- Merits
- 42
I've done an A/B TEK this weekend using Q21Q21's A/B TEK with vinegar and lime and had a very disappointing yield. Looking at it, I don't think I've even managed to get a 0.1 or 0.2% yield.
First of all: the materials that I've used are of the right chemical composition. I've gone to great lengths to acquire laboratory grade lime and the vinegar that I used contains 8% acetic acid. The naphtha that I used worked fine in a previous STB TEK. My MHRB was bought from mimosahostilis.mx and is a renowned source on these forums.
I have whole MHRB, so I used a coffee mill to chop them up in fibers and small quantities of powder. I made sure the fibers were are fine as possible and I measured off 100 grams of MHRB to get the hang of this TEK before trying a larger batch. When mixing in the vinegar I quickly noticed that the 100ml that I was supposed to use wasn't enough. So I added about 175ml of vinegar and approx the same amount of water. Thoroughly mixed it all and I let that mix sit for about an hour while I mixed it 4 to 5 times at various intervals. I weighed off the amount of lime that I was supposed to use and gradually mixed it in, concluded it was way too wet and kept adding lime. Now, I'm not entirely sure but I don't think I've added a factor 1.75 of the required lime to compensated for the higher amounts of water/vinegar. So, this could be a reason why the yield is so low.
Next up I let that mix sit for about 12 hours and at various intervals mixed it a bit. The day after I added the naphtha but used more than in the TEK, about 1.5x / 1.75x of what the TEK said. Again, I could've used too much and the DMT wouldn't crystallize due too much naphtha. So I'm currently evap'ing the naphtha in front of a fan.
So, there are a few things that I'm considering:
- Add more lime to the mix, stir it thoroughly, let it sit for 12 to 24 hours and then do another pull
- Evap half the naphtha and then do a freeze precip(currently happening)
Any other thoughts? Is there anything I can do with the current batch or should I consider it lost?
First of all: the materials that I've used are of the right chemical composition. I've gone to great lengths to acquire laboratory grade lime and the vinegar that I used contains 8% acetic acid. The naphtha that I used worked fine in a previous STB TEK. My MHRB was bought from mimosahostilis.mx and is a renowned source on these forums.
I have whole MHRB, so I used a coffee mill to chop them up in fibers and small quantities of powder. I made sure the fibers were are fine as possible and I measured off 100 grams of MHRB to get the hang of this TEK before trying a larger batch. When mixing in the vinegar I quickly noticed that the 100ml that I was supposed to use wasn't enough. So I added about 175ml of vinegar and approx the same amount of water. Thoroughly mixed it all and I let that mix sit for about an hour while I mixed it 4 to 5 times at various intervals. I weighed off the amount of lime that I was supposed to use and gradually mixed it in, concluded it was way too wet and kept adding lime. Now, I'm not entirely sure but I don't think I've added a factor 1.75 of the required lime to compensated for the higher amounts of water/vinegar. So, this could be a reason why the yield is so low.
Next up I let that mix sit for about 12 hours and at various intervals mixed it a bit. The day after I added the naphtha but used more than in the TEK, about 1.5x / 1.75x of what the TEK said. Again, I could've used too much and the DMT wouldn't crystallize due too much naphtha. So I'm currently evap'ing the naphtha in front of a fan.
So, there are a few things that I'm considering:
- Add more lime to the mix, stir it thoroughly, let it sit for 12 to 24 hours and then do another pull
- Evap half the naphtha and then do a freeze precip(currently happening)
Any other thoughts? Is there anything I can do with the current batch or should I consider it lost?
