Making Fermented Pokeberry Ink

[fiberdrunk]

  On 8/23/2009 at 1:31 AM, mnpd said:

Fermented Pokeberry Ink Manufacture

 

 

 

After several failed tries, I think I finally succeeded in producing the authentic product. For those who are interested, the process described here makes about 3 ounces of what I believe to be quality and well preserved ink.

 

Since this post was from last year, I'm curious how your ink has held up? Thank you for your original post. I discovered it after I made my own simpler ink today. You can see my ink recipe/sample here. I know my ink won't be permanent. I am curious how long it will last and whether I should store it in the fridge. I found the recipe in a pioneer cookbook at the library.

 

eta: some in this thread questioned the toxicity of poke berries. According to Susan Weed's herbal books, it is the seeds inside the berries that are the toxic part, and those only if crushed and consumed. So don't swallow the crushed seeds!

Edited July 29, 2010 by fiberdrunk

[wallylynn]

Pokeberries are starting to ripen here. Took about 1/2 hour to collect them. Longer than I thought and I only got 3/4 of a bottle of berries.

 

I didn't mash them. I was hoping that they'd ripen more but they've started fermenting already. I'll add more berries once there are more to harvest and top off my bottle. The berries stained my hand, but on paper it was kinda weak. I'll try a bunch of things: reducing/concentrating it, adding rusty nails, etc.

[Doc H]

  On 8/23/2009 at 8:24 PM, mnpd said:

I don't know what ink was used on official documents back in the 16th Century, but lots of references state that the "inkberry" was used on the Declaration.

 

 

The residue in Philip Syng's inkstand indicate that the Declaration was signed with irongall ink....

[Northwoods]

  On 8/13/2010 at 1:09 AM, Doc H said:

  On 8/23/2009 at 8:24 PM, mnpd said:

I don't know what ink was used on official documents back in the 16th Century, but lots of references state that the "inkberry" was used on the Declaration.

 

 

The residue in Philip Syng's inkstand indicate that the Declaration was signed with irongall ink....

 

After reading that about the pokeink and the D of I I did whatever searches I could but couldn't find a reliable substantiation. When the Declaration went to the calligrapher to be officially transcribed, it would have certainly have been written in an iron gall and likely signed with same, but it's possible that Jefferson's drafts could have been done using more household materials, like pokeink.

[fiberdrunk]

  On 8/23/2009 at 1:31 AM, mnpd said:

Fermented Pokeberry Ink Manufacture

 

 

I found some Pokeberry ink “recipes” on the ‘Net, but none that use the fermentation that I suspect is crucial in making in ink that has good shelf life.

 

Finally, the color itself. I've been able to artifically age the ink by leaving the inked paper in direct sunlight for a day. The ink turned orange. Ink written on composition book paper which is kept in the dark hasn’t shown a color shift in several weeks. I don’t know how much time is required before the ink turns to brown, but it seems that exposure to light can be responsible for at least some of the aging.

 

I've got 2 batches of pokeberry ink going (one fermented batch, and one unfermented batch with vinegar and salt). When enough time has passed, I'll post how it holds up to mold and how well the color holds out.

 

One question I have... I noticed after just a few days with the fermented batch, that the ink goes on bright pink, but as soon as it dries, it looks more like a dull lavender or grayish blue. My unfermented batch stays pink on the page, even after dry. Did you get the same results? I don't mind the lavender color, but I was just curious if anyone else got that result. I used a fine-mesh metal strainer rather than a coffee filter... it's possible the metal reacted with something in the fermented berry juice. Or maybe this is just normal? Anyone else try these recipes?

[fiberdrunk]

  On 10/16/2010 at 2:00 AM, fiberdrunk said:

 

One question I have... I noticed after just a few days with the fermented batch, that the ink goes on bright pink, but as soon as it dries, it looks more like a dull lavender or grayish blue. My unfermented batch stays pink on the page, even after dry. Did you get the same results? I don't mind the lavender color, but I was just curious if anyone else got that result. I used a fine-mesh metal strainer rather than a coffee filter... it's possible the metal reacted with something in the fermented berry juice. Or maybe this is just normal? Anyone else try these recipes?

 

OK, I think I figured this out. It was the paper causing the most rapid color change! I used Hammermill Ultra Premium Inkjet paper (acid-free) and it caused the fermented pokeberry ink to turn lavender upon drying on the page (and a nice gray by the next day). It doesn't do this on Strathmore Calligraphy Paper. The non-fermented pokeberry batch has retained its pink color on both papers. Go figure!

 

eta: I know that pokeberry is fugitive and turns brown, so I was expecting that, but not lavender and gray! lol

Edited October 18, 2010 by fiberdrunk

[wallylynn]

I read on one of the websites that discuss your use of vinegar and salt that pokeberry is similar to litmus (and red cabbage and hydrangeas) and that it'll change color depending on how alkaline or acidic it is. It said the vinegar helps to keep the acidity and the red/pink color. Maybe something in the acid-free paper is actively neutralizing the acid in the pokeberry. Just a guess...

 

My pokeberries seem to have stopped fermenting. Time to find a little jar and make a quill.

[Paddler]

You folks are doing good work. Keep posting. What you find out is interesting to many others!

 

Paddler

[fiberdrunk]

Another update. My fermented pokeberry ink no longer turns lavender upon drying on the page. Now it turns a light gray (it's magenta wet, then immediately turns gray).

 

My non-fermented ink (with the apple cider vinegar and salt) has still retained its same magenta color as the day I made it (so far). I'm expecting them both to turn brown soon.

 

I noticed there are pokeberry ink sellers on both eBay and Etsy this fall (black walnut ink, too).

Edited November 2, 2010 by fiberdrunk

[fiberdrunk]

Another update. I'd have to say my fermented pokeberry ink experiment is failing, lol. The bottles keep building up pressure and today I had a nice magenta ink explosion, lol. :gaah: I also noticed the fermented ink had a film that began to grow on top of the ink after only about 2 weeks. Obviously, my ink is still very biologically active. I don't know what the solution is. Would adding alcohol make it worse? If I were to heat the ink after fermentation, that would stop the fermentation, but could possibly adversely affect the magenta color. On the other hand, the non-fermented pokeberry ink (with apple cider vinegar and salt for a preservative) has not caused any explosions and has retained its color nicely (so far).

 

You can see color samples of both inks here. The first one is on acid-free Strathmore calligraphy rag paper. I show how many days old the ink is on the first sample, to show how fast the color has degraded. The second one is on cheap composition graph paper, which suffered even more color degradation with the fermented pokeberry ink. It turned brown within hours. (I did expect both inks to turn brown eventually, but not quite this fast.) The fermented ink has a greater tendency towards feathering as well.

 

Did anyone else encounter exploding ink with the fermented recipe? My ink is kept in a cool room (65 F, even colder at night). The ink was not bottled until it had finished the 24-hour fermenting period. Only then it was bottled, but it still builds up pressure. If I don't use the fermented ink every few days or so, it builds up too much pressure inside. I think in the future I'll stick with the vinegar/salt recipe. How's everyone else doing with their ink? (By the way, the non-fermented recipe I used can be seen here.)

 

eta: for grammos

Edited November 8, 2010 by fiberdrunk

[wallylynn]

Most likely 24 hrs wasn't enough to complete the fermentation. Mine kept building up pressure for a month, I had to leave the bottle cap slightly loose.

 

My sample test has also turned brown for the most part. It was mixed inside a stack of papers so it wasn't light that did it. The berries are still inside the bottle but the cap is now tight, it's not fermenting anymore. No mold yet. I don't have another bottle to put the ink into.

[fiberdrunk]

  On 11/8/2010 at 2:29 AM, wallylynn said:

Most likely 24 hrs wasn't enough to complete the fermentation. Mine kept building up pressure for a month, I had to leave the bottle cap slightly loose.

 

My sample test has also turned brown for the most part. It was mixed inside a stack of papers so it wasn't light that did it. The berries are still inside the bottle but the cap is now tight, it's not fermenting anymore. No mold yet. I don't have another bottle to put the ink into.

 

Thanks for the tip. I'll try leaving the lid off partially. I've also dropped some whole cloves in. I'd still like to try to salvage what is left, just in the interest of seeing how the ink ages and such. I'm a process-oriented person and enjoy working through problems like this, trying to figure them out. My writing samples were kept in the dark as well, so I know that wasn't it. The fermented ink retains its pink color better on acid-free paper than on non acid-free, I've found, except for Hammermill Ink Jet Paper which is acid-free... they must coat it with something that reacts unfavorably with pokeberry ink.

 

ETA: as messes go, at least it was a pretty one

Edited November 8, 2010 by fiberdrunk

[fiberdrunk]

My fermented pokeberry ink did finally stabilize. I left the lid off the ink for a few weeks and tossed a couple of whole cloves into it (for a preservative). It's now a nice deep purple. You can see a comparison of colors between the non-fermented batch I made and the fermented one below. The non-fermented pokeberry ink (with cider vinegar and salt for a preservative) still has that bright magenta and has never changed. But it's nice to have 2 different shades of ink, all from one berry. (Note: on some papers, the fermented pokeberry turns brown fast.)

 

I'm also wondering, since the fermented pokeberry is prone to feathering on some papers, if that might improve with the addition of gum Arabic? Has anyone tried adding that to their pokeberry ink?

 

http://farm6.static.flickr.com/5124/5357615970_1982dc18bb_z.jpg

Edited January 16, 2011 by fiberdrunk

[Gobblecup]

Wow, very interesting! How did you make the Walnut Iron Gall ink?

[fiberdrunk]

  On 1/18/2011 at 8:28 PM, Gobblecup said:

Wow, very interesting! How did you make the Walnut Iron Gall ink?

 

I totally missed this question. I blogged about how I made this ink here. But basically I did a batch of black walnut ink and added steel wool to it at one point to impart the iron.

[Jenzum]

  On 8/23/2009 at 1:31 AM, mnpd said:

Fermented Pokeberry Ink Manufacture

 

Re: "The Declaration of Independence was reportedly written in fermented Pokeberry Ink:" I've seen this statement about the Declaration of Independence being written in pokeberry juice ink in a lot of places on the Internet, but the first forumulation of pokeberry juice ink was well documented in primary sources as having occurred in 1815-- well after the writing of the Declaration of Independence.

 

Here's a transcription of a news article from the 3 April 1816 edition of the "Intelligencer":

 

"Mr. [Laurence A.] Washington of Buffalo [Virginia] has discovered that the juice of Pokeberry Phytolacca Decandra makes excellent red ink-- He gathered the berries in October [1815], squeezed the juice, and passed it through a flannel bag-- After having gone through a fermentation, he filtered it through linen, and then through paper-- After standing a few weeks, he added certain portions of alum and alcohol, when it became ink of a most beautiful color.

 

It has often been thought that the Phytolacca Decandra was capable of being brought to valuable uses both as to colours and medicinal purposes-- It is an indigenous plant, and enters into our Materia Medica-- See the works of Drs. Barton and Thatcher-- Its dying qualities, when properly managed, can not now be doubted."

 

A number of other newspaper articles dating from 1816 include excerpts of a letter from the inventor describing his experimentation process in more detail. --Jenzum

[fiberdrunk]

Fascinating! I wonder what his proportions of alum and alcohol were? I'll have to try this next year. When I did the fermented recipe last year, I didn't use alum or alcohol and the ink eventually molded over. It was also highly changeable before it molded. Thanks for sharing!

Edited October 10, 2011 by fiberdrunk

[Patrician]

  On 8/23/2009 at 2:29 PM, psfred said:

The Declaration of Independence, is, of course, written in iron/gall ink, as all permanent documents were at the time. Fermenting poke berries will add some alcohol (which you could provide by tipping in some denatured alcohol) and probably adds some glycerol that acts as a nice flow modifier (no feathering, smooth writing).

 

I don't think you will make the ink any more resistant to fading, though, unless you add some iron to react with the tannins and make ferro-gallic ink.

 

Pokeberry in was quite common in the early days of the US, but everyone knew it faded badly. Iron gall ink was well known, and anyone interested in permanence would have used it instead, or added the green copperas to the pokeberry ink to make it iron gall.

 

Peter

 

Peter

 

A close relative, a curator, took part of a team of experts trying to solve the fading and degradation of the document to no avail. It is written using a home made poke-berry concoction, not (British) ferrogalic ink. And the results of the experiment hasn't withstood time.

[Jenzum]

  On 10/18/2011 at 4:27 AM, Patrician said:

  On 8/23/2009 at 2:29 PM, psfred said:

The Declaration of Independence, is, of course, written in iron/gall ink, as all permanent documents were at the time. Fermenting poke berries will add some alcohol (which you could provide by tipping in some denatured alcohol) and probably adds some glycerol that acts as a nice flow modifier (no feathering, smooth writing).

 

I don't think you will make the ink any more resistant to fading, though, unless you add some iron to react with the tannins and make ferro-gallic ink.

 

Pokeberry in was quite common in the early days of the US, but everyone knew it faded badly. Iron gall ink was well known, and anyone interested in permanence would have used it instead, or added the green copperas to the pokeberry ink to make it iron gall.

 

Peter

 

Peter

 

A close relative, a curator, took part of a team of experts trying to solve the fading and degradation of the document to no avail. It is written using a home made poke-berry concoction, not (British) ferrogalic ink. And the results of the experiment hasn't withstood time.

 

 

Hi, curators at the National Archives--the repository of the Declaration of Independence--say that the Declaration was engrossed with iron gall ink. In the 1800s, it was well accepted that a wet copying procedure which removed a significant quantity of ink from the original document was undertaken; though now, for some reason never explained, we are told that there is some question about this. What are the facts behind the controversy? Can your curator expert tell us? I have read that the 1820-1823 copies were suspected to have been made from a wet press operation with a copper plate; however the earlier 1818 copies made by Benjamin Owen Tyler were "curiously exact imitations" of the original, down to the smallest detail, suggesting that there may have been more than one wet press operation which damaged the document. Add to that the fact that the declaration was carried around, rolled, and even folded! and then placed on display with no atmospheric controls whatsoever for thirty years before it was retired into a safe and brought out only for special occasions. It's no wonder there was significant degradation of the document. Did the panel of experts publish their findings? How can I find out more? Thanks for your time, Jenzum

[farmerjohn]

While I am new to pens I have been brewing my own wine since middle school and am a science geek so hopefully I can help out in those areas

  On 8/23/2009 at 8:43 PM, ZeissIkon said:

Probably not. The fermentation preserves the berry juice as much by removing the sugars that would be primary food for bacteria as by adding alcohol (since I think it very unlikely you produce enough alcohol to make the mix antiseptic; yeast won't tolerate more than 14% and antiseptics are generally 30% or stronger). Add enough alcohol to prevent spoilage and you'll risk damaging pens that are made of materials incompatible with alcohol (which is most of them), though the ink would still be usable with a dip pen.

I think it very unlikely that an ink well known to fade would be used on what the Founding Fathers considered an important document, though it's very possible it was used for day to day applications. However, as noted, the color of the berries strongly implies a high tannin content (as does the ink turning orange in the sun -- the purple fades, but orange tannin doesn't, or fades much more slowly), so simply adding some copperas to the fermented ink would convert it to a much more permanent type, and the purple color would serve to make it easier to see the writing while waiting for the oxidation color to appear.

there are many yeasts that will tolerate much higher just have to shop around for the right culture

 

  On 8/24/2009 at 12:47 AM, psfred said:

Also, if you ferment the berries in an iron pot, guess what? Ferro-gallate ink! Or more likely, add a few rusty nails.

I may have to try this, as pokeberries are hardly uncommon around here....

Peter

I do not know that the iron in the pot would be sufficient to make a complete reaction would probably be better to use iron2 sulfate (FeSO4) and about $10 for 500grams (this is what was used in iron gall inks and why alot of traditional iron gall inks had high sulfuric acid content vs modern inks using hydrochloric

 

 

  On 8/28/2009 at 2:01 AM, marpin said:

I'm not sure just how bad these berries actually are... I came across an old publication where the authors tried pretty hard to kill mice with them, without too much luck. Of course, seeing as the toxicity is due to secondary metabolites, there is quite possibly a wide variation in toxic dose between different cultivars, or plants grown in different conditions, or harvested a different times. And there's always the issue that mice might respond rather differently to men.
http://digital.library.okstate.edu/oas/oas.../v43/p54_57.pdf

If the pigment is due to anthocyanins, then there are ways to produce crude extracts. Unsurprisingly, most involve chromatography, though I found a few bulk procedures. In particular, from http://www.freshpatents.com/-dt20090416ptan20090099373.php:
"Lietti, in U.S. Pat. No. 4,413,004, discloses a method of extracting anthocyanins from bilberry by extracting the fruit with anhydrous methanol containing hydrochloric acid, followed by adding lead acetate to precipitate the anthocyanins as the lead salts."
and from Elisia et al (2007) Food Chem. 101(3):1052-1058:
"Four batches of 100 g of frozen blackberry were blended with 100 ml of 80% (v/v) ethanol using a Waring blender for 5 min. The slurry was transferred to an Erlenmeyer flask, and extracted overnight. The extract was filtered through a Buchner funnel using Whatman filter paper (No. 1) and rinsed twice with 25 ml of 80% ethanol. The filter cake was transferred to a new Erlenmeyer flask and was re-extracted with 150 ml of 80% ethanol using an orbital shaker at 400 rpm (Innova 4000, New Brunswick Scientific, NJ) for 1 h. The filter cake was extracted for the third time with 80% ethanol overnight and all filtrates were pooled together. Sample extractions were performed in quadruplet. The ethanol in the pooled filtrate was removed under vacuum at 35 °C. The residue was then freeze-dried and kept at 4 °C."

BTW, the toxic principle in castor beans is a ribosomal inhibitor (cleaves 28S rRNA), not a neurotoxin.

Thanks I love experiments to do with my organ chem. set ^ just made my day experiment to come next summer

 

  On 11/7/2010 at 11:35 PM, fiberdrunk said:

Another update. I'd have to say my fermented pokeberry ink experiment is failing, lol. The bottles keep building up pressure and today I had a nice magenta ink explosion, lol. :gaah: I also noticed the fermented ink had a film that began to grow on top of the ink after only about 2 weeks. Obviously, my ink is still very biologically active. I don't know what the solution is. Would adding alcohol make it worse? If I were to heat the ink after fermentation, that would stop the fermentation, but could possibly adversely affect the magenta color. On the other hand, the non-fermented pokeberry ink (with apple cider vinegar and salt for a preservative) has not caused any explosions and has retained its color nicely (so far).

You can see color samples of both inks here. The first one is on acid-free Strathmore calligraphy rag paper. I show how many days old the ink is on the first sample, to show how fast the color has degraded. The second one is on cheap composition graph paper, which suffered even more color degradation with the fermented pokeberry ink. It turned brown within hours. (I did expect both inks to turn brown eventually, but not quite this fast.) The fermented ink has a greater tendency towards feathering as well.

Did anyone else encounter exploding ink with the fermented recipe? My ink is kept in a cool room (65 F, even colder at night). The ink was not bottled until it had finished the 24-hour fermenting period. Only then it was bottled, but it still builds up pressure. If I don't use the fermented ink every few days or so, it builds up too much pressure inside. I think in the future I'll stick with the vinegar/salt recipe. How's everyone else doing with their ink? (By the way, the non-fermented recipe I used can be seen here.)

eta: for grammos

 

 

  On 11/8/2010 at 3:20 AM, fiberdrunk said:

Thanks for the tip. I'll try leaving the lid off partially. I've also dropped some whole cloves in. I'd still like to try to salvage what is left, just in the interest of seeing how the ink ages and such. I'm a process-oriented person and enjoy working through problems like this, trying to figure them out. My writing samples were kept in the dark as well, so I know that wasn't it. The fermented ink retains its pink color better on acid-free paper than on non acid-free, I've found, except for Hammermill Ink Jet Paper which is acid-free... they must coat it with something that reacts unfavorably with pokeberry ink.

ETA: as messes go, at least it was a pretty one

LOL^ sounds like my first brewing attempt when I was in middle school the bottles exploded. What is happening is that the time you did not give the yeast enough time to convert all the sugars to alcohols so even if your filtration got rid of all the yeast there is enough food present for wild bacteria and yeasts to grow

 

my advice would be for your next batch try using white labs WLP099 yeast it yields up to 25% alcohol by volume (about $7 for a culture) and I would recommend using a clean glass container with a brewing air lock (about $2-4and reusable ) but if you want to do it as cheap as possible you could use a 1 gallon milk jug cleaned and sanitized well.

would look something like this

http://www.stormthecastle.com/mead/images/visitors-mead-pictures/seans-mead.JPG

keeping the air lock on it for 2-3 weeks would allow most of the sugar to be consumed and the yeast to go dormant as well as a lot of sediment settling to the bottom so you have less work when it comes time to filter just siphon off all but last 2 inches or so. most folks making wine typically let it sit in the carboy at least two weeks I tend to go 4 I wait two siphon off to another container then let settle another two then syphon and bottle.

 

note: do not fill the carboy/container more than 2/3s full to allow for the yeast/froth layer

 

 

  On 10/10/2011 at 3:02 PM, fiberdrunk said:

Fascinating! I wonder what his proportions of alum and alcohol were? I'll have to try this next year. When I did the fermented recipe last year, I didn't use alum or alcohol and the ink eventually molded over. It was also highly changeable before it molded. Thanks for sharing!

The reason it molded over is the alcohol content was too low typically anything over 20% ABV will not go bad might want to get some pure grain spirits from the liquor store and add enough to put it over that thresh hold, as for the alum I would imagine it was used as a preservative seeing it is used as a pickling agent in foods as well as in tanning leather