Does anyone here TLC test?

[Moe.Red]

I called them to see if they might still sell 5 grams, and was told that they don't ship to residential addresses.

But I finally found a company that would, they state it on their website. I also discovered something very interesting - and money saving. There are two different types of Fast Blue BB with different CAS numbers. You said you were using CAS 120-00-3 - there is also one ' CAS 5486-84-0 - Fast Blue BB Salt hemi(zinc chloride) salt' which does not need to be frozen or even refrigerated. I had my doubts, but the data sheet said it is used in TLC testing of cannabinoids. I got five grams for $50 something shipped. The company I got it from is called 'Chemsavers' (just add a dot com) I'm not sure if I'm allowed to post the link here.

So anyway I got everything together for the price of one of those kits that will allow me to do more tests, than I'll ever need. I did my first one last night with my homegrown Jack the Ripper , and a commercial Durban Poison. It didn't come out so great - very weak and fuzzy. I'm not sure, but I am unsure of the timing in the eluent and the dye bath. Try try again!

View attachment 1115044

That's awesome dude. Sorry this is a PITA, try buying Chloroform in bulk...

So you didn't ask me, but I hate to see people struggle so let me give you a couple bits of feedback.

#1 - you have a usable result! may not be exactly what you had hoped, but there is data there. Here's what I am seeing:

The samples do not look like they are decarbed. Since you are working with aluminum plates, your only option is to do that decarb prior to preparing your samples. Why decarb? Because the large oval at the bottom is where all the acids are stuck. So THCa is showing up in the bottom, whereas THC (delta 9) is showing in the larger orange dot. If you were to decarb first, your THC dot would get larger and you will have a more accurate representation of the actual THC percent. The oval at the bottom will go away.

Also, since all the acids are lumped together, you do not really know what is CBDa, THCa, THCVa, CBGa, etc. Decarbing separates those out and moves them up the plate so you can see what you really have.

What I find exciting for you is that you can clearly see multiple minor cannabinoids there already on the right. Those will only get better as you do!

#2 - It looks like on the left there may have been 2 dots laid down rather than one. It takes a steady hand for sure. But that explains the weird shapes in the end result.

#3 - you have a result all the way at the top. Hard to see exactly what because it is off the plate. Making the plate a little longer or letting the eluent run a little less time will move those dots where you can read them. I find 13-15 minutes on a 20cm plate is about perfect.

#4 - I don't think you want to scrape a line across the silica like that or even write deeply directly under your lane. Basically you want the eluent to wick up as evenly and precisely as possible. When it has to jump over gaps and things like that, you are going to get some potentially unpredictable results.

But seriously, that is a really cool result. I see THCv, CBG, CBC, and obviously THC. Your Jack the Ripper may actually be a better mix if you try again, that Durban tho - thats what we like to see! I'm jealous. Congrats on getting started on this.

 

[Ali_Tarpate]

That's awesome dude. Sorry this is a PITA, try buying Chloroform in bulk...

So you didn't ask me, but I hate to see people struggle so let me give you a couple bits of feedback.

#1 - you have a usable result! may not be exactly what you had hoped, but there is data there. Here's what I am seeing:

The samples do not look like they are decarbed. Since you are working with aluminum plates, your only option is to do that decarb prior to preparing your samples. Why decarb? Because the large oval at the bottom is where all the acids are stuck. So THCa is showing up in the bottom, whereas THC (delta 9) is showing in the larger orange dot. If you were to decarb first, your THC dot would get larger and you will have a more accurate representation of the actual THC percent. The oval at the bottom will go away.

Also, since all the acids are lumped together, you do not really know what is CBDa, THCa, THCVa, CBGa, etc. Decarbing separates those out and moves them up the plate so you can see what you really have.

What I find exciting for you is that you can clearly see multiple minor cannabinoids there already on the right. Those will only get better as you do!

#2 - It looks like on the left there may have been 2 dots laid down rather than one. It takes a steady hand for sure. But that explains the weird shapes in the end result.

#3 - you have a result all the way at the top. Hard to see exactly what because it is off the plate. Making the plate a little longer or letting the eluent run a little less time will move those dots where you can read them. I find 13-15 minutes on a 20cm plate is about perfect.

#4 - I don't think you want to scrape a line across the silica like that or even write deeply directly under your lane. Basically you want the eluent to wick up as evenly and precisely as possible. When it has to jump over gaps and things like that, you are going to get some potentially unpredictable results.

But seriously, that is a really cool result. I see THCv, CBG, CBC, and obviously THC. Your Jack the Ripper may actually be a better mix if you try again, that Durban tho - thats what we like to see! I'm jealous. Congrats on getting started on this.

Oh man, thank you so much for the help. Every point you mentioned is right on the money and makes perfect sense. I did not decarb - I thought if it was cured, it wasn't necessary. I think I'll do it in my kiln, which has precise control (because I built the controller.) Yup, two dots on the left. The streaks went up too high because I left it in the eluent too long. The scraped line is where I used a pencil, but the substrate is too soft for that. I'll try all of your suggestions, and hopefully have some better results to show. It's so hard to find relevant info on this - everyone says to buy a kit.

A couple of questions, if I may:

How much solution do you use for your original spots? I tried one ul, and it seems awfully small.

How long and at what temp for decarb? I've seen all different figures.

How long in the dye bath? Is it critical

BTW - I just received some very expensive (mostly shipping) Novarine THCV:THC seeds. I might have to wait until fall to plant them, though. It gets mighty hot here in southern AZ in the summer, and I don't know if I can keep things cool enough in my tiny grow chamber. Like you and others, I'm looking for high THCV strains.

 

[Moe.Red]

A couple of questions, if I may:

How much solution do you use for your original spots? I tried one ul, and it seems awfully small.

How long and at what temp for decarb? I've seen all different figures.

How long in the dye bath? Is it critical

BTW - I just received some very expensive (mostly shipping) Novarine THCV:THC seeds. I might have to wait until fall to plant them, though. It gets mighty hot here in southern AZ in the summer, and I don't know if I can keep things cool enough in my tiny grow chamber. Like you and others, I'm looking for high THCV strains.

I use 1mL eluent in the sample to mix with .1g of plant, and 2 uL in the spot on the plate.

Decarb is (assuming dried) 90 minutes at 128-130*C. But the cool thing now is that you have the tools to dial in your process completely. If you do a TLC and there are still acids on the plate, you need to go longer. Too long or too hot and you will actually see the cannabinoids start to decrease.

I don't use a dye bath, I spray it on with a little bottle used mostly for cosmetics. Something like this



On the Novarine, that's pretty cool. I just ordered diet durban for 420, and I have original Durban Poison in full flower now, and THC Victory in Veg. Should be an interesting summer!
https://www.amazon.com/gp/product/B077FHP4KH/ref=ppx_yo_dt_b_search_asin_title?ie=UTF8&psc=1

 

[Ali_Tarpate]

I use 1mL eluent in the sample to mix with .1g of plant, and 2 uL in the spot on the plate.

Decarb is (assuming dried) 90 minutes at 128-130*C. But the cool thing now is that you have the tools to dial in your process completely. If you do a TLC and there are still acids on the plate, you need to go longer. Too long or too hot and you will actually see the cannabinoids start to decrease.

I don't use a dye bath, I spray it on with a little bottle used mostly for cosmetics. Something like this



On the Novarine, that's pretty cool. I just ordered diet durban for 420, and I have original Durban Poison in full flower now, and THC Victory in Veg. Should be an interesting summer!

Try Again. Mr Moe, I followed all your suggestions - decarbed at exactly 128°C for 90 min. I only have one ul capillary tubes, so I hit them all twice - might cause the blurryness? And I wonder why they are all run together instead of more discreet dots, like my first crude attempt? When I look at the plates in sunlight, the colors are a little more vibrant - I swear the smear under the THC blob has a slight purplish tinge. The orange color is easily seen. The first set are Chernobyl and Durban Poison store-bought.The JTR is my homegrown. I used the sample size of .1gram, as Moe mentioned, left in the hexane fora couple of hours. I let the eluent creep up to just before the very top of the plate

This one is just the JTR left in the hexane overnight, and left it in the chloroform for maybe 30 sec. after it reached the top of the plate.

The left one (top bud sample) is the one that looks slightly purplish to me in the THCV area when I look at it in the sunlight. I don't know why they all have that horizontal line across them about halfway down.

Long post, but I think this is an interesting subject, and wish more people were into doing TLC.
https://www.amazon.com/gp/product/B077FHP4KH/ref=ppx_yo_dt_b_search_asin_title?ie=UTF8&psc=1

 

[Moe.Red]

So using both hexane and chloroform? I’m confused on your process a bit.

 

[Ali_Tarpate]

So using both hexane and chloroform? I’m confused on your process a bit.

I use hexane first, as the solvent for the extraction in the tubes, then chloroform for the eluent in a jar to soak the plates. Then I dissolve the fast blue in a sodium hydroxide solution. This is what I learned from the tutorial I follwed. I really dislike working with chloroform, too - it's so volatile, like it wants to crawl out of the bottle. Do you use chloroform for both processes?

 

[Moe.Red]

Can you link the tutorial you are following?

I did experiments early on with 2 chemicals, I wanted to see if my ethanol extractions could be the base for my chromatography column, and I was able to get good separation with eth bath and chloroform eluent. But I have not tried to do it the way you are.

You did get a good decarb but that straight line all the way up tells me there is an issue with the polarity of the chemicals - I think. Seems like your separation is only partial.

 

[Ali_Tarpate]

It's a forum like this, and a very long thread with many of the details later on.

This site will not let me post the link - it changes the URL to invalid.com !

Try this - it's rollitup dot org then /t/diy-thin-layer-chromatography-tlc-of-cannabinoids-at-home-tutorial.953423/

 

[Moe.Red]

It's a forum like this, and a very long thread with many of the details later on.

This site will not let me post the link - it changes the URL to invalid.com !

Try this - it's rollitup dot org then /t/diy-thin-layer-chromatography-tlc-of-cannabinoids-at-home-tutorial.953423/

OK, found it. This one is going to take a while to read, let me do that and get back to you tonight. Cheers.