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Old 11-05-2004, 03:41 AM   #1
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Has anyone successfully made a homebrew gel?

Has anyone successfully brewed up their own gel using Carbomer940? Ive been reading and searching as much as I could, and the best instuructions I could find were in this thread:

Help with making gel

It sounds simple enough. I tried an 8Oz test run, (I mixed all the ingredients together, adjusted the PH, and then tried adding the Carbomer 940 to no avail - which isnt what's recommended but once I saw that Carbomer clump up I know what people are talking about when they say its a pain in the ass)

Using this reciepe:
Isopropyl Alcohol 40%
Isopropyl Myristrate 12%
Isopropyl Palmitate 12%
Oleic Acid 10%
Propylene glycol 10%
DMSO 10%
D-Limolene 6%

Im about to just order some spray heads from lemelange and go with a spray, just to get my cycle started. Also considering adding PEG400 to the mix.

Any advice??

BV
 




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Old 11-05-2004, 11:07 PM   #2
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Well, gave another shot following these directions:

Quote:
Carbomer 940 can be used to gel a mix better than 934.
Mix .5 g carbomer to the 10% gycerol and mix well.
It will take up to 15 minutes for the carbomer to wet and disperse
Adjust the pH of this initial mix to 7.2-7.4 with triethanolamine or a drop or two of NaOH
Add this to the rest of the ingredients and check pH again.
If you use OA the pH will instantly drop to acidic and you will have to adjust again.
If gelling the brew be sure to use an adequate volume of d-Limonene as this is the emulsifier that allows the water and oil based ingredients to mix.

When making a gel the order of addition is very important.
First, add the carbomer to the PG/glycerol/PEG-400 and allow to "wet".
If you are not using a hand mixer it will take up to 30 minutes to properly wet. Mix well.
Second, add the other water soluble ingredients and mix well. Adjust with the TEA (triethanolamine)
...usually it will take about 1 mL per gram of carbomer give or take a bit. It will gel immediately.
I would not recommend adding the DMSO until the end as polar compounds (DMSO and i-prop) tend to make the carbomer clump.
After it gels add the oil soluble ingredients and mix well. Voila! A lotion is born!
Chemo
And still no success!! I was using NaOH to basify, and I dont think that's a good idea. Adding all the water-soluble ingredients together (except the IPA and DMSO, I tried to bring the PH up to 7.4 and after a few drops of concentrated NaOH solution, a white precipitate fell out of the solution.

I think triethanolamine is the only way to go here. Plus, the lithmus paper I have dosent seem to read PH properly once greasy materials like P.Glycol, IPM, and IPP are added to the mix.

Any way, I tried mixing everything together, and I got a murky whiteish solution, and big glop of clear gel at the bottom. I added NaOH dropwise with constant stirring trying to get it to dissolve, but nothing.

In order to do this right, Im going to need triethanolamine and a good digital PH meter,and its too much of a hassle.

So spray it is!! Ill work on this gel stuff later, considering I already have the Carbomer940.

BV
 




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Old 11-06-2004, 12:08 AM   #3
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Quote:
Originally Posted by BigVrunga
Well, gave another shot following these directions:



And still no success!! I was using NaOH to basify, and I dont think that's a good idea. Adding all the water-soluble ingredients together (except the IPA and DMSO, I tried to bring the PH up to 7.4 and after a few drops of concentrated NaOH solution, a white precipitate fell out of the solution.

I think triethanolamine is the only way to go here. Plus, the lithmus paper I have dosent seem to read PH properly once greasy materials like P.Glycol, IPM, and IPP are added to the mix.

Any way, I tried mixing everything together, and I got a murky whiteish solution, and big glop of clear gel at the bottom. I added NaOH dropwise with constant stirring trying to get it to dissolve, but nothing.

In order to do this right, Im going to need triethanolamine and a good digital PH meter,and its too much of a hassle.

So spray it is!! Ill work on this gel stuff later, considering I already have the Carbomer940.

BV
Add more NaOH to thicken the gel, but I was never able to make a good high capacity gel with a number of carbomers. Liquids can hold much greater concentrations. I may try some other matrix one day, maybe HPC or something, I'll let you know if it works, but I'd say don't waste you time bud.
 



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Old 11-06-2004, 06:40 PM   #4
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Thanks for the input once again, Dr.D. I agree, the spray has just as good or better absorption and is FAR less of a pain to mix in your kitchen. Ive been looking into MethylCellulose as another gelling agent, seems like that's what's most often used in commercial gel-type products, like lotions and soaps. Maybe adding some PEG400 might increase the solubility of products in the gel?

Im going to give it one more shot. Starting with 50ML DH2O, adding .5g Carbomer940 and then bringing up the PH until I get a gel. Then, Ill add my water soluble ingredients, D-Lim, Proylene Glycol and finally Oleic Acid. We'll see what happens!

For those that are interested, here's some info on why Carbomer and MethyCellulose work the way they do, and some info on how to use them in a solution:

http://www.chemistrystore.com/Using%...lcellulose.htm

http://www.personalcare.noveoninc.co...inalsafety.pdf

Thanks,
BV
 




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Old 11-06-2004, 07:28 PM   #5
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Partial success!!! Added 1/4tsp Carbomer940 to 50ml DH20, let it sit for 10minutes after some vigorous stirring. Added 5 drops Concentrated NaOH, and VIOLA! Superthick gel!!! Nice!

Mixed in 30ml IPA, and it stayed in gel form.

Now, Im trying this:

Started with 97ml 91% IPA, added 1/2tsp Carbomer940. I thought about it, and I dont know what ingredient in the original to replace with the DH20. So, if I can gel up the 97IPA I need, and then each ingredient one at a time I may have it. Water solubles first, then the D-Lim, then the PG. After each ingredient, if I see the solution start to crash, Ill add NaOH dropwise until it goes back to a gel.

Hmmm...its crazy, but it just might work!

BV
 




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Old 11-07-2004, 04:16 AM   #6
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YES! Ive got a beaker with 240mL of a creamy white lotion that looks, feels, smells, evaporates, and burns exactly like the original BDC T-gel. Whoohoo!!

Basically, the original liquid transdermal recipe is not suited to gelling with Carbomer, it has to be modified.

I started with 25ml DH2O and added 1/4tsp Carbomer940. After this had become throroughly saturated, I brought the PH up with a concentrated NaOH solution (1tsp NaOH in 50ml DH20). The solution became a thick gel immediated after about 4drops of NaOH.

Then I added 75ml 91% IPA, which thinned out the gel a bit and mixed right in. Started adding 23ml Oleic Acid next, and the solution broke up into a clumpy gel, started to turn a milky white.

I added the Oleic Acide a little at a time,adding NaOH dropwise each time to bring the PH up and put the mix back into a gel. I had to add about 1.5ml NaOH before I came back to a smooth consistency.

Started to add IPM, and it would not mix with the gel. After some thorough mixing, nothing. I added a little DH2O and it went right in. That was the key. Still a bit clumpy though. Added more NaOH and it smoothed out a little bit, but still not what I wanted. I had about 100ml of gel that I had made earlier from 50ml dH2O, Carbomer, and IPA. I dumped the solution I was working on (about 125ml worth) in with this and mixed it together, and the extra IPAgel gave it a nice consistency. It seemed a little out of solution (some IPM and IPP wouldnt go in) - a little more dH2O fixed that up.

I took 175ml of this IPM/IPP/IPA/Oleic Acid gel and poured it into a separate beaker. To this I added 25ml DMSO, which mixed right in. Added 15ml D-Limolene, and finally 25ml Propylene Glycol, which mixed nicely thanks to the D-Lim and gave the gel a nice, smooth, lotion-like thickness. No clumping whatsoever, its perfectly smooth and has properties very similar to T-Gel.

Broke out my digital PH meter, measured the PH of the final mix at ~5.8

So, the PG,DMSO,and D-Lim are still at their original concentrations of 10%,10%,and 6%. The IPA,IPM,IPP,and OA have all been cut with dH2O to facilitate gelling with the Carbomer. I dont have exact measurements yet, but I can estimate that its more like:


IPA 25%
IPM 9%
IPP 2%
OA 8%
DMSO 10%
PG 10%
D-Lim 6%
dH2O 30%

I dont know how much the PH solubility or absorption was affected by cutting with water - Im pretty sure that since the DMSO is still at 10% it wouldnt be reduced from the original formula.

It evaporates quickly and leaves the skin feeling soft and slightly greasy. It burns a bit at first, but so did T1 the first few times I applied it.

Now Ill mix up some spray (WAY less of a hassle!!), and see which one I like better.

BV
 




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Old 11-07-2004, 01:09 PM   #7
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That's kind of what I did by gelling up water and IPA initially. Its the OA that drops the PH, but its also a penetration enhancer so its not something you want to leave out.

You dont have to add a lot of base to get the solution to gel, I just kept stirring and adding NaOH drop by drop and it gels as soon as the proper PH is reached. Initially gelling the Carbomer in H2O and IPA made a huge difference, though.

You could make a decent gel from H2O,IPA,DMSO,DLim,and PG but I dont know how effective it would be.

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Old 11-07-2004, 02:45 PM   #8
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It could work - Sodium Bicarbonate is a weaker base than NaOH, but then again is is triethanolamine, which is the base most often used in cosmetics. You might have to add too much Sodium Bicarbonate, which could affect the solubility of the PH's you're trying to dissolve in the gel.

The issue here is - you might have to initially buffer the water/carbomer solution too high in order for it to stay in gel form after adding the oleic acid. If the PH goes too high, the carbomer will precipitate right out of the mix.

An idea might be to mix the Oleic acid/water FIRST, then bring that to a PH of 7.5 - 8 and try to gel that with the carbomer. THEN add IPA,IPM. Once you get the IPM mixed in you're golden - the other products gel up just fine. I did water/carbomer into a gel, and then IPA, then the Oleic. After gelling the Oleic acid, I didnt really need to adjust the PH again.

The final PH of my mix was around 5.8, which is right about what commercial lotions and soaps are at.


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Old 11-07-2004, 06:38 PM   #9
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Klaus,
I understand what you're getting at - it could work very well but I dont have the materials to experiment with it at the moment.

From what Ive seen, PH isnt so much of an issue with making the gel. Its that a good concentration of H2O has to be present in order for all the ingredients in the orignal BDC spray recipe to gel correctly. If there isnt enough water, you can add as much base as you want and all you'll get is a clumpy mess.

Im going to try and nail down a reliable method here - so far its:

1.)dH2O/Carbomer
2.)adjust PH until a gel forms
3.)add IPA
4.)add Oleic acid
5.)adjust PH until it goes back into a gel
6.)add IPM/IPP
7.)add water until smooth
8.)add DMSO(10%)
9.)add D-Limoene(6%)
10.)add PG(10%)

You dont need an electric mixer or anything, I was using a glass stir rod and everything mixed just fine.

Now, to see if 10g of 4AD will dissolve in the gel I just made...

BV
 




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Old 11-07-2004, 09:31 PM   #10
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Quote:
Originally Posted by Klaus
Oh, I was under the impression that pH was causing the clumpiness, not the H2O concentration. Hmm... that does make it a bit more complicated.
Yes, it is, but after a certain inflection point, the pH has no greater gelling effect. In fact, after about 7.5 it's detrimental.
 



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Old 11-08-2004, 12:33 AM   #11
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Yes, a good case indeed! I was thinking dibasic potassium phosphate, but I'm not sure what it would do to the formula dynamics. Only with the IPM would it work for sure I'd say. These more complex formulas create a lot of stability issues. I don't remember the effective pH range for penetration, but the optimum is slightly acidic I'd guess, so maybe another buffer than what I was thinking would be better. Solubility characteristics will be the limiting factor.
 



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Old 11-08-2004, 01:51 AM   #12
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I think its a great idea, but the PH of the solution really isnt that big of an issue from what Ive seen.

The PH was causing the clumpiness to a degree, but the added H2O is what allowed the IPA/OA/H2O gel to mix with the other ingredients.

With Carbomer and PH, I noticed that too acidic of a solution caused the gel to break up into 'globs'. The carbomer was still dissolved, but it was very clumpy. Too high of a PH, and the Carbomer crashed out of solution.

Without enough H2O, the IPM/IPP wouldnt mix with the gel.
The average PH of your skin is 5.5, I think that's ideal for most lotions. Dont know what the ideal for penetration enhancement is, though.
 




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Old 11-08-2004, 03:50 AM   #13
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Well, 10g of 4AD wouldnt go into the gel. It took about 6 grams and then started to separate. I finally got 10g in about 320ml of gel, which is definately less than ideal!

Im going to give this another shot with PEG400.

BV
 




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Old 11-08-2004, 07:55 AM   #14
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You may need to increase the alcohol concentration, or dissolve you hormones in the alcohol before you add. Like I said, I experimented a lot with this years ago, but then decided, why? What's wrong with solution? I know that works and could think of no real advantage in the gel. Even had I figured it out, I couldn't think of an application where I'd favor it over the liquid. If you look at the EtOH concentration of Rx AndroGel, they use 68.9% and that's only at 1% test! It takes too long to dry also and requires a big surface area. Why not make a high-power liquid w/ 10%+ concentrations capacity to cover small, thin areas? Nevertheless, if you get the formula right, let me know and I'll probably try it anyway! I'd think that the alcohol content will have to be kept as high as possible and water minimized. Also, have you thought of using alternate acids like cap or lin in place of the OA?
 



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