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Fountain-Pen-Safe Walnut Ink


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#1 PerytonPneuma

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Posted 07 December 2016 - 23:11

Hello all,

 

I would like to start this topic with one goal: making walnut ink that is able to be used in a fountain pen.

 

I have made walnut ink twice before, in 2013 and 2014. I used almost none of it for writing or drawing, and the want to use this ink is what got me into fountain pens in the first place.

 

This year, I have collected a huge amount of walnuts and I am processing them right now. They have been boiled once, and in order to maximize the amount of ink I can get, I will be boiling them again or letting them soak for a long time with fresh, distilled water. Then I will be condensing the ink down to a good concentration.

 

Insofar as I am, I think I have to:

Remove the sugars

Remove the acids

Remove impurities

Preserve it

Add in substances to give it the correct surface tension, dryness/wetness, consistency, and permanence on the page.

 

Anything info, advice, or comments you guys can give is greatly appreciated! Especially anything on what chemicals/things are generally safe and/or unsafe for pens, and, if you know, why exactly they are safe or unsafe.

 

 

My current ideas for removing the sugars:

 

Drying the ink to crystals and COMPLETELY BURNING the ink (like in a crucible, not throwing them into a bonfire). Have to make sure the sugar does not caramelize, as if it completely burns it should only be CO2 and water vapor produced, but if it caramelizes then elemental carbon will be left behind. So unless you want carbon in it (and I don’t know if you could grind it fine enough to put it into a pen), it has to be burned completely.

 

Adding yeast and fermenting until the yeast no longer grows. Then boiling off the alcohol and adding more yeast; repeating until yeast no longer has anything left to ferment. Making sure to seal the container when fermenting; if the yeast has oxygen, then it will start making acetic acid (vinegar) eventually. Would letting it mold have the same effect, or be beneficial? I heard once that it is good to let it mold, but I do not know if that is true or not.

 

I have tested to see if there are even sugars needing to be removed (as even if sugars do not impair pen functionality, I don't want them in there). I took some walnut hull liquor and put some yeast in it, then capped it tightly and let it sit for a few days. It smelled like alcohol afterwards. As a control, I did the same thing with about the same ammount of water as I had of walnut juice, and it smelled only a tiny bit like alcohol; not at all as strongly as the walnuts did.

 

 

For removing the acids:

 

I've heard of adding hydrochloric acid, which I actually should have some of, but this seems risky and I don't know enough of the science behind it to feel certain that adding two acids together can actually cancel out.

There was some form of hydroxide that someone mentioned adding to neutralize acid, but I can not remember what kind it was. HOK? I don't know. I will have to learn more about pH; my other ideas are lye or washing soda, but I do not know if those are good ideas for pen use. I know lye can react with fats to produce glycerine, which I have heard can be an additive to pen ink, so that is what I am leaning toward most right now--even though there shouldn't be very many oils or fats in the walnut ink at any time in processing.

 

I found somewhere talking about the corrosive properties of iron-gall ink (which is sort of similar to Walnut ink, although I am trying to keep iron out of my ink) that the acids and the iron are what make the ink so aggressive and not archival-friendly. In order to make the best ink possible, I want to get as close to a pH of 7 as possible, and have that pH be as completely stable as possible. I don't think I should have a problem with the iron, as I've been using distilled water, unless the walnut liquor can leech iron out of (it was stained before I used it, so I think it's just plain) steel (my pot). In which case, it would also be damaging to the nib, and I will have to find a way to stop that from happening.

 

 

For preserving it:

 

I do not want to use alcohol as it causes feathering and I don't want to take the chance of harming the plastic, even if pure ethanol that has not been methylated (so, the kind of alcohol that yeast will produce) is safe.

 

In theory, iodine should work great as a preservative. So long as the source iodine does not contain ether, which can break down pen components. Google says that salts or using it elemental, dissolved in solution, is how tincture of iodine is made, so those are the forms I am going to try I think. Given the color of walnut ink and the small volume of iodine needed, the iodine shouldn't have much impact on color at all. Even if does, Lugol's or "white" iodine might work.

I think this would be pen-safe as I heard a rumor that iodine is already an ingredient in some inks. Can anyone attest to this?

 

I have used clove oil before (though not enough), and I could use it again in larger quantities, or use it in addition to iodine. I might buy cloves and add them to the process after fermenting, or I might just buy eugenol if I can find it pure enough.

 

 

For removing impurities:

 

I'm thinking of letting it settle, and then pouring off the liquid. If it is dye based (which I think it is) then there shouldn't be anything lost that is actually important. And after that I plan on running it through a coffee filter. Can particles small enough to go through a coffee filter clog the capillary system of a pen? I don't think so, but I can't test that for sure yet.

 

 

Things to add in:

 

I know the least about the things that I need to add to it to make it flow well and work well.

I have heard the term "surfactants," that lubricants of some kind are a good idea, and have found this bit of info on a page I haven't finished reading yet:

 

"Collectively known as ’vehicle’, these additional ingredients include pH modifiers, humectants to retard premature drying, polymeric resins to impart binding and allied properties, defoamer/antifoaming agents to regulate foam efficiency, wetting agents such as surfactants to control surface properties, biocides to inhibit the fungal and bacterial growth that lead to fouling, and thickeners or rheology modifiers to control ink application." - link

 

I do not know quite what I am going to do, besides not adding gum arabic (which I added to previous year's runs, and I'm glad I found out it isn't fountain pen safe before I dumped a bunch into this year's run).

 

 

I will be updating this thread as I make the ink, and if/when I have a recipe that actually does produce pen-good ink, I will edit this post and add it to the top so it's the first thing people see when they come to this thread. Sorry I don't have pictures for you all right now; imagine, if you will, several orange five-gallon buckets and a stained six-gallon pot all messy with dried splotches of brown. Empty milk-gallon shaped bottles with "great value distilled water" on their labels, mostly clean, piled together. And a concrete floor with a bit of a brown glow in some spots too.

 

I would also like to thank Fiberdrunk for posting about the walnut ink she makes; I remember referring to her notes when I first made mine.

 

Tl;dr, I am trying to make walnut ink pen-friendly and I appreciate any advice you guys can give!

 

---

I'm also new as you can tell and I apologize if it's not okay to post this.


Edited by PerytonPneuma, 08 December 2016 - 11:50.


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#2 inkstainedruth

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Posted 08 December 2016 - 01:50

My understanding is that you *don't* want to use gum arabic if you're going to be putting the ink in a fountain pen.  Beyond that, I'll leave it to the experts to chime in.

If there had been stuff like making ink in my high school chemistry class I would have paid a LOT more attention....  :blush: 

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#3 PerytonPneuma

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Posted 08 December 2016 - 11:48

My understanding is that you *don't* want to use gum arabic if you're going to be putting the ink in a fountain pen.  Beyond that, I'll leave it to the experts to chime in.

 

Thanks! I have heard that it might clog the feeding system and, actually, now that you mention it, I don't think I've head about it's use specifically in fountain pen ink.

 

I'll scratch it off the list; one chemical bites the dust.



#4 PerytonPneuma

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Posted 09 December 2016 - 18:20

An update:

 

I am going to start fermenting out the sugars today.

 

Supposedly one of the bad things about iron gall inks are that they can clog the feed when they oxidize and particles of iron precipitate out. So my thinking is that I could react all of the tannin in solution with iron, and oxidize it until it precipitates out, then filter it out. This should leave me with the walnut dye, which is what I want. It may be, however, that this reaction damages the dye, or bonds with it and will mess it up somehow. Or that the particles of iron, while large enough to clog the capillary system, will be too small for me to catch with filter paper. If it works, it seems like this would take care of most of the acids, and would let it not corrode metal nibs.

 

My other idea is still reacting out the tannins, but keeping the metal in solution. I found somewhere that this kind of reaction can happen with any of the transition metals, and so I'd like to try using other metals. The smallest of the the transition metals would be scandium, but I don't know if I can find a source of that at a resonable price. The other metals I'm thinking about are copper (I love the color, and it would be cool if it made it look more coppery), aluminium (not a transition metal, but maybe), titanium, and maybe nickle. Cobalt would be interesting too, but price is again an issue. In keeping the metals in solution, I am really just hoping that they like to stay in water more than iron does.

 

I'm also thinking about lead (also not a transition metal). Lead is a huge atom, and it should be the easiest to let settle out of soltion.

 

Both lead tannate and copper (cupric) tannate are real chemicals, I've found. I don't know the colors, and I haven't checked the rest of the metals next. Cupric tannate I found here, cited as a pigment: link. So maybe I could find a way to grind it into nanoparticles?

 

Does this approach seem viable to everyone else? Saying it all went to plan, there would still be some acids (like citric acid I think), in there and I am considering using limestone to get those out. This would add calcium (I think calcium carbonate?) and I do not know if taking it back out of the ink (as I would have to do if the particles were clogging) would mean that the ink would then become acidic again. I know pH is not the end-all be-all of ink, and some good inks have very high pH. I think this is okay because the acid evaporates before it eats the paper; if that is the case, and if that happens with the leftover acids in the walnut ink then it should be okay.

 

Edit: also, it says here that activated carbon can filter out tannins. Assuming this is true, and assuming that it will not also filter out the dye, would the other acids still pose a problem with reacting to stainless steel nibs? I can test this by trying the filtering and then trying to react it with iron, but at the moment I do not have any activated charcoal filters.


Edited by PerytonPneuma, 09 December 2016 - 19:49.


#5 El Gordo

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Posted 09 December 2016 - 19:50

Looks like a major project to me ...

 

Some simple questions :

- if you made the ink before and you followed Fiberdrunks guidelines, but did not write with the ink: would it make sense to make it exactly the same and do some testing on that one ?

 

- if you dry the ink into crystals and then completely burning the ink: isn't that going to destroy all the organic matter, including the dye molecules and much more?  Could be turning everything into carbon, no.  OK also suited for making a permanent ink, but not for fountain pens. But how are you going tho differentiate the burning so that the dye survives at temperatures that convert sugars to CO2?

 

I am sorry to say put I have the impression that you did a lot of research, which is good, but that your are mixing up a lot of information from different sources into a very complex, probably expensive, experiment. 

 

May I suggest to do this project in a stepwise manner and start with walnut ink recipes that can be found spread over the net.  Investigate them, look at the comments people have given, especially with respect to FP friendlyness.  What are the problems reported, how did they tackle these (if they did).

With this in mind, do you observe similar things, does it write well, does it attack a cheap nib, ... ?

About all the additives you mention, how much are you going to add? Wouldn't it be best too first look how your basic brew behaves?  If you don't know this, how will you decide what and how much to add? 

 

Well that would be my advice, since you asked for it.  Have fun with your project, but keep it safe. Looking forward to your further exploration.


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#6 PerytonPneuma

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Posted 09 December 2016 - 20:55

Looks like a major project to me ...

 

Some simple questions :

- if you made the ink before and you followed Fiberdrunks guidelines, but did not write with the ink: would it make sense to make it exactly the same and do some testing on that one ?

 

- if you dry the ink into crystals and then completely burning the ink: isn't that going to destroy all the organic matter, including the dye molecules and much more?  Could be turning everything into carbon, no.  OK also suited for making a permanent ink, but not for fountain pens. But how are you going tho differentiate the burning so that the dye survives at temperatures that convert sugars to CO2?

 

I am sorry to say put I have the impression that you did a lot of research, which is good, but that your are mixing up a lot of information from different sources into a very complex, probably expensive, experiment. 

 

May I suggest to do this project in a stepwise manner and start with walnut ink recipes that can be found spread over the net.  Investigate them, look at the comments people have given, especially with respect to FP friendlyness.  What are the problems reported, how did they tackle these (if they did).

With this in mind, do you observe similar things, does it write well, does it attack a cheap nib, ... ?

About all the additives you mention, how much are you going to add? Wouldn't it be best too first look how your basic brew behaves?  If you don't know this, how will you decide what and how much to add? 

 

Well that would be my advice, since you asked for it.  Have fun with your project, but keep it safe. Looking forward to your further exploration.

 

I had not considered the dye burning along with the sugar, but I think you're probably right. That is a very good point. I'll scratch that off the list, thanks for pointing that out!

 

I've already made dip-pen ink out of walnuts, and I still have some from both of my batches. Making more now would be pointless as I'm still not going to write with it. So far it hasn't been that expensive, and although I do want to save money I'm more concerned about the ink being safe. No one seems to be putting it into fountain pens, and I have been looking into people using iron gall (sort of similar) in their pens.

 

And I must have given the wrong impression on adding stuff in--I only want to buy and add what I have to. So I do plan on taking it slow when adding that stuff, and testing it with a dip nib to see what it needs. My older walnut ink had too high of a surface tension; it clung to the nib and would not feed down into the tines, so I do think I will need to add something to counter that. But I don't have a clue what actual chemical it is that I need to add, and that's what I'm trying to figure out.

 

I suppose looking into lubricants is a little bit overboard. I just really want this to be the best ink possible.

 

Thanks for your comment!



#7 PerytonPneuma

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Posted 11 December 2016 - 03:51

Found some good resources, and have a few ideas. I'll post them all up properly tomorrow, and for now just mention that I did find a source suggesting the use of calcium carbonate (in the form of eggshells) to dispel the acid (actually in regard to iron-gall ink, but the chemistry between walnut ink and iron gall is somewhat similar). I don't know if would be okay in a fountain pen though.

 

I'm thinking more and more about all of the people I've come across posting that it's okay to use iron gall inks so long as you flush your pen every few months. It is a comforting thought. I have enough walnut juice that I might make a few different kinds, some iron darkened (the influence of the iron gall chemistry) and some with the just the walnut dye as isolated as I can possibly get it.

 

And I might be letting the walnut juice ferment over Christmas, so the actual experimentation portion of this might not leave the theoretical stage for a while. But I have seen from places that fermenting is good for iron gall ink too -- it breaks down the gallotannic acids to gallic acid, which is better (in some way).

 

Another thing I've noticed is that most recipes don't call for the use of an iron nail or steel wool (like I've used in the past), but iron sulfate. I don't know where the sulfur goes after it reacts, but I'd like to see if it's possible to remove it too. 

 

But I'm rambling now. I'll post more tomorrow.



#8 amberleadavis

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Posted 15 December 2016 - 01:07

Remember to test with pens that aren't too expensive.

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#9 PerytonPneuma

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Posted 16 December 2016 - 15:19

Remember to test with pens that aren't too expensive.

 

I will, I've got a cheap old pen lined up. Thanks!

 

 

Also, I'd like to dump the resources I've gathered so far:

 

http://pubs.acs.org/...rnalCode=jceda8
http://pubs.acs.org/...1021/ed083p1568
https://www.chemistr...1013163.article
http://www.chemistry...hemistry-of-ink
https://en.wikipedia...iki/Gallic_acid
https://sites.google...-iron-gall-inks
https://web.archive....com/links/links
http://irongallink.org/
http://www.worldwide...Ink/chap16.html
http://www.fountainp...c-do-they-need/
http://www.fountainp...-pokeberry-ink/
http://www.ebi.ac.uk...iId=CHEBI:30778
http://www.soci.org/...John_Duffy.ashx
https://www.research...fouling_pigment
http://www.rose.org/...stance-Move.pdf
https://www.google.c...tents/US1361139
http://www.sciencedi...300944006000026
http://irongallink.o..._indexd7ce.html
http://faculty.georg...u/jas2/DYES.pdf
http://link.springer...0971-009-2037-8
https://en.wikipedia.org/wiki/Dye
https://inkophile.wo...-iron-gall-ink/
http://kwzink.com/la...iron-gall-inks/
http://irongallink.o..._indexedde.html
https://www.loc.gov/...ia/IGIPonce.pdf
http://textilelearne...h-reactive.html
http://www.marcuslink.com/pens/ink/
https://en.wikipedia...ki/Reactive_dye
https://sites.google...from-fibredrunk
http://what-when-how...s/ink-analysis/
https://en.wikipedia.../Violet_(color)
http://www.fountainp...s-such-a-thing/
https://en.wikipedia.org/wiki/Aniline
https://sites.google...from-fibredrunk
https://sites.google...jane-austen-ink
http://onlinelibrary...190108/abstract
https://sites.google...all/pomegranate
http://onlinelibrary...1556.x/abstract
https://www.research...ountain_Pen_Ink
http://www.wearingwo...t-natural-dyes/
http://www.wearingwo...r-natural-dyes/
http://www.wearingwo...-use-with-kids/
http://www.platinum-..._about_ink.html
https://www.ncbi.nlm...pubmed/18960252
https://www.loc.gov/...IGIBrostoff.pdf
http://www.sciencein...07/issue6/galls
http://www.dharmatra...active-dye.html
http://citeseerx.ist...p=rep1&type=pdf
https://fountainpend...uction-quality/
http://www.materials...n-gall-inks.php
http://nzic.org.nz/c...Apr09_Smith.pdf
https://en.wikipedia...i/Iron_gall_ink
http://pubs.acs.org/...rnalCode=ancham

 

Most of them have to do with iron gall ink, but not all of them.


Edited by PerytonPneuma, 16 December 2016 - 15:19.


#10 amberleadavis

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Posted 10 January 2017 - 05:35

So are you starting to make them?


Fountain pens are my preferred COLOR DELIVERY SYSTEM (in part because crayons melt in Las Vegas).

 

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