MrAcuminata
Rising Star
G'day team, had some success extracting white crystals from 50g AANPRB with a yield of 0.6% so far and potentially more soon. I believe the freezer I'm using doesn't quite get cold enough to crash everything out first go so the second freeze is currently in progress. If more crashes out the yield goes up. Stay tuned. This is the best I've gotten from a 50g run so far.
KEY DIFFERENCES IN MY APPROACH:
- Instead of going straight to a 2hr acid bath at the start, I added just under boiling acidic solution (200ml distilled water and 50ml vinegar) in the bark vessel and left it to soak over the previous night before beginning the extraction the following day.
- This time I took a "less is more" approach to my acetic acid and sodium hydroxide values, using 20g NaOH instead of 25g for basifications.
- At the first basification stage I allowed an extra hour worth of heat baths to really give the soup time to do it's thing.
- The crude xylene pulls (5 x 50ml) that followed were done in a cold shed (it's winter here currently) so this time I kept the soup warm with additional baths as required.
- These Xylene pulls underwent a further A/B with a 1:4 vinegar to distilled water solution at room temp (250ml total)
- This time the Shellite/Naphtha (5 x 50ml) pulls that followed the 2nd basification were done much cooler than my previous attempts where I was heating excessively.
- Finally instead of putting the combined pulls straight in the freezer, I placed the dish on a chair and used a fan to blow cold air on it until i could see the shellite clouding.
KEY DIFFERENCES IN MY APPROACH:
- Instead of going straight to a 2hr acid bath at the start, I added just under boiling acidic solution (200ml distilled water and 50ml vinegar) in the bark vessel and left it to soak over the previous night before beginning the extraction the following day.
- This time I took a "less is more" approach to my acetic acid and sodium hydroxide values, using 20g NaOH instead of 25g for basifications.
- At the first basification stage I allowed an extra hour worth of heat baths to really give the soup time to do it's thing.
- The crude xylene pulls (5 x 50ml) that followed were done in a cold shed (it's winter here currently) so this time I kept the soup warm with additional baths as required.
- These Xylene pulls underwent a further A/B with a 1:4 vinegar to distilled water solution at room temp (250ml total)
- This time the Shellite/Naphtha (5 x 50ml) pulls that followed the 2nd basification were done much cooler than my previous attempts where I was heating excessively.
- Finally instead of putting the combined pulls straight in the freezer, I placed the dish on a chair and used a fan to blow cold air on it until i could see the shellite clouding.
