Home TLC Thin layer chromatography

[PhenoMenal]

I didnt read the full thread

I've read the full thread about three times, which is about as many times as i've seen every Seinfeld episode

Would love to see links to your sources for the correct dye

for security reasons that's probably not a good idea, but you've got the CAS number now (5486-84-0, "Fast Blue BB Salt") so there's nothing stopping you getting the correct one

Just google around, and if you cant find any Add To Cart's that you like simply email some labs and ask if they can get it in for you. Because it needs to be stored in the freezer it's best if you can find a lab in your country, then they'll probably send it over in a box of dry ice.

 

[theJointedOne]

I've read the full thread about three times, which is about as many times as i've seen every Seinfeld episode

not that there's anything wrong with that

 

[dongle]

Yeah I skimmed over it like I said. Got most of the important details to get started. Would have had immediate success if I bought premade plates to begin with rather than trying to DIY

 

[G.O. Joe]

I mean, for fucks sake, why not just clearly specify gypsum in the product description?

What did you want and what is so wrong with gypsum? If you buy silica gel plates or TLC powder you deliberately buy those the 60, G, F254 or UV254, RP-2, RP-18. Maybe the particle size is specified in the ad, maybe not. Maybe the percentage of CaSO4, maybe not. After such scenarios you'd think sellers would go to requiring the business account.

It's possible to make plates with the tape and rod method or dipping or pouring, but notice the fineness of the silica and binder sold for TLC. If gel for column chromatography (or homemade or commercial silica gel) and plaster is substituted it should be milled down. I wonder what happens with different inorganic additives in the slurry, for cannabinoid analysis. Silver nitrate on prepared plates is very effective in some separations but some simple alternative can surely be found for mixing in homemade plates, for specific separations such as THC and CBD.

Fast Blue BB base can be converted with ice, hydrochloric acid, sodium nitrite, sodium chloride, and zinc chloride, if you're up to the challenge.

 

[dongle]

G.O. Joe, do you offer consulting services, by chance?

 

[Jack El Frutero]

If you google "062-05463" you'll see a few references. Store in your freezer.

Thanks, PhenoMenal, I've just placed an order for correct salt, $170 for 5g, ouch!

 

[Jack El Frutero]

Fast Blue BB base can be converted with ice, hydrochloric acid, sodium nitrite, sodium chloride, and zinc chloride, if you're up to the challenge.

How challenging is the procedure?

Thanks.

 

[dongle]

Thanks, PhenoMenal, I've just placed an order for correct salt, $170 for 5g, ouch!

Are you in the USA?

What did you pay for the 100g of thr wrong one?

 

[dongle]

Looks like this stuff breaks down pretty quick even under indoor fluorescent lighting. Had this stuff in clear dipping container with clear plastic wrap about 5ft away from a 4x 4' fluorescent tube fixture and after a couple hours the bright yellow liquid turned almost clear. I didnt really make notice until I saw one of the plates not dying correctly.

 

[dongle]

Wet plate, crude BHO. Top plate, I fell asleep at the wheel and let it develop too long. From top lane to bottom lane, 3 application spot, 1, 2.

Bottom plate, same sample, top to bottom: 3 small applications, 2 small, 1 big, 1 small.

Seems 1 "big" application followed by 2 small applications is best.
Dry plate, same:

4 lane plate under UV during developing, highlighting spot size and intensity

Degraded/spent FBBB solution:

Fresh solution for comparison:

 

[Jack El Frutero]

Are you in the USA?

What did you pay for the 100g of thr wrong one?

Yes.

$105.

 

[dongle]

If you can get it from Sigma, I think it was $58 for 5g

 

[G.O. Joe]

G.O. Joe, do you offer consulting services, by chance?

I'm not sure I have anything to sell, especially with me not being in the cannabiz or a legal state.

How challenging is the procedure?

Thanks.

There are two parts. The first paragraph of Organic Syntheses collective volume 3 page 295 describes the first part of the process for making Fast Blue B from its base, a typical diazotization (tetra-azo actually).

In a 1.5-l. beaker are placed 400 ml. of water and 31 ml. of concentrated hydrochloric acid (sp. gr. 1.19). This solution is heated to boiling, the flame is removed, and 40 g. (0.16 mole) of o-dianisidine (Note 1) is added. The hot mixture is stirred for about 3 minutes, until only a small amount of solid remains. The beaker is then placed in an ice-salt mixture and its contents are stirred mechanically until the temperature has dropped to about 15°. At this point 35 ml. more of concentrated hydrochloric acid is added. When the temperature of the mixture has fallen to 10–13°, a solution of 23.3 g. (0.33 mole) of 97% sodium nitrite (or an equivalent amount of sodium nitrite of higher or lower purity) in 50 ml. of water is added from a dropping funnel in the course of 10–15 minutes. The contents of the beaker are then stirred for 15–20 minutes at 5–10°, and finally filtered rapidly with suction from an appreciable amount of dark material (Note 2).
1. Eastman Kodak Company's technical grade, melting at 133–135°, was used.
2. Usually the pores of the filter paper become partially clogged after about half of the mixture has been filtered so that the rate of filtration is cut down considerably. In this event a fresh funnel and filter should be employed.

The second part is precipitating this as the zinc salt, by mixing with an aqueous solution saturated with salt and zinc chloride and letting it sit.

 

[dongle]

After reading that, paying street cocaine prices seems reasonable.

 

[Jack El Frutero]

Thanks, G.O. Joe!

 

[PhenoMenal]

Houston this is dongle, we have good separation!
looks like some healthy CBG levels in that sample too

 

[dongle]

Houston this is dongle, we have good separation!
looks like some healthy CBG levels in that sample too

IIRC 3rd party analytical lab HPLC/MS testing shows 91.x% d9thc and 1.5% cbg on this sample.

I'm a little disappointed no one asked why the 1st single-lane test I did with the premade plates was noticeably streakier than the subsequent ones...

 

[PhenoMenal]

so why was the 1st single-lane test you did with premade plates noticeably streakier than the subsequent ones?

(you've just got up and running and still experimenting with dialing it in, so i didn't think anything of it!)

 

[dongle]

so why was the 1st single-lane test you did with premade plates noticeably streakier than the subsequent ones?

I have no fuckin idea.

What, you think I'm a chemist or something?

 

[dongle]

Just kidding.

I think it might be due to skipping the oven "activation" step. I'll see if I can repeat it again.

Do you cook your plates in the oven to drive off any built up moisture prior to use? I've been throwing a couple 10x20 plates in the convection oven for about 110C for half an hour, and storing it in a ziplock bag until ready for use.