful of this ink; it will leave a deep purple-black stain in a porcelain sink. During the blackening process, the ink becomes frothy and an odor becomes evident. This odor is not putrid and not fetid, but it is definitely biological smelling. The odor dissipates in time. No worries about your letters carrying a pong.

 

Adding gum Arabic to the ink will make it write dryer. It also destroys its water resistance.

 

SterilInk from Tryphon did not prevent my ink from growing SITB, even when I used a double or triple dose.

 

Ink Safe from Tryphon did not prevent my ink from growing SITB, either. It did, however, increase the flow through the nib. On certain hard-surfaced papers, this gave dark borders to the lines and greatly increased the writing's contrast. The surfactant in Ink Safe will destroy the ink's water resistance.

 

Experiments with copper show that it can inhibit bacterial growth. I tried a coil of bare copper wire in a bottle of walnut ink for several months. It did not develop SITB in that time, while a single control did. I have not done the more extensive testing needed to draw a conclusion from this. I also don't know if the ink reacts with the copper in a similar fashion to iron. More testing is needed in this area.

 

Paddler

Edited October 6, 2010 by Paddler

[Northwoods]

Interesting! I wonder how glycerine would play instead of alcohol? It'd thicken it slightly instead of thin it, and may offer some lubrication, and perhaps be as good or better a preservative. I also presume that you could dehydrate the dye entirely and reconstitute as needed to aid preservation.

 

It makes a gorgeous colored ink!

 

Thanks for sharing.

[Paddler]

Interesting! I wonder how glycerine would play instead of alcohol? It'd thicken it slightly instead of thin it, and may offer some lubrication, and perhaps be as good or better a preservative. I also presume that you could dehydrate the dye entirely and reconstitute as needed to aid preservation.

 

It makes a gorgeous colored ink!

 

Thanks for sharing.

 

I tried glycerine. It doesn't lubricate at all. It could be a preservative; I haven't tested it for that, though. Glycerine is actually an alcohol.

 

You can dehydrate the dye completely. If you dehydrate the dye extracted from green husks, you get something resembling tar, probably due to the sugar content. This stuff is difficult to handle. If you let the husks turn black and ferment the sugar away for a couple of months, the dye will dehydrate down to three crystalline fractions: one is brown colored and nearly amorphous; one consists of flat, black squares that grow on the substrate vertically; one consists of long black needle-like crystals. I will try to make more of this and experiment with it this winter. I don't have enough of these crystals left to really play with them.

 

Paddler

Edited October 7, 2010 by Paddler

[lws]

That's crazy cool.

[wallylynn]

a few questions:

 

1. can you add this info to the Homemade ink sticky topic? with maybe a link to this thread for discussion.

2. Are you using this in fountain pens, or only dip pens?

3. how does the alcoholic ink compare to fermented ink? (I couldn't tell if you made both, or was waiting to ferment in the future)

3a. Have you tried denatured alcohol instead of rum/vodka? it should make the calculation easier, and cheaper on the wallet (but not tasty and potentially blinding).

4. Is it bad if it turns to vinegar? Most recipes I've seen say to let it ferment and mold.

 

Nice to know I don't need many walnuts to make a small jar of ink. Thanks for the tip of using the dehydrator as an alternative to simmering on the stovetop.

[ag273n]

hmmm.. gets me wondering what other stuff could be made into ink..

[fiberdrunk]

1. The ink has no lubricity. Zilch. It feels like you are writing with plain water. The nib just drags along.

 

 

Thank you for the great info! I wonder if Kodak Photo-flo might help with lubrication? They use it in black & white photo processing.

 

eta: the sample looks beautiful!

Edited October 7, 2010 by fiberdrunk

[DavidHandmade]

1. The ink has no lubricity. Zilch. It feels like you are writing with plain water. The nib just drags along.

 

 

Thank you for the great info! I wonder if Kodak Photo-flo might help with lubrication? They use it in black & white photo processing.

 

eta: the sample looks beautiful!

 

With no background in chemistry, physics, or ink recipe experimentation, I'll ask a naive question or two:

 

What about using mineral oil or castor oil, or something similar to aid "lubricity"?

 

I realize that oil & water don't mix - but, could you create an "emulsification", similar to culinary practices?

 

How about a "synthetic" additive that won't biodegrade in the bottle?

 

- just wondering...

[Northwoods]

I tried glycerine. It doesn't lubricate at all. It could be a preservative; I haven't tested it for that, though. Glycerine is actually an alcohol.

Yes, and hygroscopic, which makes it a good preservative.

 

You can dehydrate the dye completely. If you dehydrate the dye extracted from green husks, you get something resembling tar, probably due to the sugar content. This stuff is difficult to handle. If you let the husks turn black and ferment the sugar away for a couple of months, the dye will dehydrate down to three crystalline fractions: one is brown colored and nearly amorphous; one consists of flat, black squares that grow on the substrate vertically; one consists of long black needle-like crystals. I will try to make more of this and experiment with it this winter. I don't have enough of these crystals left to really play with them.

 

Paddler

 

That is fascinating. I wonder which components are needed? It would be interesting if they weren't all necessary, especially the amorphous brown (though that probably is what creates a lot of the color). That's possibly organic matter, and might be a breeding ground for SITB.

[Paddler]

a few questions:

 

1. can you add this info to the Homemade ink sticky topic? with maybe a link to this thread for discussion.

2. Are you using this in fountain pens, or only dip pens?

3. how does the alcoholic ink compare to fermented ink? (I couldn't tell if you made both, or was waiting to ferment in the future)

3a. Have you tried denatured alcohol instead of rum/vodka? it should make the calculation easier, and cheaper on the wallet (but not tasty and potentially blinding).

4. Is it bad if it turns to vinegar? Most recipes I've seen say to let it ferment and mold.

 

Nice to know I don't need many walnuts to make a small jar of ink. Thanks for the tip of using the dehydrator as an alternative to simmering on the stovetop.

 

1. I was going to put it into the sticky thread, but figured it would get lost in there. There are many pages of discussion and no information like this.

 

2. Dip pens only. I don't have the means to filter this adequately for fountain pens. Even filtered through a pollen filter, this ink settles a little.

 

3. I don't have enough experience with the fermented ink to make a good comparison. I do know that both of them make a good culture medium for bacteria and mold.

 

3a. I did not try denatured alcohol. I figured the methyl alcohol content would make it feather and bleed more. Maybe not.

 

4. If it turned to vinegar, you would have acetic acid in the ink. It takes acetic acid a loooooong time to evaporate. Until then, your letters would smell like a salad. What would the acid do to the paper in the meantime?

 

Paddler

[Paddler]

hmmm.. gets me wondering what other stuff could be made into ink..

 

A good project would be to try hickory nut husks. Hickory is in the same family as walnut and butternut. The husks turn black eventually. Squirrels takes the husks off the nuts for you.

 

Paddler

[DavidHandmade]

hmmm.. gets me wondering what other stuff could be made into ink..

 

A good project would be to try hickory nut husks. Hickory is in the same family as walnut and butternut. The husks turn black eventually. Squirrels takes the husks off the nuts for you.

 

Paddler

 

HEY! I've got a 80+ foot-high Shagbark Hickory Tree in my backyard! The squirrels are ravaging through the canopy now... I'll go out and see if there are any husks worth collecting...

[Paddler]

1. The ink has no lubricity. Zilch. It feels like you are writing with plain water. The nib just drags along.

 

 

Thank you for the great info! I wonder if Kodak Photo-flo might help with lubrication? They use it in black & white photo processing.

 

eta: the sample looks beautiful!

 

I have Photo-flo, but didn't try it for lubrication. It is so active as a wetting agent, I figured it would cause too much feathering. It would be easy to tell. Just dip your pen into it and write. The effect should be most evident that way.

 

The smoothest ink I have ever tried is Japanese and Chinese ink stick ink. That has a substance called "borneol" in it. I wonder where I can get some. Problem is, that stuff oxidizes to make camphor in liquid ink that has been kept for a while.

 

Paddler

[Paddler]

1. The ink has no lubricity. Zilch. It feels like you are writing with plain water. The nib just drags along.

 

 

Thank you for the great info! I wonder if Kodak Photo-flo might help with lubrication? They use it in black & white photo processing.

 

eta: the sample looks beautiful!

 

With no background in chemistry, physics, or ink recipe experimentation, I'll ask a naive question or two:

 

What about using mineral oil or castor oil, or something similar to aid "lubricity"?

 

I realize that oil & water don't mix - but, could you create an "emulsification", similar to culinary practices?

 

How about a "synthetic" additive that won't biodegrade in the bottle?

 

- just wondering...

 

Emulsified oil would never dry. You would have greasy letters. The transparent writing would be interesting.

 

The synthetic additive is the answer. Ink manufacturers evidently use it, but what is it?

 

Paddler

[DavidHandmade]

1. The ink has no lubricity. Zilch. It feels like you are writing with plain water. The nib just drags along.

 

 

Thank you for the great info! I wonder if Kodak Photo-flo might help with lubrication? They use it in black & white photo processing.

 

eta: the sample looks beautiful!

 

With no background in chemistry, physics, or ink recipe experimentation, I'll ask a naive question or two:

 

What about using mineral oil or castor oil, or something similar to aid "lubricity"?

 

I realize that oil & water don't mix - but, could you create an "emulsification", similar to culinary practices?

 

How about a "synthetic" additive that won't biodegrade in the bottle?

 

- just wondering...

 

Emulsified oil would never dry. You would have greasy letters. The transparent writing would be interesting.

 

The synthetic additive is the answer. Ink manufacturers evidently use it, but what is it?

 

Paddler

 

Uhh - well... considering this is a "family" forum, and with all due respect to the sensibilities of all who read this Forum, one or two things come to mind...

 

Are you familiar with certain...um...how can I say..."personal moisturizers"? :embarrassed_smile:

 

...the silicone variety come to mind...

[Paddler]

 

 

That is fascinating. I wonder which components are needed? It would be interesting if they weren't all necessary, especially the amorphous brown (though that probably is what creates a lot of the color). That's possibly organic matter, and might be a breeding ground for SITB.

 

I was considering crystallization as a means to purify the ink. The long, thin crystals should be easy to separate from the others. Do that enough times, and you could have quintessential walnut ink.

 

Another interesting phenomenon: Drip the ink into high proof alcohol and the dye precipitates immediately. Doing this with different alcohol dilutions causes different fractions to precipitate. The last one to fall out has a red color. This one is probably responsible for the warm tone of the ink. I didn't try this with butternut ink.

 

Butternut husks have a really tenacious yellow dye in them. You need steel wool to get it off of a stainless steel chopping knife.

 

There is a lot of interesting work to do here. This winter is going to be fun.

 

Paddler

Edited October 7, 2010 by Paddler

[Paddler]

*snip*

Uhh - well... considering this is a "family" forum, and with all due respect to the sensibilities of all who read this Forum, one or two things come to mind...

 

Are you familiar with certain...um...how can I say..."personal moisturizers"? :embarrassed_smile:

 

...the silicone variety come to mind...

*snip*

 

I tried "Kentucky Jelly". No joy there (so to speak).

 

To my knowledge, silicone is not water soluble. Is there a product that makes it so? Maybe I could buy a packet of "Shmoos" anointed with (Nonoxynol-9?) something. Hey, that might solve two problems: lubricity and biocide. Thanks for the idea.

 

Paddler

[handwriter]

My grandad was a carpenter and he used something called "nogalina" to varnish the wood. In Spanish "nogal" is walnut tree, and hence "nogalina". He made it himself, I do not how, I was a child when he retired and he passed away years ago. I remember the wood treated with it got a dark color. I figure the dye in that stuff was the same as in yours.

I googled "nogalina" and there are several pages about it, like this one (only Spanish, it seems), wher it says that it is extracted from walnut shells:

http://es.wikipedia.org/wiki/Nogalina.

 

In this page, about inks [http://www.caligrafiar.com.ar/v2/taller_05.asp], it says that a solid powder called nogalina can be purchased in wood-related supply stores.

 

It seems that the English for nogalina is "walnut stain", there are plenty of web info on it but guess you already know that.

 

As sources of iron or coper I'd suggest highly soluble salts as iron sulfate and copper sulfate instead of the metals. Iron sulfate (ferrous sulfate) is used as iron supplements to treat iron deficiency and, if I remember correctly, to make iron gall ink. Copper sulfate is a blue crystalline stuff that is in many chemistry sets. As with any chemical, both should be manipulated with due precautions.

[DavidHandmade]

*snip*

Uhh - well... considering this is a "family" forum, and with all due respect to the sensibilities of all who read this Forum, one or two things come to mind...

 

Are you familiar with certain...um...how can I say..."personal moisturizers"? :embarrassed_smile:

 

...the silicone variety come to mind...

*snip*

 

I tried "Kentucky Jelly". No joy there (so to speak).

 

To my knowledge, silicone is not water soluble. Is there a product that makes it so? Maybe I could buy a packet of "Shmoos" anointed with (Nonoxynol-9?) something. Hey, that might solve two problems: lubricity and biocide. Thanks for the idea.

 

Paddler

 

 

Wet makes a product called "Naturals" (or "All Naturals" - something like that - the bottle has a pale violet cap); not silicone-based; holds up in/under water (for a while); it's not totally water soluable, though. -but that might get you over to an "emulsification" again, unfortunately...

 

...hadn't thought of "Shmoos" with the Nonoxynol - great idea, though!

[wood]

The first batch I sent Paddler was over five years old and never grew anything. Like he said I make mine with 100 proof vodka which I use for my herbs anyhow. I have tried many experiments trying to scent the stuff, not that it smells bad but I would have liked to cedar scent the ink. I never had any luck. If anyone in their ink experiments figures out how, please let me know. I can tell you now there is not much of a chemist in me. I've let it sit outside for half a winter then strained and added the alcohol. It still makes ink. My idea of thinning it when I accidentally get too much vodka or too much water when the husks are bleeding out is to leave the lid off for awhile. I tend to avoid anything that requires measuring or math and I still get a good brown ink. If I can make it, anyone can!

 

wood