Iron Gall Ink - Precipitation

[AceNinja]

I've always heard of that iron gall ink will tend to precipitate solid particles after storage for a few years, but never really saw a photo of it.  Well today I would like to share some of my photos of it.

 

For context, I've recently bought 2nd hand 50ml of Diamine Registrar's Blue Black from my local pen community here.  Just because I really wanted to try this ink, and it's just so difficult to get this ink at my location (not without paying extremely high shipping fee).  The seller does make it clear to me that he bought this ink (100ml bottle) about 7 years ago, he didn't know if there's precipitation problem, as he just didn't check/use the ink regularly, and just bought and didn't use it.  So I just decided to go ahead to buy from him.  He loaded the ink into 5 unit of 10ml sample bottle and ship it to me.

 

Upon receiving, I pour the inks into an empty 62.5ml pelikan bottle.  After pouring, I can really see solid particles left over in 2 of the sample bottle, especially the most left one.  So I imagine that when he fill the first 3, the ink level in the original bottle is still high enough so the particles didn't get sucked into the syringe/eye dropper during transfer, and as the ink level gets lower, most of the particles got sucked into the last draw, and deposited into the last sample bottle.  So I decided to snap some photo and share with all for knowledge.  I've since already inked up a pen with this ink, so far still behaving nicely, no clogging yet.

 

It's really difficult to check if there's anymore particles in the pelikan bottle, the ink is quite dark colour, and the particle is also dark colour, its difficult to see if they're there (or not).

 

[TSherbs]

Quite striking evidence!

[XYZZY]

About a year ago I tried filling a pen with some D. Registrars that had been sitting for at least a year, the bottle probably first opened 4 years prior.  When I wrote with it the line was very pale gray that didn't darken much.  So I knew the iron had precipitated out.

 

I poured the ink into a folded paper towel, adding water a couple times to get all of the sludge out.  I recall I had what looked to be about 1/4tsp of metal granules on the paper towel.  I went to find tripod and camera to have pictures to post, got distracted with a work emergency, and came back to find somebody had thoughtfully cleaned up my mess.  Sigh.

 

Despite never doubting the recommendation to not shake IG inks, that was clearly proof.  Although I now have a cunning plan...get one of those oversized magnets that comes with health warnings, shake an IG ink, then place the bottle on the magnet so that it can pull the iron granules down before the rest of the ink settles out.  Because everybody needs an excuse to buy a magnet with a health warning (guys, back me up on this!).  
 

I have a can of compressed argon for preserving opened wine, but it come out with enough velocity that I'm not going to stick it into an ink bottle.  It would just launch the ink everywhere.  Perhaps the next time I open an IG I'll try a butane lighter before capping the bottle.

[Schaumburg_Swan]

... out of my bottle of ESSRI under the microscope:

[Lithium466]

Dreamy! 😍

[txomsy]

Please consider that precipitation is induced by oxidation. As oxygen combines with iron, you get a precipitate and less oxygen in the gas part. The process will stop once there is no more oxygen. When you open the bottle, you renew the oxygen and the process.

 

I have had IG inks opened after decades and used them with no issue, with precipitates once used that were no different from what a new bottle would leave.

 

It all depends on how often you open it and for how long you leave the oxygen to react.

 

If you first open the bottle to use it continuously, then likely the oxidation that can take place in between fills will not exhaust the oxygen and be minimal, as will be the precipitate once the bottle is completely used up.

 

If you open the bottle, take a load, wait a year for the next one, and so on, when you finish the bottle twenty years from the first fill, it will likely have a noticeable precipitate.

 

If you open it, and wait one+ year(s), a small part of the iron will have precipitated but most will still be in solution, then if you use it normally (not waiting one year between refills) you will likely not notice anything, only a small difference. Or use it normally, wait twenty years, and then continue using normally: in the long interval, IG will have precipitated until oxygen was exhausted -but no more- and the quantity will depend on how much air was in.

 

[ Added: another factor is where does reaction take place: it will happen where IG and O2 are in contact, so usually only in the ink surface, unless you agitate, move or shake the bottle, which will mix tiny O2 containing air bubbles with the ink and increase the reaction surface. Much like you can waste a good wine bottle by shaking. Note the usually: plastic bottles may allow gas diffusion and then O2 can renew and can attack the ink from more sides. Similarly, badly or non-tightly closed bottles will allow air renewal. That means that some bottles will be more prone to precipitation than others. ]

 

Shortly put, try to understand the process, reason it out and you should be all safe if you apply basic common sense and precautions. If not, then, just try to check somehow the deposit, try to avoid filling from the bottom, try not to mix air and IG ink to reduce the reaction surface (i.e. do not shake) and avoid re-suspending precipitates.

 

Easy. No need to fret about it.

[AceNinja]

15 hours ago, XYZZY said:

About a year ago I tried filling a pen with some D. Registrars that had been sitting for at least a year, the bottle probably first opened 4 years prior.  When I wrote with it the line was very pale gray that didn't darken much.  So I knew the iron had precipitated out.

 

I poured the ink into a folded paper towel, adding water a couple times to get all of the sludge out.  I recall I had what looked to be about 1/4tsp of metal granules on the paper towel.  I went to find tripod and camera to have pictures to post, got distracted with a work emergency, and came back to find somebody had thoughtfully cleaned up my mess.  Sigh.

Interesting, so those particles can be filtered out huh, maybe need to get some coffee filter paper sometime in the future.  Also interesting to see that the more it precipitated out, the lighter the ink colour / darkening it becomes, which makes sense.

 

Previously I've a different encounter.  Last time I bought a pack of Pelikan 4001 Blue black short cartridge, when it arrives, i can see the packaging is already quite old.  When I written with it, the colour is a light-medium grey colour, slowly darken to medium-dark grey, its completely lack of any blue.  I can only imagine that the blue component has somehow already faded away.  I've bought a new bottle of 4001 BB afterwards, which behaves as it should: a very nice shading blue black ink.

 

So far for the Diamine Registrar's ink in my pen, when i wrote it, it lay down a blue black colour very similar to my pelikan 4001 blue black's colour and darkness.  Then within 3-5 seconds, it started to darken quite a lot, darken more than the 4001 BB does.  Then a week later, one might will mistaken it was written with a black ink with blue tint.  So I guess my bottle of Registrar's still has not yet precipitated out heavily.

 

 

[SLinkster]

On 10/24/2023 at 10:36 AM, XYZZY said:

everybody needs an excuse to buy a magnet with a health warning (guys, back me up on this!).  

My husband has a permanent e-stim implant that came with a ginormous "in case of emergency" external high-gauss magnet (extension kill switch, I think). Good to know there's an alternate use for it. 

[Chris1]

I had one of those large plastic bottles of the ESS Registrars' Ink - I think it was 100ml - but we didn't really get on. I found it rather dry to write with and not a great colour either. I left it for ages and then decanted much of it into an empty Montblanc bottle before ditching the rest. It has sat there unloved at the back of the ink cupboard for at least five years before I decided to take another look at it. What I found was a thick layer of black sludge at the bottom of the bottle with a blueish-grey liquid above. I wish now that I'd photographed it, but I simple dumped it and washed out the bottle.

 

I believe ESS now packs its ink in glass and it is pretty inexpensive if bought direct. 

 is

If the ink used quite quickly, the oxidation that produces the precipitate doesn't get much chance to take place; use the ink slowly and, as others have said, reintroducing oxygen into the bottle each time it is opened helps the process along. 

 

I bought Pelikan 4001 blue-black a fortnight ago and it is a nice blue-black that goes black after a while on most paper, but stays pale blue on the newsprint of my 'i' newspaper when I'm doing the puzzles and crossword. I can only wonder at the chemistry taking place that is preventing the iron from oxidising on this medium. 

[inkstainedruth]

I have hesitated to order a bottle of ESSRI, simply because I don't think I'd go through a 100 ml bottle of IG ink before it went bad.  And after have a 60 ml bottle of Akkerman IJzer-Galnoten go bad on me (and that IS a glass bottle, and was kept in the box to keep it out of the light, and keep the box in another box as well)?  I'm going to be really cautious about the other IG inks I have (a number of KWZ inks, and a couple of the Platinum Classic colors, plus the recent purchase of a bottle of 4001 Blue Black (which I like very much).  And of course I have three IG ink colors made a number of years ago by FPN member Pharmacist (and since they came in plastic bottles I have NO idea what shape those are in at this point... ).

Ruth Morrisson aka inkstainedruth

[txomsy]

One good thing about ESSRI is the shape of the bottle, which leaves minimal amount of surface at the ink/air interface, and the bottle color seems UV resistant (though it is plastic, and might allow slow evaporation).

 

Added: note that evaporation may also increase concentration and lead to precipitation, but that's not the ink's fault.

 

I had an old bottle of Montblanc Blue-Black (the IG formulation) that I opened 30 years ago, used until 1/2, and retook some 10 years ago. No problem with it whatsoever (the ink/air surface in an MB shoe bottle is maximal, but the cap was tightly closed all that time). So, if one is minimally careful with the bottle (keep it upside, in a cool, dark place and well closed --or even better decants it on a crystal bottle) then I wouldn't expect much trouble.

 

I have a bottle of ESSRI (the plastic one) of which I decanted half on the MB shoe bottle of blue-black mentioned above once I had used and cleaned it. So far I haven't noticed problems (in about some 5-6 years), but didn't pay much attention. I'll have a look again when I go back home, just in case (maybe it's gone awry without me noticing, so don't pay me much attention, I could have gone totally astray on this).

[AceNinja]

24 minutes ago, txomsy said:

(maybe it's gone awry without me noticing, so don't pay me much attention, I could have gone totally astray on this).

that could be the case.  It's really hard to notice it while it is in a full bottle or half bottle, the ink is dark colour, and precipitation is also dark colour.  It's difficult to tell if those are bubbles, some normal ink staining on bottle (the kind that can be dissolved if you shake the bottle) , or actual precipitation.  In my case, it's only easy for me to notice it because I was pouring the ink out from the long and slender ink sample tube, which provides much more surface area for the precipitation to cling onto, and at the same time with the dark ink removed from the tube, which makes it easier to spot the dark precipitation against the now lighter background.

 

Still, I don't think we should give up on IG ink just because of the possibility precipitation.  With good care/storage as the posts above, it seems still can last quite long.

I'm already on my 2nd fill of this Diamine Registrar's Blue Black, its great!

[Arkanabar]

IG ink has its caveats, proper to its use.  For those people who don't mind, there's no reason to avoid it.  And they've all been pretty much covered in this thread -- that it works by having a solid, water-insoluble dark gray precipitate form from a transparent solution when exposed to oxygen.  The only way I'd have it is in one of my jotting pens (typically a Jinhao 51A XF) for the often worn paper in narcotics administration logs, and in a small glass bottle (30mL or so).  For me to make good and proper use of it, it would have to be my primary ink for just about everything.  And first I'd have to be convinced that Pelikan 4001 Brilliant Black (which I already own) wasn't good enough for those worn and sometimes tattered pages.

[Puddinhead]

I prefer to use Diamine Registrar's Ink because of the dry application as opposed to the more brilliant and 'lively' colors available in inks now days. 

 

The discussion in this thread is informative; I appreciate the insights offered by all contributors and while I receive the words of caution about IG inks, to date there have been no problems in any of my pens using the Registrar's ink, neither the less expensive Lamys, a Parker Centennial (modern), and an 'early' modern CS Churchilll. Thanks for the education on IG inks.

[inkstainedruth]

I wasn't all that enamored with the sample of Diamine Registrar's I tried a few years ago.  It had nice shading but that was all you could say in its favor.  Wondered if it was starting to go bad because the color was a washed out blue-grey. 

When I tried Akkerman Ijzer-Galnoten, it was SUPER dark (much nicer than the Diamine Registrar's. [There have been discussions about whether the Akkerman inks are made for them by Diamine or not....]  But unfortunately I didn't use it fast enough and about halfway through the bottle it started to go bad, with the iron precipitating out.... 

Not sure of the other IG inks I have at this point: a number KWZI IG colors, a few of the Platinum Classic colors (I just got samples of Sepia Black and Khaki Black recently to try them -- I really like Lavender Black and Forest Black), and a bottle of Pelikan 4001 Blue Black; plus a few of the old IG inks made a number of years ago by FPN member Pharmacist (those made by him are so old I have NO idea what shape those are in ).

I've been curious about ESSRI, but the size of those bottles are such (100 ml, so even more than the bottle of Ijzer-Galnoten) that there is no way I'd be able to go through one before it went bad -- even if that was the ONLY ink I used for months....

Ruth Morrisson aka inkstainedruth

[XYZZY]

20 hours ago, inkstainedruth said:

I wasn't all that enamored with the sample of Diamine Registrar's I tried a few years ago.  It had nice shading but that was all you could say in its favor.  Wondered if it was starting to go bad because the color was a washed out blue-grey. 

When I tried Akkerman Ijzer-Galnoten, it was SUPER dark (much nicer than the Diamine Registrar's. [There have been discussions about whether the Akkerman inks are made for them by Diamine or not....]  But unfortunately I didn't use it fast enough and about halfway through the bottle it started to go bad, with the iron precipitating out.... 

Not sure of the other IG inks I have at this point: a number KWZI IG colors, a few of the Platinum Classic colors (I just got samples of Sepia Black and Khaki Black recently to try them -- I really like Lavender Black and Forest Black), and a bottle of Pelikan 4001 Blue Black; plus a few of the old IG inks made a number of years ago by FPN member Pharmacist (those made by him are so old I have NO idea what shape those are in ).

I've been curious about ESSRI, but the size of those bottles are such (100 ml, so even more than the bottle of Ijzer-Galnoten) that there is no way I'd be able to go through one before it went bad -- even if that was the ONLY ink I used for months....

Ruth Morrisson aka inkstainedruth

Ruth I’m getting more and more convinced that you got a bad sample of the Diamine Registrars. Your description sounds like what I’ve seen from an old bottle, not a new bottle. Instead of going for 100ml of ESSRI you might consider a new 30ml bottle of registrars. 
 

From what I’ve learned of IG ink reading FPN I am skeptical of IG samples, especially for a strong IG.  IGs start going bad once exposed to oxygen, and you have now idea how long your sample was sitting on a shelf before it was sent to you. And since samples are frequently 2 or even 1.5ml of liquid in a 5ml vial you’re getting a fair amount of air to help that ink go stale. If the sample had been decanted from a new bottle and the vial filled to the top (dangerously full, like Noodlers) that might be different.

 

Can an IG sample be good? Sure. But it seems to me that there is much more opportunity for it to not be representative of the real thing. 

[inkstainedruth]

Yeah, I'm starting to suspect the same thing.  I don't remember where I got the sample from, but I think it was 2 or 3 ml....  

I have enough other IG inks to last me a while (and really liking 4001 Blue Black now).  But I might think about trying a 30 ml bottle of Diamine Registrars sometime in the future.

Ruth Morrisson aka inkstainedruth