Internal Journal: Future's Pesticide Remediation Tek

Brine is cheap, magsil-pr is not.

3 Likes

The magsil method is preferably a two solvent system of ethyl acetate and an alkane like hexane. Please take a peek at the SOP linked on the EPA website.

4 Likes

The SOP proposes various solvents and methods depending on what you are trying to extract.

Would anyone be kind enough to provide me with a picture or description of how to set up the pesticide removal glassware from Lab Society? I am new to remediation and want to make sure I am on the right path. Just got the LS pesticide kit in the mail and am eager to process my first pass material. Thanks in advance !

2 Likes

Dm me or contact me at 1(833)MAKE-OIL, and Iā€™ll help ya out :v:ā€¦ Im feeling generous today lmao.

2 Likes

I thought the polar wash only yielded trace cannabinoids?

Hows that list going? Ive been building one as well

Quick dumb question-
The 60L of saline solution is made in a 50L reactor but subsequently do the 20L pH 9, 6, and 4 washes occur in the reactor as well? Does one then transfer the mix of saline and distillate/heptane into a sep. funnel for separation?

Kinda dropped off the list of most pressing issues honestly, my method development veered off that trackā€¦thankfully

Hi all,

A quick thanks to Future4200 for his open attitude about information in the industry. We all want to make better, cleaner product.

I want to round up the knowledge in this thread about pesticides that can and cannot be removed using the described liquid/liquid extraction and normal phase column chromatography. The Rf of pesticides in TLC systems tends to follow the octanol/water partition coefficient, Log P or Log Kow. We know this tech works on myclobutanil based on published work, and in this thread permethrin and bifenthrin do not. Log P of bifenthrin is reported on pubchem to be 6.00, permethrin is 6.5 from the same source. Myclobutanil is 2.94. Since this is a logarithmic scale, we are looking at a 3 order of magnitude (1000x) difference in polarity between them which probably means that permethrin and bifenthrin are co-eluting with the target compound (Log p of dronabinol is 6.97 from the same source).

Iā€™m currently waiting for results on a spiromesifen remediation. This pesticide has a Log P of 4.55. Since it will not be protonated or deprotonated by the mild acidic and basic conditions of the liquid-liquid extraction, a successful chromatographic separation is necessary. Iā€™ll update this post with my results as soon as theyā€™re available.

Anyone else worked on pesticides less or more polar than myclobutanil that would like to share their results?

On a second front, Can anyone post the system used for the successful separation of non-polar pesticides using reverse-phase (mobile and stationary phase, how you monitored it if you did).

Lastly, It would be valuable to establish a list of pesticide Rfā€™s for this heptane/silica system along with the Rf of the target compounds (as many cannabinoids of interest as is possible). If no established reverse phase system is developed, a table of Rfā€™s for each pesticide in such systems would be very valuable. Iā€™ll see if I canā€™t convince the higher ups to fund the work for the more common pesticides that we see internally (Iā€™d gladly take input from others on problematic pesticides that they have found and see if I canā€™t publish their Rf as well).

8 Likes

I found 4.75 to be the Log P value for piperonyl butoxide. It doesnā€™t have any ionizable groups within the bounds of the pH range used. Itā€™s a hard maybe as to whether it will work. Worth running on TLC to see if PBO moves much off the baseline. My guess is that it will pollute some of the later fractions, but you can collect smaller fractions. But then you gotta test themā€¦

1 Like

Update

I got the Log P 4.55 pesticide clean using heptane/MgSil system.

6 Likes

Hey there-
Attempting my first shot at pesticide remediation using the LS kit and Futureā€™s SOP.
I have scaled down from 60L saline solution and 500g distillate to 6L saline and 50g distillate because I lack access to a 50L reactor as described in the ACRON article. Instead I will stir in my bf and pour into the sep. funnel.

I am having trouble getting one of my 2L batches of saline solution to pH 9. This could be because I only have pH 4 and pH 7 calibration solution no pH 10. This could also be because I only have 2L to add sodium bicarb to rather than 20 so the solution seems over saturated with powder but will never read above 7.2? I know my pH meter can read 8.5 at least because it confidently reads 8.5 from our shops water cooler alkaline water.

Any advice for getting my 3% saline solution of 2L up to pH 9? Maybe sodium hydroxide or something?
Could I use the alkaline water thats already at 8.5? I have read that in addition to sodium bicarb, salt and distilled water, alkaline water also contains calcium. Is that cool or no?

Thanks in advance

1 Like

you will want to start with distilled water, city water has lots of unwanted junk. Go slow when changing the ph, you can easly over do it. NaOh will work to change the Ph.

1 Like

Canā€™t believe the people who think they have an amazing proprietary way for remediation using columns.
Sure, with chromatographic methods you can clean anything up. Plus it is pretty basic chemistry, really not all that much creativity involved. But it is just not economical. Much better off spending a couple hundred bucks on making sure your starting material is clean.

2 Likes

Has anyone had any experience with removing Propiconazole from 1st pass disty? I am wondering if I can run a saline wash and skip the magsil column chromatography and that will be sufficient. Iā€™ve read that Propiconazole is only water soluble at 100mg/L so I am hesitant to only do the brine wash. Any advice?

What are your starting ppm?

0.684 ug/g

So 0.684mg/kgā€¦

Which means you need how much water to wash a kg?

(Assuming 100mg/L)

Seems to me if you wash each kg 3x with a liter, you should be goodā€¦
[3x 100x and then someā€¦]

2 Likes

Hi ghettoyellow, would you be willing to share how to remove bifenazate? One of my Crude batches just tested positive for 2.7 ppm of Bifenazate and the Action Limit in my State is .1 ppm.

I would welcome anyone elseā€™s advice too. Thanks.