So there I was, doing an A/B extraction. Afterwards I needed to go back to the Lewis acid. As the freebase form is caustic and liquid and short-lived. Sure, I could dump some 37% hydrochloric acid into it, but it was non-polar (vm&p naptha) and the water in the hydrochloric acid meant it wouldn't precipitate and I would be left with a polar solution of
Acid salt that would need more work to collect. Here's what I came up with;
Here is the basic apparatus. 1000 ml erlenmeyer flask, for the Hcl acid. A Claisen adapter on your to facilitate the pressure equalizing funnel above it, which has a 24/40 to 19/24 adapter. On the other arm of the Claison adapter is the 100° turn down/ vacuum port of a vacuum distillation rig. The other side of the turn down has a 24/40 stopper
As you see the funnel did get the kek clips before I was done. The hot plate is only being used for the clamp. No way I could let this tower of glass free stand.
The hose comes out of the vacuum port of the 100° turndown, and goes to my vacuum pump cold trap, which is filled with H2So4, the dry the gaseous HCL. Then out another hose to the freebase container. This worked well and I learned a lot.
1. When the H2So4 hits the HCL (aq) it pressurized the entire contraption because there is some resistance created by the tubing and the second bubbler. As the pressure increased, the funnel gained pressure and was inclined to run-away (drip faster and faster). It took some effort to keep it dripping only a drop or 2 a second. You had to turn it on and then immediately turn it down but not off.more than once I dropped several millileters straight. Which gassed me as much as the RM
2. This vinyl tubing isn't great for hcl gas, I should have used the latex hose I have.
3. The stoichiometry, I couldn't find on line. Every post I seen asking about this particular route was met with " This is dangerous " and " you're going to put your eye out!". I started with a 1/1 mole ratiowhich was almost 3:1 Hcl:H2So4 because the hcl is 37% and the H2So4 was 95%. After I had used up the H2So4, I added more several times until I didn't get a reaction when it dripped. That amount was double what I started with. So the balanced equation is 2:3 H2So4:HCL. I'm not sure how many liters or cubic feet of gas I ended up making but it was 150 ml of 37%, or 55ml of pure hcl in the theoretical aqueous phase.
4. I set it up beside a window with a box fan blowing out, but it was still pretty nasty at times. HCL gas is heavier than air so it lies on the floor.
So there you have it. Criticism and critique are encouraged. I'll try to field any questions you might have. Thanks for looking!
P.S. I still don't know why my pictures are sideways. They weren't and then one day they were. If anyone knows how to fix that I'd like to know also
Acid salt that would need more work to collect. Here's what I came up with;
Here is the basic apparatus. 1000 ml erlenmeyer flask, for the Hcl acid. A Claisen adapter on your to facilitate the pressure equalizing funnel above it, which has a 24/40 to 19/24 adapter. On the other arm of the Claison adapter is the 100° turn down/ vacuum port of a vacuum distillation rig. The other side of the turn down has a 24/40 stopper
As you see the funnel did get the kek clips before I was done. The hot plate is only being used for the clamp. No way I could let this tower of glass free stand.
The hose comes out of the vacuum port of the 100° turndown, and goes to my vacuum pump cold trap, which is filled with H2So4, the dry the gaseous HCL. Then out another hose to the freebase container. This worked well and I learned a lot.
1. When the H2So4 hits the HCL (aq) it pressurized the entire contraption because there is some resistance created by the tubing and the second bubbler. As the pressure increased, the funnel gained pressure and was inclined to run-away (drip faster and faster). It took some effort to keep it dripping only a drop or 2 a second. You had to turn it on and then immediately turn it down but not off.more than once I dropped several millileters straight. Which gassed me as much as the RM
2. This vinyl tubing isn't great for hcl gas, I should have used the latex hose I have.
3. The stoichiometry, I couldn't find on line. Every post I seen asking about this particular route was met with " This is dangerous " and " you're going to put your eye out!". I started with a 1/1 mole ratiowhich was almost 3:1 Hcl:H2So4 because the hcl is 37% and the H2So4 was 95%. After I had used up the H2So4, I added more several times until I didn't get a reaction when it dripped. That amount was double what I started with. So the balanced equation is 2:3 H2So4:HCL. I'm not sure how many liters or cubic feet of gas I ended up making but it was 150 ml of 37%, or 55ml of pure hcl in the theoretical aqueous phase.
4. I set it up beside a window with a box fan blowing out, but it was still pretty nasty at times. HCL gas is heavier than air so it lies on the floor.
So there you have it. Criticism and critique are encouraged. I'll try to field any questions you might have. Thanks for looking!
P.S. I still don't know why my pictures are sideways. They weren't and then one day they were. If anyone knows how to fix that I'd like to know also