syrian rue blew up

[spooner]

Just like the title says the rue fizzed up everywhere lol.

The Tao of Rue Extraction was the tek being used
100g of Esphand was ground up and boiled with 5 cups of water and 1 cup of vinegar for 1 hour
The result was then filtered through a mesh strainer and left to sit over night, this pull was performed 3 times
By morning the solids had seperated and the yellow liquid up top was Decanted off
The yellow liquid was filtered through cotton then coffee filters
Sodium carbonate was made by placing pure baking soda in the oven for 1 hour at 200F
8g sodium carbonate was mixed into 800ml of warm water and dissolved
the solution was then slowly poured into the yellow liquid and it slightly fizzed and made no color difference
sodium carbonate was put strait into the yellow liquid then it fizzed up crazy and went everywhere lol

Why was there no color change at all? As you slowly mix in sodium carbonate it should start pulling out the alks and making the liquid milky, none of this was happening

 

[Vodsel]

the solution was then slowly poured into the yellow liquid and it slightly fizzed and made no color difference
sodium carbonate was put strait into the yellow liquid then it fizzed up crazy and went everywhere lol

Why was there no color change at all? As you slowly mix in sodium carbonate it should start pulling out the alks and making the liquid milky, none of this was happening

The yellow liquid you filtered from the rue is acidic. Sodium carbonate will react at first with the acetic acid, first neutralizing the solution, then basifying it as pH goes above 7. Apparently your mix did not go over 7.

Solution: Add more base to the liquid, no need to dissolve it in water. Eventually it will reach the pH required for the alkaloids to precipitate.

 

[spooner]

Thankyou for the fast reply!
so just slowly keep adding the sodium carbonate?
and the way the carbonate was prepared seems correct?

 

[Vodsel]

Yes and yes. Keep adding it in small amounts, and stirring, until no more color change is appreciated. But at this stage of the extraction, a little excess of sodium carbonate will not hurt, so don't worry much.

Edit: Wrong, 200F is not enough. Sorry.

 

[spooner]

A couple of spoon fulls have been put in now and it just seems to be settleing at the bottom, would placing the jar in a hot water bath be beneficial?

 

[Vodsel]

A couple of spoon fulls have been put in now and it just seems to be settleing at the bottom

But did the solution turn milky with precipitate when adding/stirring?

pH raise will occur regardless of temperature at this level, there's no need to warm up the solution.

 

[spooner]

no it has all just settled to the bottom no color change occurred at all

 

[spooner]

that has been the color the whole time you can even see the carbonate just chillin at the bottom

 

[arcologist]

Are you sure you have sodium carbonate? 1 hour at 200 F maybe isn't enough to convert from bicarbonate, I've heard 400F is necessary to completely convert it. Sodium bicarbonate is a weak base compared to sodium carbonate so you won't get all of the harmaline to precipitate because you can't get the pH above around 8.5.

This would explain why you didn't observe a color change, it takes a pH of around 11 or 12 to fully precipitate all of the alkaloids, especially harmaline which is responsible for the milky quality (harmine is more red/brown).

 

[spooner]

well how long would you suggest I leave it in for then at 400F? computer said 1 hour at 200F is all that it needs. So is my soultion ruined now?

 

[spooner]

Or should the failed sodium carbonate be filtered out, then recook the baking soda at 400F for an hour

 

[Vodsel]

Even if what you added was not sodium carbonate but bicarbonate, some precipitation (harmine) should have occurred. But if you have a whole lot of solution now for those starting 100g, the alkaloids might be very dilluted and the precipitation might have been barely visible.

Regardless, your solution is not ruined. The alkaloids are there. If you're unsure about the sodium carbonate preparation, just bake some more using time and temperature in excess. One way to make sure that the conversion has been made (other than the subtle differences in both) is weight. Baking soda should lose about 20% of the weight in the conversion to sodium carbonate.

Edit: and according to the conversion wiki, arcologist is right. 200F is not enough. So my first "yes" was wrong, sorry about that. I always used sodium carbonate from the store.

 

[spooner]

Baking soda is being rebaked at 450F for a total of 2 hours
should the failed carbonate be filtered out?