How to test polymerization - FWFL

How do you test whether or not the mineral oil & castor oil has fully polymerized, while making Felix’s World Famous Lube?

I stirred one batch at 300F for 30 minutes, but the two oils separated. Then I added stearic acid (accidental FWWFL version) and heated repeatedly. At room temperature, it is nearly one color and applesauce in consistency. When heated, it separates into two oils. If I stir it when heated, it will remain mixed. I only see the two colors when it is cooling down, but not yet apple sauce (grease?).

I stirred a second batch (1/2 cup mineral oil & 1/4 cup castor oil) for 90 minutes at about 320F (minimal fumes emitting from the pot). I have not added anything to this two oil mixture. It has cooled down now, but I see two different oils. The mineral oil is very cloudy - not clear as it was in the bottle. The castor oil portion is also cloudy, but still the same color as in the bottle.

Note: I am using a laser thermometer. The emissivity value was set empirically, and temperatures may be off 10-ish degrees.

Does the cloudiness indicate polymerization?

> How do you test whether or not the mineral oil & castor oil has fully polymerized, while making Felix’s World Famous Lube?
I don't have an answer for this.

However, just because you see 2 "oils" separate afterward does NOT mean polymerization did NOT occur.
In other words, if polymerization occurs, you will not necessarily always have one homogeneous liquid afterward.

It could be the case that complete polymerization occurred but there was an excess of one of the oils so that the
excess (which did not get used during polymerization) will still appear as a one of the separate oils,
and the other separate oil is the polymerized oil.

when you add the stearic acid or sodium sterate it should cause the 2 oils to stop separating.
if not, add some more.

http://www.castpics.net/subsite/Lube/Felix.html

The high heat is what does the trick. You want it all just bellow the smoke point. Keep a class B fire extguisher near by and the door open. More than one screaming fire has happened making this lube.

I now use a hot plate outside for lube cooking

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My understanding, and I'm by no means a chemist, is that polymerization changes the oil from short chain molecules to long chain molecules. The two different oils used here, castor oil and mineral oil, probably have a different specific gravity and thus separate when they cool. The polymerization process doesn't give the two oils the same specific gravity, it changes the molecules. I made a batch of FWFL a few years ago and I experienced the same issue you describe. I just shook the jar with the polymerized oils to mix them well just before measuring out the correct amount for the batch I was making. That's been about 8 years ago. I'm still using that batch and it has always worked as advertised. I didn't add the stearic acid to the oils until the recipe called for it later in the process.

If polymerization does not join different oil chains together, then the freezing points for the polymerized oils should be greater than than of the virgin oils.

I used a syringe to collect 2 tsp of the cooked castor oil, and the cooked mineral oil. I placed each in a 4 ox mason jar. I put 2 tsp of the virgin oils in mason jars too. Then I put these four mason jars inside a glass baking pan, and filled the pan halfway with water. Then the pan/water/oil assembly went into the fridge.

After 10 minutes, the virgin castor oil has a higher viscosity than the cooked castor oil. The cooked castor oil seems to have some mineral mixed in homogeneously.

The two mineral oils are too close to tell a difference as of yet. More to come...

Roughly 45F, and the virgin castor is still significantly more viscous than the polymerized version. Not much different between the virgin & polymerized mineral oil.

I placed the assembly in the freezer. When the water in the glass baking pan developed a skin of ice (32F), the polymerized mineral oil was noticeably cloudier than the virgin oil. The virgin caster oil is near the consistency of Vaseline, but still some fluidity is observed. The polymerized castor oil is cloudier & runnier than the virgin. The polymerized castor oil also shows signs that mineral oil may be precipitating out as droplets.

If mineral oil is precipitating out of caster oil at 32F, then I wonder if the polymerization is being reversed.

24 hours at -8F and the two mineral oils are noticeably different - the polymerized version is significantly more viscous and cloudy. The polymerized version of the castor oil is less viscous and cloudier. The polymerized castor oil also has small white droplets that precipitated.

I think I can see the polymerization. After 7 days of sitting in a mason jar at room temperature, the caster oil has developed droplets.

The droplets appear to have a higher viscosity but similar density as the more fluid regions of castor oil. When I tip the jar on its side, the droplets at the bottom of the jar almost stick to the wall. Droplets floating in the castor oil look like air bubbles, but I believe they just won’t mix with the more liquid region. Pictures attached.

Attachment 278740Attachment 278741

I’ll look at my frozen samples soon, and make another post if I find anything different from what I previously shared.

I will heat this jar to 170F now, so I can take a 3 tbsp sample for mixing 98% sodium stearate 1 grain at a time until I have a homogeneous mixture/suspension. That may delay &/or affect future observed changes to this mixture.

The frozen samples were at -12F for a few days now.

The virgin castor oil is frozen solid, but the polymerized castor oil is not. The polymerized castor oil is mostly frozen & white, but a small region of clear sludge is present in the middle. The white beads I mentioned earlier are probably the same droplets as my room temperature experiment, but they frozen sooner.

The virgin mineral oil has a different surface tension from the polymerized mineral oil. The polymerized mineral oil curls at the glass jar surface when the jar is tipped like water beading on wax. The virgin mineral oil flows up the wall of the glass jar when tipped, wetting the surface (i.e. not beading).

That’ll be all for my freezing experiment. The reduction in freezing temperature of the polymerized castor oil is surprising, because a simple elongation of the hydrocarbon chain should increase the freezing temperature. All well, something changed. Time to make some lube and see what happens.

So indicators of polymerization: 1) Droplets precipitate in the castor oil (both at room temperature & during the freezing process), that seem to have higher viscosity & higher freezing temperature. 2) Increased viscosity of the mineral oil when held around -8F. 3) Both oils show cloudiness when cold.
Of course, this assumes polymerization has actually occurred and I didn’t make some error in the process.

Heating the oil mixture produced interesting results.

170F - the more liquid portion of the castor oil did mix with the mineral oil, but the higher viscosity droplets did not mix.

200F - The oils separated, but mix same as at 170F. The droplets may be dissolving a little, but quickly grow again when the stirring is stopped.

250F - Before mixing, bubbles can be seen rising from the bottom of the mason jar. Stirring produces a small amount of foam. Mixture is more clear than at lower temperatures. Non-mixing droplets persist.

275 - The droplets at the bottom of the jar are boiling, but are too heavy to float to the top. Droplets stuck in the bottom audibly sizzle when poked with a spoon. When I pick a loose droplet up with a spoon, it falls back to the bottom like a rock.

280F - Some smoking, and the boiling droplets are creating ticking noises.

The failure of the droplets to mix with the rest of the oil is curious.

Why did the droplets take days to form?

Is it best for the soap to be added before droplets are formed, or does that not matter?

I decided to use sodium stearate (98% pure) instead of soap, since ivory has changed over the years. 5 grains of sodium stearate is about the saturation point, but I had to put 6 grains in to know. What happened was the heavy droplets in the more liquid phase of castor oil became suspended in the mineral oil, and the liquid phase of the castor oil did not mix. So I worked my way up to an additional 15 grains of stearic acid (purity unknown), and now everything is emulsified at room temperature. Time to mix it with bees wax and see how bad I did ��

Note: The heavy droplets in the castor oil were pretty much totally emulsified with the first grain of sodium stearate. So my concern about not adding the soap when polymerization is first completed was not legitimate.

I cut the green stuff out of a purchased bullet and pan lubed. Looks ok...

Attachment 278869

This leaking onto a sheet of paper occurred in a thermal chamber at 55C [131F], but not at 53C [127.4F]. The sample did not melt at 59C [138.2F]. Temperature started at 40C and raised to 59C over a period of 5 hours. The picture without lube is just the underside of the paper.

Attachment 278993Attachment 278994

I was thinking about the oil that weeped into the paper at 55C, and about the heavy castor oil with droplets. So I made a very small batch of lube using only castor oil with droplets - I extracted (with syringe) the heaviest half of the polymerized castor oil that I had previously frozen.

The result was a weep temperature of 62C. This batch of lube was harder and did not stick to the paper, so I need to repeat this experiment to ensure equal ability of the two lines to contact the paper and transfer weeping oil near the melt temp of the wax.

I also need to figure out if the lube works if the mineral oil is discarded after polymerization is complete.

Heavy droplets (not air, sinks quickly in mineral oil) in the heaviest 50% of castor oil:
Attachment 279074

Oil weep at 62C:
Attachment 279075

I shot 13 rounds through my Uberti .45 Colt SAA, using 255 grain cast bullets from Hunters Supply, lubed with my last concoction that had no mineral oil. The lands and grooves inside this barrel do not look very smooth, and the gun’s history is unknown.

Not sure if some powder touched wax residue on the bottom of the bullets, but there seems to be in burnt powder in my barrel. Loaded with 8 grains of True Blue, which should be going around 900 fps.

The barrel isn’t clean, but I don’t think I see leading - kinda inexperienced there. There is some waxy residue on the muzzle of the barrel, which was wiped dry before I went out.

Four of my last six bullet holes were touching each other, from 20 yards free hand shooting. So accuracy is good.

I was worried that using only castor oil would cause accuracy issues from being too slippery, or that the harder mix might cause leading. Neither happened, so I’ll shoot some more and see if things get too dirty. If no issues there, I’ll try to raise the weep & melt temperatures again.

The mineral oil gets consumed. When I separate the mineral oil from the castor oil after polymerizing, I notice a 25% reduction in the volume of mineral oil.The result is the mix ratio goes from 2:1 to 1:1.

I’ve also noticed that the oils become darker, but this could just be due to heating the oils.

Might want to change the lube but anyway ... https://web.wilkes.edu/arthur.kibbe/lab6.html
Blending of Immiscible Liquids