This is the 1st time I post, so my apologies if I am posting in the wrong place/way. I am a self-professed newbie having a lot of problems separating Naptha. I have read extensively on this site from the FAQ & troubleshooting sections to forum posts concerning separation « anxiety » (couldn’t resist…) I am using « QT’s Extraction for students » (from erowid - I know, I know, but I am already in neck deep and just want to get out so I can start a simpler tech…), with muriatic acid, naptha (Coleman camp fuel) for a solvent and NaOH (lye acquired in a soap-making shop) as a base. I used 133 g pre-powdered MHRB split into 4 large mason jars.
Followed the tech as closely as possible (but a vague tech leads to vague technique…). Here is an abreviated version of my lab notes (sorry for the length and the details, but I really have no idea where I went wrong):
Day 1 acidified demineralized water to ph 2. Poured to cover MHRB in 4 jars and shook till mixed. Heated under 50 degrees C (122F) then let sit.
Day 2 48 hours later – filtered all through coffee filters 2 X.
Repeated day 1 & 2 twice more then discarded MHRB.
Day 7 defatted with about 100 ml naptha in each jar. Shook vigorously for 20 mins.
Day 8 24 hours later : removed naptha and pink cloudy guck. Filtered through coffee filters 2 X (still some mhrb residue.)
Repeated day 7 & 8 twice more. No more visible MHRB residue.
Day 13 Mixed NaOH to ph 12 in tap water (ran out of demineralized water – is this where I went wrong ?) This is where things get a little sloppy; Added teaspoon after teaspoon of base to defatted jars (tech called for about 10, but when I got to 30 in each jar (containing an extraction from an initial 33g MHRB in each) there was still no heat or change of colour or consistency. I added 2 tsp NaOH to my remaining (approx) 500ml of base. And added tsp after tsp – at 8 a reaction started (grey to black sludge, but curiously no temperature change…) and by 12 tsp I reached target ph (11 in my case – although very difficult to tell ph differences between 10 and 13 : green grey to grey green to grey, so I can’t really be sure of the exact ph…) Oh yeah, shook vigorously all the while (what can I say – I’m a noob! I won’t shake next time I promise…)
Day 14 Now things get strange: 24 hours later and the mixture seems to have separated into 3 distinct layers : a 2mm band of burgundy liquid sandwiched between two layers of grey sludge ! I remixed (this time by slowly overending jars for 10 mins each to avoid bubbles & emulsion…) then let sit for 48 hrs.
Day 15 Same 3 layers. Following the troubleshooting guide on this site, I added 25 ml naptha & remixed slowly and waited 5 hours . No change. Added 4 tsp of same NaOH preparation as before.
Day 16 24 hrs later. Some change : mixture has now separated into 2 layers -
the liquid has settled to deep burgundy (a grey silt like sediment has accumulated on the bottom) and the solvent has sort of separated into a distinct layer, although seems to be emulsified if I understand the term correctly (bubbles, not translucent and pinkish in colour). There is however, a thin film of clear solvent on the top (roughly ½ mm…). Added 5 tsp of NaOH mixture, mixed end over end, put in warm water, cooled and waited :
Day 17 no change… Added 2 tsp of salt into one jar as a test, then overended to mix (curiously, it thickened up, turned to black sludge and despite my efforts to the contrary, formed thick bubbles on the surface). 10 hours later, full circle : a thin burgundy layer sandwiched between 2 thick grey layers !
At a loss as to what to do next… only thing i haven’t tried is filtering through cotton. Doesn’t sound like it’ll work and I am dreading it, but if I’m told to, I’ll buckle up and hit it. Current status is 3 jars in 2 lyers as per day 16 and one in grey sandwich hell as per day 17.
I can send pictures if it’ll help, but my camera battery is charging at the moment. I have 2 (obvious) questions : What did I do wrong and what do I do next? thanks in advance, guys.
Followed the tech as closely as possible (but a vague tech leads to vague technique…). Here is an abreviated version of my lab notes (sorry for the length and the details, but I really have no idea where I went wrong):
Day 1 acidified demineralized water to ph 2. Poured to cover MHRB in 4 jars and shook till mixed. Heated under 50 degrees C (122F) then let sit.
Day 2 48 hours later – filtered all through coffee filters 2 X.
Repeated day 1 & 2 twice more then discarded MHRB.
Day 7 defatted with about 100 ml naptha in each jar. Shook vigorously for 20 mins.
Day 8 24 hours later : removed naptha and pink cloudy guck. Filtered through coffee filters 2 X (still some mhrb residue.)
Repeated day 7 & 8 twice more. No more visible MHRB residue.
Day 13 Mixed NaOH to ph 12 in tap water (ran out of demineralized water – is this where I went wrong ?) This is where things get a little sloppy; Added teaspoon after teaspoon of base to defatted jars (tech called for about 10, but when I got to 30 in each jar (containing an extraction from an initial 33g MHRB in each) there was still no heat or change of colour or consistency. I added 2 tsp NaOH to my remaining (approx) 500ml of base. And added tsp after tsp – at 8 a reaction started (grey to black sludge, but curiously no temperature change…) and by 12 tsp I reached target ph (11 in my case – although very difficult to tell ph differences between 10 and 13 : green grey to grey green to grey, so I can’t really be sure of the exact ph…) Oh yeah, shook vigorously all the while (what can I say – I’m a noob! I won’t shake next time I promise…)
Day 14 Now things get strange: 24 hours later and the mixture seems to have separated into 3 distinct layers : a 2mm band of burgundy liquid sandwiched between two layers of grey sludge ! I remixed (this time by slowly overending jars for 10 mins each to avoid bubbles & emulsion…) then let sit for 48 hrs.
Day 15 Same 3 layers. Following the troubleshooting guide on this site, I added 25 ml naptha & remixed slowly and waited 5 hours . No change. Added 4 tsp of same NaOH preparation as before.
Day 16 24 hrs later. Some change : mixture has now separated into 2 layers -
the liquid has settled to deep burgundy (a grey silt like sediment has accumulated on the bottom) and the solvent has sort of separated into a distinct layer, although seems to be emulsified if I understand the term correctly (bubbles, not translucent and pinkish in colour). There is however, a thin film of clear solvent on the top (roughly ½ mm…). Added 5 tsp of NaOH mixture, mixed end over end, put in warm water, cooled and waited :
Day 17 no change… Added 2 tsp of salt into one jar as a test, then overended to mix (curiously, it thickened up, turned to black sludge and despite my efforts to the contrary, formed thick bubbles on the surface). 10 hours later, full circle : a thin burgundy layer sandwiched between 2 thick grey layers !
At a loss as to what to do next… only thing i haven’t tried is filtering through cotton. Doesn’t sound like it’ll work and I am dreading it, but if I’m told to, I’ll buckle up and hit it. Current status is 3 jars in 2 lyers as per day 16 and one in grey sandwich hell as per day 17.
I can send pictures if it’ll help, but my camera battery is charging at the moment. I have 2 (obvious) questions : What did I do wrong and what do I do next? thanks in advance, guys.
The oily spot looks very much like SWIM's pulls when she uses heated naptha.