so having issues with an extraction at the moment on some acacia longifolia flowers:
.I soaked an unknown amount of flowers (didn't measure sorry) in methylated spirits for a few days until the flowers had lost all their yellow colour. the metho ended up a lime green colour.
. the metho was strained until completely transperant
. 20g NaOH was added to 100ml warm water. the solution was left until it went clear and then added to the metho solution. instantly the solution clouded with brilliant orange precipitation. the precipitates sat on top until the solution was agitated and then dissolved. the whole solution ended up a light orange colour
so the issue lies in the next step as I am unsure what is going on - I added about 80ml toluene to the solution. there was no distinct layer seen, even before being mixed... like adding water to water. it just seemed to become one solution. now I assume this had something to do with using a dominantly ethanol solution, but I've mixed non polar with ethanol solutions fine in the past.
the wierd thing is there is a very dark red layer of about 50ml sitting at the bottom of the flask. I thought that this may have been the toluene reacting strangely, so I separated it.. I was a bit naughty and put my finger in to see whether it felt like non polar solution or whether it was a soapy liquid (as would be with lye)... seemed the latter... and i just added some toluene again just then and no layer formed at the top. the solution cloudded up with beads of liquid suspended in the solution which eventually dissolved after agitation.. exact same thing happened with water... this has me completely stumped i've never seen anything like it. both non polar and polar area the same solution... and theres a wierd dark red solution at the bottom and i dont know what that is
Any input would be appreciated here. by the way... after adding the lye to the metho solution, the floral smell became really dominant. smells beautiful!
.I soaked an unknown amount of flowers (didn't measure sorry) in methylated spirits for a few days until the flowers had lost all their yellow colour. the metho ended up a lime green colour.
. the metho was strained until completely transperant
. 20g NaOH was added to 100ml warm water. the solution was left until it went clear and then added to the metho solution. instantly the solution clouded with brilliant orange precipitation. the precipitates sat on top until the solution was agitated and then dissolved. the whole solution ended up a light orange colour
so the issue lies in the next step as I am unsure what is going on - I added about 80ml toluene to the solution. there was no distinct layer seen, even before being mixed... like adding water to water. it just seemed to become one solution. now I assume this had something to do with using a dominantly ethanol solution, but I've mixed non polar with ethanol solutions fine in the past.
the wierd thing is there is a very dark red layer of about 50ml sitting at the bottom of the flask. I thought that this may have been the toluene reacting strangely, so I separated it.. I was a bit naughty and put my finger in to see whether it felt like non polar solution or whether it was a soapy liquid (as would be with lye)... seemed the latter... and i just added some toluene again just then and no layer formed at the top. the solution cloudded up with beads of liquid suspended in the solution which eventually dissolved after agitation.. exact same thing happened with water... this has me completely stumped i've never seen anything like it. both non polar and polar area the same solution... and theres a wierd dark red solution at the bottom and i dont know what that is
Any input would be appreciated here. by the way... after adding the lye to the metho solution, the floral smell became really dominant. smells beautiful!
