Biocide Shootout Tests

[LizEF]

Thank you, @SamCapote!  Don't know that I'll ever use this info, but it's good to have.

[amberleadavis]

@SamCapote when I first started on FPN you were one of the people who welcomed me.  I read this thread and I added the Natural Pigments biocide to SOME but not all of my inks.  The ones that I inoculated are still good, but others from the same company have degraded.  I'll have some pictures to show you soon. 

 

Thank you for being part of my inky journey. 

[SamCapote]

On 10/4/2023 at 1:02 AM, amberleadavis said:

@SamCapote when I first started on FPN you were one of the people who welcomed me.  I read this thread and I added the Natural Pigments biocide to SOME but not all of my inks.  The ones that I inoculated are still good, but others from the same company have degraded.  I'll have some pictures to show you soon. 

 

Thank you for being part of my inky journey. 

You have always been so wonderful and making this forum as great as it is.  Thank you for being in my life!  🥰

[grayautumnday]

On 10/19/2010 at 1:24 PM, pharmacist said:

There are two very effective fungicidical/fungistatical products and excellent for ink making: salicylic acid and phenol. The concentration must be high enough: for salicylic acid this is 1 gram/500 ml and for phenol 1 gram/1000 ml. So you must calculate the total amount in your solution. Both preservatives are enhanced by lowering the pH-value (acidifying the ink by adding hydrochloric acid).

Keep in mind that lowering pH to acidify below neutral will mean a hastened decay for the documents on which the ink is used.

[grayautumnday]

On 10/19/2010 at 5:19 PM, atypical said:

This looks like a very interesting experiment.

 

I checked some old (1939) DIY ink recipes and found the following phenol concentrations:

- Document ink (iron-gall) - phenol: 1 gram , water: 1 litre

- Red ink (eosin dye) - phenol: 15 grams, water: 3500 grams

- Blue ink (naphthol blue-black dye) - phenol: 7 grams, water: 3500 grams

- Bright blue ink (methylene blue dye) - phenol: 15 grams, water: 2.5 litres

- Black ink (nigrosin dye): phenol: 15 grams, water: 2.5 litres

 

From the 1994 MSDS for Koh-I-Noor India Ink: 0.45 % phenol.

 

A modern recipe for iron-gall ink from Kremer Pigmente specifies 1 gram of ascorbic acid in 1 litre of water to prevent moulding.

 

I hope this information is of some use to you.

As someone who has been doing amateur textile/skin/hair/home surface cleaning/care/stain removal formulation for almost 30 years (one of my first adult jobs was carpet/upholstery stain remediation) - can you pretty please share the name of the 1939 source you referenced, and any suggestions on how one might be able to locate that publication?
 

Thank you for your contributions!

I know I'm gravedigging old posts, but this forum has been one of the most amazing resources for me.

 

I'm already disabled and have mostly lost the use of my left hand for the foreseeable future. I used to use processing raw textile fiber, spinning yarn, knitting, weaving etc to manage pain, those things are now all effectively inaccessible, so I've revived my interest in papermaking, bookbinding, fountain pen calligraphy and letter writing... and I'm itching to make progress on DIY fountain pen ink formulation using my vast collection of cellulose fiber dyes... but one thing I've learned the hard way is to take things slow, research what's already been done by those with more experience, and not try to go the hard way (reinvent the wheel) - as an informatician by education, I find it frustrating how comparatively little has been preserved on 19th and early 20th century ink formulation publications (relative to textile dye resources).

[grayautumnday]

On 11/7/2010 at 10:07 PM, SamCapote said:

Well, as is often the case in life, I have good news & bad news. After only 3 weeks, my dear, lost, fungal friends have returned.

 

Surprisingly, every bottle now has clearly visible solid string-like growth....EXCEPT vials #9 & 10 which is the 1 & 2 drops of the "Proprietary Ink Maker's" biocide, which is still clear.

 

I have one other option in the works of getting a stronger concentration of the Sporicidin, but the doses I used were not BIO-CIDAL or BIO-STATIC at preventing the spores from hatching. You have to admire nature's tenacity.

 

But I'm not done yet. This just makes things more interesting.

 

This also validates what pharmacist said earlier about the amount of Phenol required.

There are a few approaches that might help:

1a. Remove the ink from their bottles. Remove all liners and liner adhesive from caps, then replace liners with new PTFE liners of the same diameter and thickness (check Amazon/online industrial/lab supply categories for PTFE liners by EISCO, JG Finneran, SEOH, Nalgene, or other lab supply brands.)

1b. Consider getting "reagent storage bottles" made of borosilicate with PTFE liners or HDPE bottles with silicone o-ring gaskets) to hold ink permanently or until original bottles sterilized.

1c. Sterilize all bottles before and after ink transfer. Wash inside and outside thoroughly at least twice, air drying completely between washes. Use effective biocidal soaps such as betadine surgical/veterinary soap for the first wash and Hibiclens surgical/wound soap (chlorhexidine is far more effective against fungi than alcohol or chlorine bleach). Anyone you know who has dealt with ringworm breakouts in an animal shelter or daycare will probably be able to help advise. Make sure to sterilize all washing and rinsing and drying areas thoroughly before and after placing containers in those areas.

2. Heat and hold the ink at a temperature high enough for a long enough time to kill almost all bacteria and spores in the ink. This may affect the ink color.

 

3. Once sterilized, adjust the pH of the ink upward a modes using a combination of sodium carbonate (if you have a basic grasp of lab safety, able to research SDSs and do a bit of learning about risk factors, and know where to get formulation ingredients such as MakingCosmetics or LotionCrafter, consider also/instead TEA - you can adjust the pH higher without making it more reactive and therefore more likely to degrade metals/plastics).
E.g. One of the most effective ways to keep fungal colonies from regrowing on home surfaces is to apply a strong solution of sodium carbonate (soda ash - the main ingredient in washing soda) mixed with a bit of TSP to the surface after cleaning. 

4. After twice washing bottles with broad spectrum fungicidal-heavy soaps, scrubbing out all nooks/crannies/threads and fully air-drying 12-24 hours after each wash, if possible heat all non-melting storage bottle components in an oven on low (can't remember what the best temp is, but generally I aim for 200F) for 2-4 hours, or place in boiling water and hold at least a gentle boil for an hour, then turn off the oven or stove and allow the pot/oven to cool slowly. Fast temp changes are very likely to cause cracks/shatters in glass/borosilicate/plastics.

 

5. Add a double concentration of heavy duty broad spectrum preservatives known to be especially effective for fungi. Ideally, use full-dose percentages of 2-3 preservatives known to play nice with each other. Make sure the pH range of the ink is in the pH effectiveness range of every preservative. Examples: Liquid Germall, Optiphen Plus, Euxyl PE 9010. Silverion 2400 is inappropriate as it works best at an acidic pH and contains acids.

 

6. Store inks in an area with active dehumidification such as frequently checked/dumped/refilled calcium carbonate moisture absorber tubs or a frequently-emptied electronic dehumdifier.

 

7. Thoroughly wash and dry hands and tools and work areas before handling any ink bottle, wash and dry again before handling another. Wash and thoroughly air dry all pen components - don't store pens moist. Don't dip nibs into bottles - transfer ink out of bottles into a well and never empty ink from a well back into a bottle. Use sterile single-use pipettes or syringes to transfer ink, or buy glass pipette tubes and a bulb that can be sterilized adequately in an oven, steamer, or boiling and fully air dried after every use.

[SamCapote]

On 9/9/2024 at 6:28 PM, grayautumnday said:

There are a few approaches that might help:

1a. Remove the ink from their bottles. Remove all liners and liner adhesive from caps, then replace liners with new PTFE liners of the same diameter and thickness (check Amazon/online industrial/lab supply categories for PTFE liners by EISCO, JG Finneran, SEOH, Nalgene, or other lab supply brands.)

1b. Consider getting "reagent storage bottles" made of borosilicate with PTFE liners or HDPE bottles with silicone o-ring gaskets) to hold ink permanently or until original bottles sterilized.

1c. Sterilize all bottles before and after ink transfer. Wash inside and outside thoroughly at least twice, air drying completely between washes. Use effective biocidal soaps such as betadine surgical/veterinary soap for the first wash and Hibiclens surgical/wound soap (chlorhexidine is far more effective against fungi than alcohol or chlorine bleach). Anyone you know who has dealt with ringworm breakouts in an animal shelter or daycare will probably be able to help advise. Make sure to sterilize all washing and rinsing and drying areas thoroughly before and after placing containers in those areas.

2. Heat and hold the ink at a temperature high enough for a long enough time to kill almost all bacteria and spores in the ink. This may affect the ink color.

 

3. Once sterilized, adjust the pH of the ink upward a modes using a combination of sodium carbonate (if you have a basic grasp of lab safety, able to research SDSs and do a bit of learning about risk factors, and know where to get formulation ingredients such as MakingCosmetics or LotionCrafter, consider also/instead TEA - you can adjust the pH higher without making it more reactive and therefore more likely to degrade metals/plastics).
E.g. One of the most effective ways to keep fungal colonies from regrowing on home surfaces is to apply a strong solution of sodium carbonate (soda ash - the main ingredient in washing soda) mixed with a bit of TSP to the surface after cleaning. 

4. After twice washing bottles with broad spectrum fungicidal-heavy soaps, scrubbing out all nooks/crannies/threads and fully air-drying 12-24 hours after each wash, if possible heat all non-melting storage bottle components in an oven on low (can't remember what the best temp is, but generally I aim for 200F) for 2-4 hours, or place in boiling water and hold at least a gentle boil for an hour, then turn off the oven or stove and allow the pot/oven to cool slowly. Fast temp changes are very likely to cause cracks/shatters in glass/borosilicate/plastics.

 

5. Add a double concentration of heavy duty broad spectrum preservatives known to be especially effective for fungi. Ideally, use full-dose percentages of 2-3 preservatives known to play nice with each other. Make sure the pH range of the ink is in the pH effectiveness range of every preservative. Examples: Liquid Germall, Optiphen Plus, Euxyl PE 9010. Silverion 2400 is inappropriate as it works best at an acidic pH and contains acids.

 

6. Store inks in an area with active dehumidification such as frequently checked/dumped/refilled calcium carbonate moisture absorber tubs or a frequently-emptied electronic dehumdifier.

 

7. Thoroughly wash and dry hands and tools and work areas before handling any ink bottle, wash and dry again before handling another. Wash and thoroughly air dry all pen components - don't store pens moist. Don't dip nibs into bottles - transfer ink out of bottles into a well and never empty ink from a well back into a bottle. Use sterile single-use pipettes or syringes to transfer ink, or buy glass pipette tubes and a bulb that can be sterilized adequately in an oven, steamer, or boiling and fully air dried after every use.

 

 

Some good ideas, but I would not want to heat my ink high enough to kill mold spores, nor add sodium carbonate, nor religiously scrub and heat bottles in the oven, nor most of the things you mentioned because it would just be too much hassle.  Using an adequate biocide alone is the most tenable solution for me.  

 

[grayautumnday]

On 9/16/2024 at 1:06 PM, SamCapote said:

 

 

Some good ideas, but I would not want to heat my ink high enough to kill mold spores, nor add sodium carbonate, nor religiously scrub and heat bottles in the oven, nor most of the things you mentioned because it would just be too much hassle.  Using an adequate biocide alone is the most tenable solution for me.  

 

Makes total sense.

 

In that case, maybe consider checking out a preservative called Euxyl PE 9010? It's a phenol-heavy preservative that's been specifically tested for treating formulations that have been exposed to microbial contamination.
 

Preservatives get "used up" - the more contamination there is, the quicker the preservatives get exhausted. Hence there being a "shelf life" on any product that contains (or attracts) water. So if you know there's already heavy contamination, no preservative will adequately treat a solution at the percentage rates recommended for initially-microbe-free solutions.