Red Ring of Death

What exactly does that mean?

@midsfactory I think @JohnLong is referring to filling the jar with nitrogen from a can or cylinder before capping. I’ve been using a foodsaver jar sealer attachment and have (so far) seen a significant decrease in oxidization (the red ring). I’m going to compare them side by side soon. If I can accomplish the same thing without a consumable I will stick with that method.

3 Likes

Thank you for showing me the foodsaver part. I can’t believe I don’t already have that… What sort of lid would you use to inject nitro into a ball jar?

2 Likes

@mldsfactory I’m not sure on the process for backfilling jars with nitrogen… you’d have to ask @JohnLong. I’m curious as well.

1 Like

You can drill holes in lids and use bulkhead fittings perhaps. I’m sure there are some special devices that allow vacuum and backfill with standard lids (I can’t imagine if the food industry didn’t do so - just gotta find the tabletop version)

I’ve also noticed that if you heat the distillate without stirring, the oxidized layer drops right to the bottom. It’s not gone, but you can pull non-discolored distillate off the top like that (it’s usually not so bad that I ever feel the need to though). Centrifuging kind of works without dispersing the oxidized layer, but internally stirring definitely won’t work. The oxidized layer is probably heavier in molecular weight than the rest of the distillate.

1 Like

back fill jars with inert gas, cap them loosely with the rings on and place these jars into your vaccum oven. Pull a vaccum on the oven then fill with inert gas, do this three times. Then pull a hard vaccum on the oven, release air into the oven rapidly and the lids will seal from the pressure differential. Nitro sealed mayson jars!

13 Likes

Makes me sound silly, huh?

Didn’t mean to come off like that! One thing I’ve learned is there is a hellava lot of ways to skin a cat!:smirk_cat:

3 Likes

Duh! haha brilliant. Why 3 times though?

3 Likes

Because the first fill removes 99%. The second removes the 99% of the 1% remaining. The third removes 99% of the last .01% . Kinda like drying a flask on a shlenk line for air free chemistry.

4 Likes

Nitrogen should work as well, I would think. It’s inert and comes in 5 9 purity. 99.999% used in gas chromatography.

Idk, I like the argon because of its weight. It sinks down and pushes residual o2 out .

5 Likes

I have seen of course many posts and procedures that adjust the acid levels (PH) in the boiling flask. I understand that with a certain category of degredation reactions that are facilitated by oxygen that a higher PH can in theory lead to an enhanced inclination to oxidize.

However, I have to ask myself how on Earth can you measure this? I mean, a pH reading as far as I know is an indication of free hydrogen ions present at the moment the test is made. Then the question is, what reference are you using as a comparison and how exactly can this be tested so as to make the comparison relevent?

For instance when I take a pH measurement if I do not take the measurement at the same temp as the reference then the number is meaningless. Tap water generally is fairly nuetral in pH, yet heat it up and you will see a higher number of free hydrogen ions present and any pH meter not set to compensate for temperature via a special circuit (a crude but effective work around) will show the water to be a higher acidity. Let the water cool to room temp and the pH level returns to normal. So in the case of adding an acid to the boil, by what means do you test the compound first to see if it is already at the desired pH or not?

As far as oxidation occuring then on already distilled compound presumably because of an excess of free hydrogen ions facilitating oxidation of an already sensitive compound I must admit that I have seen numerous well intentioned and maybe even 100% accurate suggestions that this is occuring because of improper pH conditions either in the boil or post. The question I have for the community again is that how exactly can this be measured? If the presence of free H ions is a measure of acidity and of course there are millions of pH testers spanning a range of human activities, then why is the compound itself not tested for pH assuming that pH can indeed influence oxidation of the compound outside of the boil at ambient? The answer must lie in either the impractical nature of testing the compound itself for pH OR more likely there is simply no reference established as a basis to measure from. Currently it seems the reference being hinted at refers to water as the standard and therefor room temp as the reference against to measure.

What I am getting at here is there seems to be a good following who are adjusting pH levels but not first knowing where they are to begin with. Then when the pH adjustment does not impact oxidation I have seen again ideas to mitigate by further adding external compounds, but again without testing and knowing for sure what the levels are already and what the adjustment changes it into. Even worse from a technical point of view I have seen no paper, video, or reference that could be used in any realistic way to verify whether your additions 1) made a better difference, 2) made no difference, 3) made things worse. It is guesses and anecdotal observations and nothing wrong there but the underlying question with regards to all the pH adjustments being intentionally introduced; how do you know or not know how acidic your boil already is before you adjust it?

5 Likes

The only reason we started pHing anything was to assure our saline was acidic for disassociation and alkaline for “saponification”, or something similar to it.

These are important steps to minimize the use of MagSil-pr for pesticide remediation. But they seem to remove some of the phosphatides that can actually protect the distillate from degradation…

Adding the waxes back seems like the most natural and effective method @Beaker

And @Soxhlet is spot on with the vacuum oven nitro jar filling

5 Likes

what is your ratio of wax to distillate? i need to figure something out myself! all of my distillate carts are oxidizing within a couple of days

when youre adding argon are you adding it to the cartridge itself or to the initial container it is stored in?

When we were messing with it we would add 5% by weight. make sure you waxes are dry and don’t contain trace solvents.

1 Like

To the media bottle when filling the bottle from the receiving flask, and every time you open/ pour from the bottle.

1 Like

deliberately huffing waxes?
I feel the need to invoke @dontbanmeagainbro :wink:

Instead I’ll invoke @Beaker: Red Ring of Death - #16 by Beaker

lots of clues behind: Search results for '@beaker red' - Future4200

3 Likes

Ive ran unwinterized bho in my wiped film and the result was a very stable oil that would not oxidize. The color was yellow but the clarity was very poor.

Think of an orange peel and it’s use as a waxy protective layer for the fruit. You don’t want to consume the wax but it can be a useful tool in preventing high temp oxidation. One could distill, then winterize and roto perhaps…

4 Likes