Making your own DIY salt nic with benzoic acid.

[charlie1465]

I have been meaning to post this for some time as a description of my findings when making nic salts at home for the first time. but I have been prevaricating for a while and the BA took ages to arrive from Poland I will post each element of the process as I complete it.

Tonight we are making and quantifying the Benzoic acid solution.

The process is pretty simple but there is a bit of basic maths involved and of course you need VG and or PG, nicotine in PG and of course Benzoic acid.

Ok the baseline for this is the juul patent which says that 0.3g of benzoic acid should be mixed with 0.4g of nicotine. This can be said to be 300mg BA to 400mg nicotine.

I made a 10% BA solution in VG by mixing 10g BA with 90g VG. Heat was applied up to 55 degrees C and the mixture was stirred and shaken to dissolve as much as possible. Assuming that the specific gravity of VG is 1.25 (90g of VG is approximately 72ml) we then have a solution containing 138mg/ml Benzoic acid.

Ok i'm going to leave that overnight, agitate some more in the morning with more heat and then make the 50/50 nic salts. I see you tomorrow

 

[charlie1465]

Ok so left the BA solution overnight then reheated in microwave and shook for about half an hour. I'm currently waiting for that to settle out so that I can judge how much is in solution compared to yesterday.

As I write it looks like it still hasn't dissolved in the VG properly. I will wait and see and then possibly do another solution using PG instead. It's strange because although BA is a substance which is said to have partial solubility it is supposed to dissolve well in both VG or PG.

 

[classwife]

Moved to DIY from General E-Liquid Discussion

 

[charlie1465]

Moved to DIY from General E-Liquid Discussion

Ok thanks I wasn't sure if this was general or Liquid Or DIY...it's both really I suppose

 

[charlie1465]

Ok so the heat worked and I ended up with a fairly thick creamy VG/BA solution. So we have a solution at 138mg/ml of BA solution which we need to mix with the correct proportion of nic solution to achieve a given nic strength in a salt form.

I have 100mg/ml nic in PG. So in each ml of nic base you will need 0.544ml of 138mg/ml BA solution to get to the 3:4 ratio as required by the Juul patent. The 0.544 figure was worked out as follows 0.544ml of 138mg/ml equals 75mg of BA and 1ml of 100mg/ml nic base equals 100mg of nic base and 75:100 is a 3:4 ratio.

AS it's simpler to work out I am going to make 100ml of flavoured eliquid salt nic. I put 36 ml of 100mg/ml nic PG base in a 120ml bottle (this leaves some shaking room). Then we need to add 36 x 0.544 which equals 19.6ml of the BA solution. Then we need to add PG , VG and flavouring to make it up to 100ml at the ratio of PG/VG we require.

In my case I added 30.4ml of pure PG and then topped the bottle up to the 100ml mark with pure VG giving me a 50/50 PG/VG liquid.

Oh and I forgot to add that about 10ml of my final PG was added via PG based flavouring to achieve 100ml of flavoured 36mg/ml nic salt liquid ready for vaping.

Now it's ready for a few weeks of steeping before I test it for the first time.
I hope this helps someone especially all the european's who can't get nic salts above 20mg/ml and only then in 10ml shots. Cheers guys

 

[puffon]

Keep us posted....

 

[IDJoel]

Ok thanks I wasn't sure if this was general or Liquid Or DIY...it's both really I suppose

Just as general guideline: General e-liquid discussions apply to commercial, or ready-to-vape, e-liquids. If it is something that is being created, augmented, or otherwise "doctored;" then it falls into the realm of DIY... and it better suited to the DIY E-liquid sub-forum.

Formulating your own nicotine salts is definitely the purview of DIY.

 

[IDJoel]

As I write it looks like it still hasn't dissolved in the VG properly. I will wait and see and then possibly do another solution using PG instead. It's strange because although BA is a substance which is said to have partial solubility it is supposed to dissolve well in both VG or PG.

I don't know any of the specifics for benzoic acid. But, I am aware that other solid/crystalline ingredients (citric acid, menthol crystals) have different saturation levels based on the solvent chosen (VG, PG, water, ethyl alcohol).

Ethyl alcohol is often a very effective solvent; and can be (relatively) easily evaporated. Thus, leaving the target ingredient suspended in the remaining carriers (for vaping purposes; PG, and/or VG).

Water is another good solvent; though does not evaporate as easily as ethyl alcohol. However, being neither PG, or VG, does not effect the overall PG/VG ratio.

PG is often a better solvent than VG (in that is often has higher saturation thresholds). But, does effect the final PG/VG ratio.

VG seems to routinely(?) have the lowest saturation point of the four.

I would research benzoic acid solvents, solubility, and saturation levels (in various carriers/solvents), and consider one of the others, for additional experiments. At least to my thinking, the goal is to achieve the greatest level of saturation, in order to minimize the introduction of the additional/unecessary carrier.

 

[Morgan_Drury]

Ok so the heat worked and I ended up with a fairly thick creamy VG/BA solution. So we have a solution at 138mg/ml of BA solution which we need to mix with the correct proportion of nic solution to achieve a given nic strength in a salt form.

I have 100mg/ml nic in PG. So in each ml of nic base you will need 0.544ml of 138mg/ml BA solution to get to the 3:4 ratio as required by the Juul patent. The 0.544 figure was worked out as follows 0.544ml of 138mg/ml equals 75mg of BA and 1ml of 100mg/ml nic base equals 100mg of nic base and 75:100 is a 3:4 ratio.

AS it's simpler to work out I am going to make 100ml of flavoured eliquid salt nic. I put 36 ml of 100mg/ml nic PG base in a 120ml bottle (this leaves some shaking room). Then we need to add 36 x 0.544 which equals 19.6ml of the BA solution. Then we need to add PG , VG and flavouring to make it up to 100ml at the ratio of PG/VG we require.

In my case I added 30.4ml of pure PG and then topped the bottle up to the 100ml mark with pure VG giving me a 50/50 PG/VG liquid.

Oh and I forgot to add that about 10ml of my final PG was added via PG based flavouring to achieve 100ml of flavoured 36mg/ml nic salt liquid ready for vaping.

Now it's ready for a few weeks of steeping before I test it for the first time.
I hope this helps someone especially all the european's who can't get nic salts above 20mg/ml and only then in 10ml shots. Cheers guys

 

[ScottP]

I have been meaning to post this for some time as a description of my findings when making nic salts at home for the first time. but I have been prevaricating for a while and the BA took ages to arrive from Poland I will post each element of the process as I complete it.

Tonight we are making and quantifying the Benzoic acid solution.

The process is pretty simple but there is a bit of basic maths involved and of course you need VG and or PG, nicotine in PG and of course Benzoic acid.

Ok the baseline for this is the Juul patent which says that 0.3g of benzoic acid should be mixed with 0.4g of nicotine. This can be said to be 300mg BA to 400mg nicotine.

I made a 10% BA solution in VG by mixing 10g BA with 90g VG. Heat was applied up to 55 degrees C and the mixture was stirred and shaken to dissolve as much as possible. Assuming that the specific gravity of VG is 1.25 (90g of VG is approximately 72ml) we then have a solution containing 138mg/ml Benzoic acid.

Ok i'm going to leave that overnight, agitate some more in the morning with more heat and then make the 50/50 nic salts. I see you tomorrow

I am not a chemist but I thought I heard people were adding the BA directly to the nic base without making a separate solution first.

 

[charlie1465]

Just as general guideline: General e-liquid discussions apply to commercial, or ready-to-vape, e-liquids. If it is something that is being created, augmented, or otherwise "doctored;" then it falls into the realm of DIY... and it better suited to the DIY E-liquid sub-forum.

Formulating your own nicotine salts is definitely the purview of DIY.

Thanks...I started this thread in General eliquid but @classwife moved it and gave me a slapped wrist

 

[charlie1465]

I don't know any of the specifics for benzoic acid. But, I am aware that other solid/crystalline ingredients (citric acid, menthol crystals) have different saturation levels based on the solvent chosen (VG, PG, water, ethyl alcohol).

Ethyl alcohol is often a very effective solvent; and can be (relatively) easily evaporated. Thus, leaving the target ingredient suspended in the remaining carriers (for vaping purposes; PG, and/or VG).

Water is another good solvent; though does not evaporate as easily as ethyl alcohol. However, being neither PG, or VG, does not effect the overall PG/VG ratio.

PG is often a better solvent than VG (in that is often has higher saturation thresholds). But, does effect the final PG/VG ratio.

VG seems to routinely(?) have the lowest saturation point of the four.

I would research benzoic acid solvents, solubility, and saturation levels (in various carriers/solvents), and consider one of the others, for additional experiments. At least to my thinking, the goal is to achieve the greatest level of saturation, in order to minimize the introduction of the additional/unecessary carrier.

Yes thanks @IDJoel In fact I did a lot of research and read several very scholarly papers. You are broadly correct regarding the soluability of Benzoic acid. Mine is in a very pure form so was particularly stubborn.

The mistake I made in the first place was to not heat the solution enough. When heated to the correct temperature it disolves readily at this concentration. Eg. 10g BA in 90g (72ml) VG. I needed a VG solution for my final liquid PG/VG ratios.

So to conclude...heat is essential to make the BA dissolve especially in VG. It does dissolve more readily in PG.

 

[charlie1465]

I am not a chemist but I thought I heard people were adding the BA directly to the nic base without making a separate solution first.

Yes but the reasoning behind my method is to avoid heat exposure for the nic base. Whether it can be done without heat I don't know but I am very pleased with the results from a days steeping. I'll post a picture below.

 

[charlie1465]

This is the finished salt liquid with a 50/50 ratio and added flavouring. It's a strawberry cream flavoured 36mg/ml salt nic eliquid 100ml.

 

[charlie1465]

I am super happy with how crystal clear this is. The next thing that could be done is to test the PH but I don't have any indicator at the moment. From my reading the PH should come out to around 6 due to there being some acid's still present from the freebase nic/BA reaction

I hope this helps someone.

 

[charlie1465]

Just a thought...I would be very interested to hear some comments from the experienced commercial salt liquid user as a colour comparison??

The only thing that might skew this is that my nic was very slightly oxidised. And of course the added flavourings. My nic base was a very light amber colour. You could hardly notice the colour though when mixed with the added PG and VG so i'm guessing that most of the colour is as a result of the reaction and/or flavourings?

Any thoughts?

 

[IDJoel]

Thanks...I started this thread in General eliquid but @classwife moved it and gave me a slapped wrist

No worries. Classy has had to move more than one of mine too!

It is a learning curve; and most of the Mods/Admin are pretty tolerant, to honest mistakes. That's what they are here for.

Yes thanks @IDJoel In fact I did a lot of research and read several very scholarly papers. You are broadly correct regarding the soluability of Benzoic acid. Mine is in a very pure form so was particularly stubborn.

I your searching, and reading; did you ever come across anything that gives an idea how fast the reaction takes place? I have no idea if it is instantaneous. Or, if it takes time (and, if so, how much?).

Just a thought...I would be very interested to hear some comments from the experienced commercial salt liquid user as a colour comparison??

I have only bought two bottles of commercial e-liquid (salt). Both were roughly the same color as yours. I have also seen at least one vendor (Nicotine River) say this, about nic salt appearance, on their website:

(source)

 

[charlie1465]

I your searching, and reading; did you ever come across anything that gives an idea how fast the reaction takes place? I have no idea if it is instantaneous. Or, if it takes time (and, if so, how much?).

To be honest no not explicitly but there are hints within the stuff I have read that the process 'starts' immediately so that implies that there is a time dependant process.

In my attempt I mixed the BA solution which was the colour of milk with the freebase and then topped up the other ingredients (PG/VG Flavours). At that stage it looked extremely cloudy as you would expect from the addition of the cream like BA solution and that after shaking for about 10-15 minutes...no heat. I then put it in my usual steeping area and when I went back to check it about 3 hours later it looked like the above pictures.

So in conclusion there is a reaction which takes time to complete but as for exactly how much time all I can say is less than 3 hours. I'll control for this element of the process next time

 

[charlie1465]

@IDJoel It's very pleasing that the colour seems to be correct according to your experience and also the statement by pur nic that you quoted. I am going to try and steep as I normally would for any flavoured e liquid and then test in my pod to start with.

All being well this will enable anyone in my eurozone to easily make salts with their existing freebase which will save them purchasing two separate bases which is difficult enough anyway.

I will report back after testing

 

[sonicbomb]

I take my hat off to your chemistry skills. Personally I wouldn't trust myself to do this, especially not as the product would be going in my lungs.