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Let's grow a crystal. How to proceed?
- Thread starter steppa
- Start date
steppa
Rising Star
Ok.
As now two people suggested a slow evap I think I'll give it a try. Today I warmed it all up again to redissolve the xtals which formed in the test tube which I was using now to get them out of the tube. There was also some gunk at the bottom of the tube, which I left behind. Then I filled everything in another vessel to do a regular freeze perzip.
I think I also used waaay to much heptane. This is why I percip the xtals out first, then safe the heptane and then redissolve the xtals in the smallest ammount of heptane possible.
Or should I use another solvent? I have heptane, naphta and light naphta at hand. I guess light naphta will evap to fast? If not I'd like to use this.
As now two people suggested a slow evap I think I'll give it a try. Today I warmed it all up again to redissolve the xtals which formed in the test tube which I was using now to get them out of the tube. There was also some gunk at the bottom of the tube, which I left behind. Then I filled everything in another vessel to do a regular freeze perzip.
I think I also used waaay to much heptane. This is why I percip the xtals out first, then safe the heptane and then redissolve the xtals in the smallest ammount of heptane possible.
Or should I use another solvent? I have heptane, naphta and light naphta at hand. I guess light naphta will evap to fast? If not I'd like to use this.
I honestly can't tell the difference between light naphtha, heptane and hexane. Maybe the composition of naphthas in the UK tends to be closer to straight heptane/hexane or something. In all uses of the solvents I have noticed no difference at all.
You want to get the spice dissolved into a solution just above room temperature precipitation point when crystallizing this way. Just barely above that point. If you only get tiny crystals when the naphtha cools back to room temperature (assuming used heated naphtha to dissolve it) then that's fine. Top up with naphtha and they will dissolve back. You need to make sure all of it is dissolved at room temp. From that point on it's just a game of patience with the slow evap.
You want to get the spice dissolved into a solution just above room temperature precipitation point when crystallizing this way. Just barely above that point. If you only get tiny crystals when the naphtha cools back to room temperature (assuming used heated naphtha to dissolve it) then that's fine. Top up with naphtha and they will dissolve back. You need to make sure all of it is dissolved at room temp. From that point on it's just a game of patience with the slow evap.
soulman
Rising Star
The best crystals I ever got were by accident.
I normally get small fluffy powder like crystals with freeze precip from naptha using mhrb.
But one time, i left some spent naptha in glass having finished the process.
I had put cling film over the glass so it wouldn't evapourate, with intentions of re-using it another time.
Anyway, i forgot about it, and the cling film must not have been airtight, as when i came back to it, it had all evapourated, leaving me with a nice nugget of clear, thin shard like crystals, covered with a layer of orange oil. I think it was about 200mg
I normally get small fluffy powder like crystals with freeze precip from naptha using mhrb.
But one time, i left some spent naptha in glass having finished the process.
I had put cling film over the glass so it wouldn't evapourate, with intentions of re-using it another time.
Anyway, i forgot about it, and the cling film must not have been airtight, as when i came back to it, it had all evapourated, leaving me with a nice nugget of clear, thin shard like crystals, covered with a layer of orange oil. I think it was about 200mg
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downwardsfromzero
Boundary condition
Thought: an inert atmosphere keepeth the oxides away.