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Cold filtering😫😫😫😫

JRotten

JRotten

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Get Shredded!
So I decide to make up some MastE. Fair enough, just a few vials worth so I grab a nalgene and hand pump. Everything is cool, I get everything in the vials about to cap and it's cloudy... wtf?! So I figure the humidity is affecting my powder or just somehow I've got moisture in there. Back to the stirrer and hot plate, see some steam coming off so I figure I'm good. I filter again with a nalgene... clouds up again almost instantly. Maybe I'm missing something, so I switch my bottle of carrier, figure i'll go all in, I double the batch using all my powder, back on the stirrer, give it a nice warm stir while I sterilize my vacuum filtration setup, break out the electric pump, let the oil cool ALL the way down to room temp, no cloudiness... and I swear to god I've been sitting here watching this fucking thing drip since Jesus was a baby.

If I never post again it's because I died of old age waiting for this shit to filter. FML
 
I used to cold filter my T3s, good times.
 
You have to be gentle with the powders man... you were probably cursing and carrying on while brewing.

The powders don't like negative energy or they cloud up.


...p.s. I cleared my inbox.
 
tone said:
You have to be gentle with the powders man... you were probably cursing and carrying on while brewing.

The powders don't like negative energy or they cloud up.


...p.s. I cleared my inbox.
Click to expand...


Tone..... i want to slap your face
 
What temp are you filtering at "cold" just room temp? I have a hard time getting everything to blend at just room temp. I had a batch of Mast turn out exactly how yours did. I would still think moisture is the likely culprit. I threw out that batch started again and added another 5% BB and it turned out fine. I use a cheap infrered temp gun to filter between 110-130 with no issues. It goes reasonably fast (10 minutes or so for 500mL).

I bought an electric pump thinking it would make life easier but nothing gets a gold medal like the old mighty vac pump.
 
I blame nalgene and being to warm on the initial filter. It is now crystal clear. Yes I filtered the final time at room temp to allow anything that was in solution warm to fall out and filter. I give up on plastic filtration. I bought a real vacuum filtration setup for $130 and the filters cost me about $0.50 per batch. It requires sterilization, clean up and and a stash spot, but I feel better about the gear and have no issues.
 
JRotten said:
I blame nalgene and being to warm on the initial filter. It is now crystal clear. Yes I filtered the final time at room temp to allow anything that was in solution warm to fall out and filter. I give up on plastic filtration. I bought a real vacuum filtration setup for $130 and the filters cost me about $0.50 per batch. It requires sterilization, clean up and and a stash spot, but I feel better about the gear and have no issues.
Click to expand...

I have had the same exact issue with Nalgene bottletops. Thinking about switching over to a glass unit. Just feel its a pain in the ass to disperse say 250mls to 10ml vials. Right now I use Media bottle with a septa cap turning the 250ml media bottle into a large vial and from there I fill my vials.

Any ideas?
 
Yep. Working with a flow hood the easy way is to pour from the vacuum nipple.. (thank you Phil.. my dumbass would have never thought to pour from there)
 
tone said:
Yep. Working with a flow hood the easy way is to pour from the vacuum nipple.. (thank you Phil.. my dumbass would have never thought to pour from there)
Click to expand...

I know, when I was taught that little trick, I couldn't believe I hadn't thought of it myself...
 
Any technique that reduces the number of transfers/glassware required without sacrificing accuracy, is the way to go. Having said that. A little practice, and pouring right from the neck of the receiver flask into the vial can be done quite well.

I learned to pour into 1ml vials with the 13mm neck size(the narrow neck most pharm. vials use) directly from the neck of 100ml and 250ml volumetric flasks when I was doing a lot of quantitative analysis work. Saves a lot of time, and pipettes. You almost don't believe it can be done until someone shows you, though. Your first though is "Yea fuckin right, you want me to take that volumetric flask and pour into that tiny little 1ml vial without dumping the whole thing in my lap, yea fucking right."

JR, I don't know if this little gem has made it your way or not, but get a roll of teflon tape at the hardware store. It's a pure film of teflon used to help seal threads on water/gas pipes. Put a couple of wraps on the male part of your ground glass connection. BAM, no more leaking, no more stuck joints. And, if you find your filter membrane support leaking between the funnel and the lower fritted part, put a couple of wraps around the OUTSIDE of that joint after it has been assembled, the vacuum will do the rest to keep it sealed up. Be careful, you will be able to pull a much harder vacuum now that you have done these two things, you'll have to find something else to do with your time that you save filtering...

I need to write a book, Practical Lab Techniques and Beyond: An Introduction to Practical Chemistry and Lab Techniques for the Entrepreneur.
 
Phil6502 said:
Any technique that reduces the number of transfers/glassware required without sacrificing accuracy, is the way to go. Having said that. A little practice, and pouring right from the neck of the receiver flask into the vial can be done quite well.

I learned to pour into 1ml vials with the 13mm neck size(the narrow neck most pharm. vials use) directly from the neck of 100ml and 250ml volumetric flasks when I was doing a lot of quantitative analysis work. Saves a lot of time, and pipettes. You almost don't believe it can be done until someone shows you, though. Your first though is "Yea fuckin right, you want me to take that volumetric flask and pour into that tiny little 1ml vial without dumping the whole thing in my lap, yea fucking right."

JR, I don't know if this little gem has made it your way or not, but get a roll of teflon tape at the hardware store. It's a pure film of teflon used to help seal threads on water/gas pipes. Put a couple of wraps on the male part of your ground glass connection. BAM, no more leaking, no more stuck joints. And, if you find your filter membrane support leaking between the funnel and the lower fritted part, put a couple of wraps around the OUTSIDE of that joint after it has been assembled, the vacuum will do the rest to keep it sealed up. Be careful, you will be able to pull a much harder vacuum now that you have done these two things, you'll have to find something else to do with your time that you save filtering...

I need to write a book, Practical Lab Techniques and Beyond: An Introduction to Practical Chemistry and Lab Techniques for the Entrepreneur.
Click to expand...
. I use parafilm I have for mycology
 
JRotten said:
. I use parafilm I have for mycology
Click to expand...

It will help with the seal, but make sure none of your product comes in contact with it.

A little tip about the parafilm you may or may not know.

The parafilm is designed to be stretched before usage. (good god damn thing, that shit is expensive!)
One layer of parafilm will allow free air exchange (oxygen etc.)
Two layers of parafilm will NOT allow free air exchange.
 
tone said:
Phil.. me you and a few select members need to start our own forum.
Click to expand...

I agree you two are wizards!

personally i would like to see admin here make a sub for you guys to kick around. Same with Zygl for a supplement subforum
 
Using the millipore stericup i found if i filter above 50deg C it eats the plastic in the top even with glass receiver, must be heat solvent combo and thats only using 2% 18%(no eo) just made it very very slightly cloudy.\

next time will try 30deg C
 
If im not mistaken, the plastic that couples and holds the filter on the stericup is wither HIPS or PES, neither suitable for use with the solvents we use.

Guys, NONE of the bottle top filters or syringe filters are really made to filter non-aquesous solutions. They were really designed for use with aqueous solutions like growth media and tissue culture growth fluids.

The only way to get this stuff to work without any problems, ever, is to be using all glass and either a nylon or PTFE membrane. PVDF will work almost all the time, but ANY other material plus BA, BB and oils like MCT or MIG and you're asking for trouble, not to mention using EO and Guaiacol.

These little differences are the whole difference between a high PIP batch and a smooth as silk batch.
 
Has anyone ever purged previously opened oil or solvent bottle in a vacuum chamber. Been a few months since using them and wonder how hydrophilic some of this stuff is?
The fact that 97% ethanol drops in percentage each time exposed to open atmosphere made me start thinking about this.
 
Phil6502 said:
If im not mistaken, the plastic that couples and holds the filter on the stericup is wither HIPS or PES, neither suitable for use with the solvents we use.

Guys, NONE of the bottle top filters or syringe filters are really made to filter non-aquesous solutions. They were really designed for use with aqueous solutions like growth media and tissue culture growth fluids.

The only way to get this stuff to work without any problems, ever, is to be using all glass and either a nylon or PTFE membrane. PVDF will work almost all the time, but ANY other material plus BA, BB and oils like MCT or MIG and you're asking for trouble, not to mention using EO and Guaiacol.

These little differences are the whole difference between a high PIP batch and a smooth as silk batch.
Click to expand...


Very new to this all apart from syringe filtering.
With glass can you get sterile filter membranes.

I presume with glass as well, filtering temp isnt such a worry and as you said harsher solvents.
 
Teejay said:
Very new to this all apart from syringe filtering.
With glass can you get sterile filter membranes.

I presume with glass as well, filtering temp isnt such a worry and as you said harsher solvents.
Click to expand...
Depends on your filter material. A vacuum filtration apparatus uses whatman filter circles so yes .22micron nylon filters are about 25 cents. You can still melt the filter, but the filtration setups really do work a lot better and the filter is at least supported by a particle type filter as well.
 
Teejay said:
Very new to this all apart from syringe filtering.
With glass can you get sterile filter membranes.

I presume with glass as well, filtering temp isnt such a worry and as you said harsher solvents.
Click to expand...
Depends on your filter material. A vacuum filtration apparatus is all glass and uses filter paper, I prefer nylon. You can still melt the nylon if you are super hot.
 
JRotten said:
Depends on your filter material. A vacuum filtration apparatus is all glass and uses filter paper, I prefer nylon. You can still melt the nylon if you are super hot.
Click to expand...

This...

You want to filter while it's still warm.. but let it cool back to room temperature before you distribute into your vials. Hot oil expands. You will come up short on your fill lines if you don't let it cool down to room temperature.
 
So the glass filtration filters ptfe are paper? I haven't been able to find 47mm sterile ptfe membrane. The circular?
 
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