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Home Made Ink (Mostly Ig) & **tips And Tricks**


Sakura

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Wow Zeiss... you've done so much within a week! I was supposed to have started my ink on Monday, but I couldn't find the steel wool then I had a bunch of tests for school this week. :( Hopefully tomorrow I can get started. And 850mL?! That's a lot! That must be on large mason jar you're using... I was hoping to just use small quart ones for my experiment. :P Then transfer 'em on over to baby food jars when I'm done.

 

As for the chemical experiment...

 

PGary, what is the chemical formula for the chelate compound that FeSO4 and C6H2(OH)3COOH that you mentioned? From what I can remember in Chemistry, those should be the formulas for Ferrous Sulfate (Iron II Sulfate) and Gallic Acid... When balancing the equation, should I have H2O present in the equation or would the water be added until I like the consistency? I understand that I should have 1 mol of each of the ferrous sulfate and gallic acid, but what about the water? :)

 

Thanks for your contributions! :D This is fun.

 

-- Moo

 

**ETA: Just thought of this question as I was going to the kitchen... Do you think iron supplements would work for this experiment? I know it's not all iron, as there are fillers, coatings, etc. in those pills. I wonder if any of those fillers would have any sort of chemical reaction with the vinegar and tannin. A new experiment this will be! :)

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Hello mooshisho,

 

I think that the following page answers your question.

http://www.scienceinschool.org/repository/docs/issue6_galls.pdf

Because ferric gallate was precipitated in water, it is necessary to avoid oxidation of ferrous iron to ferric iron.

Therefore, iron gall ink is acidified and made with degassed water.

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Because ferric gallate was precipitated in water, it is necessary to avoid oxidation of ferrous iron to ferric iron.

Therefore, iron gall ink is acidified and made with degassed water.

 

Interesting -- I haven't been using degassed (or even distilled) water. I see a suggestion here, however, that it might be a bad idea to neutralize my ink's acidity, lest the iron oxidize to the ferric form and precipitate (though from the linked article, I understand it's ferric pyrogallate that actually makes the ink black; black ink in the bottle, however, can still be almost invisible on the page, so I'll settle for adding dye to mine). My ink has been protected from oxygen, sitting and reacting in a closed mason jar (it's a quart jar, BTW; an American quart is about 950 ml). Perhaps this is why it's still reddish, though considerably darker than it was on Sunday. It's well along in consuming the third steel wool ball, and a sample (taken on a bamboo skewer) wrote darker than it did a couple days ago; as well, the ink continues to darken for up to twenty-four hours, though it also seems to turn from gray to brownish over that time (perhaps that's that Fenton reaction, though I gathered that was something you'd expect over archaeological time).

 

Tomorrow, I plan to go buy some fabric dye, and bake some corn starch into dextrin to serve as the gum in the ink (though since I hope to use this ink in a fountain pen, I'll keep the gum to a minimum; I can always add more, but it's hard to take it out). In the evening, I'll filter the ink and mix in the dye and gum, and hopefully I'll be able to post some writing samples, maybe even a cell-phone or digital camera video of the ink darkening, in the evening.

Does not always write loving messages.

Does not always foot up columns correctly.

Does not always sign big checks.

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Thanks for the link, PGary, I learned a lot. :)

 

haha Zeiss... a quart jar is still quite the amount of ink~! :)

 

How does the RIT dye work as an ink? Dip pen only or alright for cartridge fill? Would I be following the directions on the package or some other proportion of dye to water...? :) I couldn't find the thread you were referring to... :(

 

The dextrin SHOULD be water soluble... to an extent. I believe that there would be a precipitate found if it were to be in alcohol though. Too much dextrin : water would make it more like an adhesive, correct?

 

-- Moo

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Hello ZeissIkon,

 

Thank you for your comment, and your research of the iron gall ink is quite interesting.

I think that your thought is correct.

The iron gall ink without dye looks like black in the bottle, but transparent or pale black when immediately writing and turn black by slow degrees.

Movie of this reaction is in my blog.

I provide the information about the dye reagents that do not precipitate with base solution of iron gall ink.

From what I tested.

 

1. Direct Blue 1 (Chicago Sky Blue 6B, Pontamine Sky Blue 6B)

2. Acid Blue 92 (Acid Blue A, Anazolene Sodium)

3. Food Blue No.1 (Brilliant Blue FCF)

4. Food green No.3 (Fast green FCF)

5. Food Yellow No.4 (Tartrazine)

6. Food Yellow No.5 (Sunset Yellow FCF)

7. Food Red No.2 (Amaranth)

8. Food Red No.40 (Allura Red AC)

9. Food Red No.102 (New Coccine)

10. Food Red No.106 (Acid Red)

 

I hope you find it informative.

Edited by pgary
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Since the last report, the ink rather abruptly (over Friday night, at most about ten hours) turned from a red-brown solution to a nice, deep black, and quit eating the steel wool, leaving about 1/8 of the mass of the last ball unreacted. I filtered the ink, then added fabric dye to make the result visible when first written on paper (even after the solution turned black, the writing was almost invisible when it first came off the pen). The resulting ink acts like, well, ink, at least on a dip pen, without any other additives, but it's pretty weak; it's a faint blue when first written, and darkens to a blue-gray after a few minutes. At least on the one paper I've tested on, it doesn't spread or bleed at all (I was concerned there might be too much surfactant in the dye), and the consistency is somewhere between water and fountain pen ink; I'll probably add a tiny bit of dextrin to thicken it after a bit. At present, however, the ink is in a double boiler arrangement on the stove, hopefully to evaporate off at least 1/4 to 1/3 of the volume. I'm confident both the color dye and the iron pigment will survive this treatment; many of the old ink recipes include boiling the ink to strengthen it after mixing, and the RIT dye includes instructions to dissolve in boiling water for some techniques.

 

Moo, dextrin is soluble enough for the amount needed to act as the gum in an ink -- since I hope to use this in fountain pens, the amount of gum will be very low (it may not need gum at all, once I've evaporated -- what a cook would call "reduced" -- the ink). The RIT dye (I bought Navy Blue) gave information about pre-dissolving the dye in a cup of boiling water for some methods; since I had almost a cup of space left in my jar after filtering the ink, I dissolved the dye that way and poured as much of the cupful as would fit into the jar (about six ounces). The jar I have is apparently not quite a quart, or the markings are inaccurate; it was at 24 ounces, and six ounces of dye solution brought it as close to the top as was comfortable.

 

Yes, that's a lot of ink, but it just wasn't practical to make a smaller batch, and for what it costs (I'm under four dollars for this batch, including the dye), it's a reasonable experiment.

Does not always write loving messages.

Does not always foot up columns correctly.

Does not always sign big checks.

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I've finally started my experiment! :) Since I didn't have any of the larger jars available, I just decided to work on a TINY amount for now; baby food jar sized. I think it's the 4oz jar. I put 31.25mL vinegar, threw in enough steel wool for the vinegar to do it's thing, then another 31.25mL of steeped black tea. Instantly, the mixture turned a dark blue/black. The next morning, I woke up to find the steel wool sludge with a bit that hasn't been eaten up yet and the mixture a dark reddish-brown. I put in some fresh steel wool to make sure that the reaction was going properly and will wait a couple of days to see what happens next. :) So far the "test" writings have turned out well.

 

Within the first few hours, it was clear upon writing and slowly became a darkish brown (just enough to be legible). Today (about 10 hours later), the writing had more colour to it and then slowly became darker. :)

 

-- Moo

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De Coloribus et Artibus Romanorum (13th C.), translated by Mary Merrifield.

 

LIII. [243] How atramentum of various kinds is made. — The method of making ink is as follows, for it is necessary, not only for use in painting, but even for every day writing. A vase is put into a hollow chamber ; and a furnace is made so as to have nostrils, that is, apertures, through which the smoke can penetrate into the vase. Some tiles must then be laid in the furnace, and upon these hot tiles resin must be put, so as to drive all the smoke and soot into the vase. Afterwards grind the soot very fine, and you will make a very bright atramentum, with which you must mix painter's size. To accelerate the process, soft charcoal of wood, or of peach-stones, ground up with glue, is useful. Charred twigs also will imitate the appearance of atramentum; but the blackest twigs must be used. If good wine is poured over them, and glue be added, they will form a colour which will appear to imitate the softness of daylight.

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After boiling my ink down to half its previous volume, it appears to work well enough with a dip pen; it's still rather light purple-blue when first written, but then darkens to a deep gray, turning brownish over about twenty-four hours (the Fenton reaction?). I inked it in my Osmiroid 75 (piston filler that can be completely disassembled for cleaning), but it seemed dry in that pen; I'd probably need to add some additional detergent to get good flow, which in turn would require some gum to prevent excessive spreading. As is, the ink writes nicely with an italic dip pen, so I'm going to leave it as is. Now I need to find an ink well; it's inconvenient to dip the pen in a quart jar, now that there's only a pint of ink...

Does not always write loving messages.

Does not always foot up columns correctly.

Does not always sign big checks.

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ZeissIkon, congratulations on your ink! I use shot glasses for temporary ink wells. They make good nib-soaking glasses, too.

May you have pens you enjoy, with plenty of paper and ink. :)

Please use only my FPN name "Gran" in your posts. Thanks very much!

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Sweet, Zeiss~! :) How about some writing samplessss? :D

 

My ink... let's see. I've been adding some more steel wool each night, and when I wake up, there's a reddish-brown mixture at the bottom, some new sludge and the steel wool floats to the top. Do I keep adding wool until new sludge stops? Is the mixture supposed to be black when the mixture is done (as opposed to my red/brown)? At the moment, there's a separation, but once I push the steel wool down, it'll turn black again.

 

-- Moo

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ZeissIkon, congratulations on your ink! I use shot glasses for temporary ink wells. They make good nib-soaking glasses, too.

 

Ah, nice thought -- I'll have to look for some at Dollar Tree next time I'm over that way. Currently, the only shot glasses I own are dedicated for the espresso machine.

 

Sweet, Zeiss~! :) How about some writing samplessss? :D

 

My ink... let's see. I've been adding some more steel wool each night, and when I wake up, there's a reddish-brown mixture at the bottom, some new sludge and the steel wool floats to the top. Do I keep adding wool until new sludge stops? Is the mixture supposed to be black when the mixture is done (as opposed to my red/brown)? At the moment, there's a separation, but once I push the steel wool down, it'll turn black again.

 

-- Moo

 

I added steel wool when the previous was all used up, and saw "black" only when I stirred up the residue at the bottom, until the whole thing "suddenly" turned black over Friday night, and then stayed that way. The steel wool floats because it has gas bubbles caught in it; that indicates it's reacting (the gas is probably hydrogen released from one of the acids as it reacts with the iron). It'll stop separating and turn a nice, solid black when it's done. I think -- you used vinegar instead of battery acid, so yours may react faster or slower than mine.

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Does not always foot up columns correctly.

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Here's the writing sample that was requested; this scan is adjusted to match the color of the paper and ink, as best my screen and eye can do. It's a very large file (about 2.2 MB), so I'm posting a linked thumbnail to spare dial-up users. If you click through the link, you can click on the image at Photobucket to get the full size scanned image (300 ppi).

 

http://i11.photobucket.com/albums/a183/dqualls/th_Iron-GallInkonSmartMossWritingPaper.jpg

 

The ink settles, and needs to be stirred before use or it's very faint. It goes on a light purple-blue, and is pretty slow drying on the two papers I've tried it on so far, but it darkens up nicely as it dries. The first sample I wrote after boiling down the ink turned rust brown in 24 hours, but this sample doen't seem to be browning (or at least not as rapidly); I'm not sure if that's due to different paper, or if the ink is still aging.

 

The sample is on Smart brand Moss color writing paper, purchased at Big Lots, a ream of 500 sheets for $5. I used a Perry & Co. Eastern Wonder pen (purchased from jbb) previously "broken in" with black ink jet refill ink, and got one to two lines per dip. I've also tried this ink briefly in a fountain pen; it doesn't flow enough to write well, though adding some detergent might improve that.

Does not always write loving messages.

Does not always foot up columns correctly.

Does not always sign big checks.

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Thanks for the ink sample. The ink and paper combo looks quite antique.

"My two fingers on a typewriter have never connected with my brain. My hand on a pen does. A fountain pen, of course. Ball-point pens are only good for filling out forms on a plane." - Graham Greene

 

"The palest ink is better than the best memory." - Chinese Proverb

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The first sample I wrote after boiling down the ink turned rust brown in 24 hours, but this sample doen't seem to be browning (or at least not as rapidly); I'm not sure if that's due to different paper, or if the ink is still aging.

 

Probably because the ink had too much iron in it.

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The first sample I wrote after boiling down the ink turned rust brown in 24 hours, but this sample doen't seem to be browning (or at least not as rapidly); I'm not sure if that's due to different paper, or if the ink is still aging.

 

Probably because the ink had too much iron in it.

 

Entirely possible. The good news for this, if you will, is that ink that's saturated with iron (as this ink is; the reaction that was eating the steel wool stopped before the third ball was completely consumed) won't corrode steel nibs. BTW, another sample, written late last night in my journal on a third paper type, had browned by this afternoon.

 

The bad news is that, from what I've read, iron-gall ink that turns brown is likely to eat the paper, because the excess iron also represents excess sulfate and it's the sulfate that damages paper. I could probably precipitate the sulfate, if I were very concerned about it: adding chalk (calcum carbonate) should do it; it would react to form gypsum (calcium sulfate), which is only very slightly soluble and could then be filtered out along with the ferrous hydroxide or ferrous oxide that forms from the orphaned iron. I'm not really that concerned about it, however; first, I want to see if I can reproduce the result based on how wet the pen was writing. The sample posted here was writing very wet and dark, while the writing in my journal, like the original tests, was much drier. If making the ink write wetter prevents the browning, I can add some detergent and make it write wetter on everything (that'll also make it work better in a fountain pen; it's currently worse than trying to write with plain water in my Osmiroid).

Does not always write loving messages.

Does not always foot up columns correctly.

Does not always sign big checks.

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ZI, your ink is beautiful! Congratulations!

 

Professionaldilettante, did you mean to include a link in your post? I couldn't find it

May you have pens you enjoy, with plenty of paper and ink. :)

Please use only my FPN name "Gran" in your posts. Thanks very much!

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ZI, your ink is beautiful! Congratulations!

 

Thanks, Gran! It's very gratifying for something so cheap and easy to make to work so well, and it's fascinating to watch the ink (very slowly) change from blue to black as it dries and oxidizes. I may have to change nibs and try it with my fine spoon point dip pens, and of course I'll be attempting to make a sample wet enough to write well in a fountain pen (a dollar's worth of this ink, even after boiling down, will replace about fifteen dollars worth of commercial ink).

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Does not always foot up columns correctly.

Does not always sign big checks.

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Another follow-up on my homemade iron tannate ink. As reported last time, I was planning to try to modify the flow of the ink to make it wet enough for a fountain pen. After some failed attempts, I disassembled my Osmiroid 75 again, cleared out the feed channels and scraped some "junk" off the feed surface that contacts the nib (probably inadequately cleaned residue from a previous experiment with a carbon particle ink that turned not not to be completely FP safe), and tried it again, and it does in fact write successfully in a fountain pen, though it's still a little on the dry side and doesn't coat the ink window the way commercial inks do (possibly need to add some flow modifier now that I have the ink "wet" enough).

 

The test sample was six ounces taken from the pint of ink left after boiling down; at first, I added a few drops of Edwal LFN (a photographic surfactant used to prevent water spots on processed film -- causes the water to sheet off instead of beading); once I was up to 12 drops in that six ounces of ink (enough LFN to treat six quarts of distilled water for photographic purposes), I brought out the big guns and added fractional drops (taken on the end of a toothpick), then several whole drops of Dawn dishwashing liquid, ending up with six drops of that on top of the 12 drops of LFN. That's where I stopped, finally concluding that there was a problem with the pen, and that's where the FP sample stands at present: after cleaning the pen properly, it writes, and isn't so dry as all that, but it's not very lubricative (the pen drags on the paper, though the paper I'm testing on does that a little with commercial inks as well) and as noted doesn't coat the ink window the way PR inks do in my Dollar 717i. I have a small bottle of glycerin, but I'm cautious about adding this, as it may be damaging to natural latex found in pen sacs (probably won't hurt the synthetic rubber piston seal in the Osmiroid, but I hope to eventually refine this process enough to use the ink in any fountain pen).

 

Now that I have the pen behaving again, I can try to decide what to add that will improve the coating (and it's okay if it also boosts the viscosity a little; this ink is a bit less viscous than commercial inks, too); it's okay if I have to add a little more detergency to restore flow afterward.

 

The ink still does turn brown over about 24-48 hours (longer if, for instance, it's closed inside a book with reduced air contact); I suspect that's unavoidable with the method I used for this batch, since the reaction won't stop until the solution is saturated with iron, but given I used rather little acid relative to the amount of iron, there probably isn't much in the way of excess sulfate present, and it's that which eats holes in the paper over time.

Does not always write loving messages.

Does not always foot up columns correctly.

Does not always sign big checks.

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