Using Heptane to Make CBD Isolate Clarification

CannaBusiness
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Hello! I have been looking through the threads on this wonderful site, but am having trouble finding exactly what I am looking for. On another thread, a kind soul posted the below directions to make isolate with pentane quickly, but when I tried to do the same method using heptane it was not very successful in terms of crystal formation. Please let me know where I am going wrong. I made sure to ramp the temperature down relatively slowly (going down to 0C over the course of 5-6 hours).

  1. Measure distillate weight
  2. Heat distillate to within 5-10c of solvent (Pentane preferably)(36c)
  3. Measure out half the weight of the distillate in solvent (1g pentane : 2g distillate)
  4. Heat solvent to within 5c of BP (ideally in glass reactor w/ reflux attachment)
  5. Combine distillate and solvent, fully mix (supersaturation)
  6. Cool to room temp
  7. Cool to 0c (precipitation)
  8. When happy with crystallization pour off liquid
  9. Use 0c solvent to wash crystals to purity over filter paper
  10. Dry in vacuum oven

Because I am using heptane rather than pentane 5 degrees of BP is about 93 C compared to 31 C when using pentane. Thanks.

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So what do you get?

Given the greater delta-T (so more room to force solubility) I’d try using 30-50% less solvent…but I’ve only crashed with hexane, and only a couple or four times…so I’m spit balling here.

Imo it’s easier to figure out the correct solvent to solute ratio by starting with isolate and adding it to hot solvent until it stops going in. (Remember playing with sugar?!?). You could probably figure it out with a gram, but 100 might be more accurate.

Remember to take the potency of your distillate into account when back calculating.

Edit: not from an “isolate” thread, but works as confirmation bias

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The info you tagged me in is from running Magsil columns, its completely different…

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sure…and I explicitly stated that the number I was quoting was

what relevance does why you dissolved it at 1:1 have?

if you can get CBD into heptane at 1:1 to do anything with it, then dissolving it as 2:1 is the wrong move for making isolate (where the goal is to achieve super-saturation).

right?!?

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does this sound familiar?

maybe the spoon offered there is of help?!?

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I don’t see a lot of SOPs that suggest stopping at 0c. Try -15c to -30c if you’ve got the equipment required to do so.

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Oh, sure, But I wasn’t making isolate of any kind… I was doing it for chromatography… But yes you can use for less solvent and achieve supersaturation