Wondering if anyone has figured out how to correct ph inline while remediating dist through magsil in heptane.
Is there a powder i can put below the magsil in a column to avoid water washing/avoid oxidation?
How would i calculate how much of said powder to use? If no one has done the calculations I’ll just do a water wash after chromatography and test the ph of the water and adjust the amount of said powder until it comes out perfect.
@Photon_noir knows, I’ll betcha!
It doesn’t sound unreasonable to be able to do that. I mean you change the ph one way running through powder why wouldn’t you be able to correct it the same way. I am interested in this as well. I am currently sitting on 2 liters of distillate that popped for Pyrethrin and Piperonyl Butoxide. I figured out how to remediate them but don’t have a chromatography column to readjust the ph.
Heard that you can use AA 1:1 ratio to magsil, I’m gonna try out various ratios to see how little AA i can use and it still work good
Also if you don’t have a chromo column I’ve used a fritted disk buchner filter under vac and it works great, just make a slurry with clean solvent first and vac it so it packs good then run your dist/heptane mix through it but don’t let it go dry and try to keep the top as undisturbed as possible, use a stainless spoon or tool to smooth it out as you go and use a cold trap to protect your pump from the heptane vapors or dont go so deep on vac that you evap heptane
Where’s the all knowing one at @Photon_noir have you tried this??
Inline ph reading without water present is not possible
I would dare say that the ph should not be affected so much as to be an isseu for distilling since magsil can be used in small amounts directly inside the boiling flask for color remediation
Look at the problem again…
Maybe @thesk8nmidget will post the column he just finished a PBO remediation through.
Here’s a pic and video.
A chromatography column is as simple as that. A column. Control the flow with a valve at the end, and you can control residence times. Obviously this works for solvents that won’t evap at room temp but I also use these same columns with a metering pump to do “closed” chromatography runs
This was as basic as I could get for a little r&d scale remediation, but I have used these same glass columns (in various sizes) to scale up to my 100l stainless columns. The Sep funnel to column is a great way to “automate” your feed rate to match your elution rate.
Yea that’s why i said I’d do a water wash and test the ph of the mix i run through it with different amounts of AA. Ive read a lot of people do water washes to correct ph after magsil and i get some pretty bad oxidation sometimes especially if i use too much magsil
You ever tried nitrogen pushing the dist/heptane mix through a closed loop instead of using columns or doing it under vac? I’m about to try the closed loop method next week and have been doing it under vac for a while. It’s so painfully slow doing it with no vac or push
yes, pushing is going to be much easier vs pulling with vacuum.
Tip on cheapest way to get push? Like will a compressor work?
Sep funnel on top is a great idea.
Yes but make sure u empty that compressor of water frequently and get an inline drying filter, to minimize the amount of water u push in.
Here is the blurb I wrote in response to customer question regarding Magsil and Spinosin, @TheFire210 …The last lines in parentheses contains the kind of answer you seek, I believe.
General recommendations for MagSil PR:
Solvent should be non-polar (e.g., an alkane, such as n-heptane), NOT alcohol.
Use 10X MagSil PR weight to contaminated cannabinoid product weight… I.e., 10g MagSil to 1g distillate.
Use MagSil PR in a column, typically as (normal phase) chromatography stationary phase, rather than as a simple filtration medium. It is best to use MagSil PR as the 2nd to last step in your pesticide remediation protocol… The last step is pH equilibration of the product by washing with pure distilled water (with NaCl, then without), until the pH of the pure water after washing is the same as it was before washing. This pH is normally 6.2 to 6.8 at typical room temperatures.
I can say with a high degree of certainty that MagSil should be an effective stationary phase in the retention of spinosoids due to its polarity, structure and effective pH (when in contact with water or molecules of opposing effective pH character, like spinosoids). Also, this effect would be best employed in combination with mobile phase (solvent) of normal (straight chain) alkanes, like n-butane (C4) to n-heptane (C7)… so it is suitable for BHO systems with in-line CRC (color remediation chromatography) columns, probably those with increasingly polar & effectively acidic media layers in the direction of flow (for example, Alumicel B or MagSil on top, then the other of the two, then Silica gel, then Alumicel N, then Alumicel A, then acid-activated clay and/or charcoal like T-41).
Three things required to make fire.
You’ve got one.
I don’t recommend deliberately adding a second.
In case you accidentally generate the third.
I suggest nitrogen. Which CAN be reused if you’re clever…
Edit: cheapest method is gravity.
Watch some actual chromatography videos to see how it’s done…Eg this one from MIT https://m.youtube.com/watch?v=B_QyhG2-VBI
And for the others not aware: MIT Open Source Classes
The MIT classes are so cool.
I used hot butane vapors to clear my heptane column lol
indeed.
staying above the UEL is another way of avoiding those pesky 'splosions…
