vizio123321
Greenlighter
- Joined
- May 31, 2010
- Messages
- 1
This is my first post and i'm not sure if this is the right place. I apologize if it should be posted in another area.
My friend was doing an extraction of amphetamine sulphate from 30 mg XR pills. Initially 10 of these pills were well crushed and well dissolved in 7 mL of water. All non-water soluble material was removed by passage of the solution through a .22 micron filter. Here is how it went, my friend needs help understanding where he went wrong and additionally what the actual substance at the end was.
A tube of about 300 mg of theamp-sulphate and other water soluble impurities were dissolved in 7 mL distilled water. To this was added approximatley 300 uL of 10 M NaOH. The calculated pH was between 13 and 14 but not directly measured. The solution was mixed well and turned a milky white color. It was left to set for 5 min. and an oily layer formed on top. To this was added 7 mL of diethyl ether. The solution was mixed and allowed to settle for 10 min. The top (ether) layer was removed and placed in a seperate tube and the aqueous layer was re-extracted with approx. 4 mL diethyl ether. The solution was again mixed and allowed to seperate and the top ether layer was added to the original and the aqueous layer was discarded. A dilute solution of H2SO4 was prepared (i'm guessing around 500 mM) the pH was around 3.3. 10 mL of the H2SO4 solution was now added to the diethy ether and mixed. The solution was allowed to settle for 10 min, and the bottom (aqueous) layer was extracted with a pipette. The remaining ether was re-extracted with another 5 mL of the H2SO4 solution and added to the original. The ether layer was discarded.
The aqueous solution was then placed on a plate and allowed to evaporate for 2 days. At the end of the evaporation, there was a white sort or speckled crust on the plate. My friend scrapped off what he could (it was not a fine white powder, rather like really really small pieces of ripped up semi-moist toilet paper) Everything that could be scrapped hardly covered the end of a razor blade. My friend had originally intended to insullfate this but instead placed it on his tounge. Additionally, he redissolved what could not be scrapped off in water and drank 1/2 the water.
Almost instanttaneously he felt his legs were week and his heart was beating a little faster. His breathing was a little more labored. He layed down for about 20 min. thinking he may have taken too much amphet. He was not feeling well and started to become worried and nervous that he made a mistake that may land him in the hospital. He almost felt poisoned in a way. After some more time passed he found the strength to get up and took a long walk out side and drank lots of water. His heart rate was 90 BPM. There were NO euphoric effects as may have been anticipated with amphetamine, and what was happening did not feel like amphet. He returned, layed down on the bed, accually slept for 1 hour, and when he awoke, he felt almost completly back to normal. No comedown, no other effects, almost the same as before he sampled the evaporated substance. He concluded whatever was on the plate was not the amphetamine sulphate he tried to extract.
-The pKa of the basic nitrogen on the aliphatic amine is around 9.5.
Can anyone help my friend and offer advice on what they think might have happened? The effects of the ingestion were meant to serve as a guide in trying to figure out what it accually was he took.
Where did the amphet. go? Should the H2SO4 solution have been more acidic? SHould he have washed the original ether extract with distilled water?
He has been racking his brain on this and can not figure out what went wrong. If there is any advice he would greatly appreciate it.
Thanks
My friend was doing an extraction of amphetamine sulphate from 30 mg XR pills. Initially 10 of these pills were well crushed and well dissolved in 7 mL of water. All non-water soluble material was removed by passage of the solution through a .22 micron filter. Here is how it went, my friend needs help understanding where he went wrong and additionally what the actual substance at the end was.
A tube of about 300 mg of theamp-sulphate and other water soluble impurities were dissolved in 7 mL distilled water. To this was added approximatley 300 uL of 10 M NaOH. The calculated pH was between 13 and 14 but not directly measured. The solution was mixed well and turned a milky white color. It was left to set for 5 min. and an oily layer formed on top. To this was added 7 mL of diethyl ether. The solution was mixed and allowed to settle for 10 min. The top (ether) layer was removed and placed in a seperate tube and the aqueous layer was re-extracted with approx. 4 mL diethyl ether. The solution was again mixed and allowed to seperate and the top ether layer was added to the original and the aqueous layer was discarded. A dilute solution of H2SO4 was prepared (i'm guessing around 500 mM) the pH was around 3.3. 10 mL of the H2SO4 solution was now added to the diethy ether and mixed. The solution was allowed to settle for 10 min, and the bottom (aqueous) layer was extracted with a pipette. The remaining ether was re-extracted with another 5 mL of the H2SO4 solution and added to the original. The ether layer was discarded.
The aqueous solution was then placed on a plate and allowed to evaporate for 2 days. At the end of the evaporation, there was a white sort or speckled crust on the plate. My friend scrapped off what he could (it was not a fine white powder, rather like really really small pieces of ripped up semi-moist toilet paper) Everything that could be scrapped hardly covered the end of a razor blade. My friend had originally intended to insullfate this but instead placed it on his tounge. Additionally, he redissolved what could not be scrapped off in water and drank 1/2 the water.
Almost instanttaneously he felt his legs were week and his heart was beating a little faster. His breathing was a little more labored. He layed down for about 20 min. thinking he may have taken too much amphet. He was not feeling well and started to become worried and nervous that he made a mistake that may land him in the hospital. He almost felt poisoned in a way. After some more time passed he found the strength to get up and took a long walk out side and drank lots of water. His heart rate was 90 BPM. There were NO euphoric effects as may have been anticipated with amphetamine, and what was happening did not feel like amphet. He returned, layed down on the bed, accually slept for 1 hour, and when he awoke, he felt almost completly back to normal. No comedown, no other effects, almost the same as before he sampled the evaporated substance. He concluded whatever was on the plate was not the amphetamine sulphate he tried to extract.
-The pKa of the basic nitrogen on the aliphatic amine is around 9.5.
Can anyone help my friend and offer advice on what they think might have happened? The effects of the ingestion were meant to serve as a guide in trying to figure out what it accually was he took.
Where did the amphet. go? Should the H2SO4 solution have been more acidic? SHould he have washed the original ether extract with distilled water?
He has been racking his brain on this and can not figure out what went wrong. If there is any advice he would greatly appreciate it.
Thanks
Yeah the freebase is soluble in ether, even seen naphtha used in some teks. It's weird it didn't work, if an oil layer formed when it was basified there must have been a significant amount extracted in the first stage, it should have all dissolved in the ether and the amount of sulfuric acid should have been enough to extract it all from the ether.