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list of experiments
Solubility book (3rd Edn)
To determine the solubility of 3,4-methylenedioxyphenylacetic acid in THF at 25C
Solubility of 3,4-methylenedioxyphenylacetic acid in methanol has been determined to be 1.0M at 25C
02:30 Placed a small amount of 3,4-methylenedioxyphenylacetic acid in a half dram vial.
02:40 Turned-on the "Lauda heating/cooling" device and set the temperature to 40C.
03:00 Pipetted out methanol (200uL) in to the vial and vortexed it for approximately one min.
03:05 The solid dissolved completely in to the solution, therefore added some more acid to the vial..vortexed it over again for another minute.
03:10 This time after vortexing some of the solid remained undissolved. This sample vial is labeled
03:20 Placed the vial in to the bath of the heating / cooling device with the temperature already set to 40C.
03:50 All the solid had dissolved- a clear homogeneous solution was observed..
03:51 Changed the temperature setting from 40C to 25C.
04:10 Obtained a video
of the solution with the temperature falling..
04:25 Temperature had reached 25C..
05:00 Observed solid crystals in the sample vial..
05:10 Obtained a clean and dry NMR tube, rinsed it with 200uL CDCl3 and then pipetted out 700uL CDCl3 (with 0.05%TMS v/v)
05:20 Removed the sample vial 132-1A from the bath.
05:21 Obtained a picture of the solution with some crystals reformed in it (
). A clear supernatant was visible.
05:25 Carefully pipetted out 100uL of the supernatant from the vial in to the NMR tube making sure it dropped directly in to CDCl3 in the tube and not touching the walls.
05:40 Obtained HNMR of the solution.
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