DIY ways to check for esters in oil?

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A well made lubricant grade ester is essentially odorless. The only definitive way to know the type and quantity of ester is by gas chromatography.

Tom NJ
 
Originally Posted By: Tom NJ
A well made lubricant grade ester is essentially odorless. The only definitive way to know the type and quantity of ester is by gas chromatography.

Tom NJ


GC for the win!!!
 
One guy here thinks you break down the base oil composition with an electron microscope
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HPGC.
 
Originally Posted By: azsynthetic
Originally Posted By: Pablo
One guy here thinks you break down the base oil composition with an electron microscope

HPGC.


If you want to know the actual chemical structure of the oil then you will need an electron microscope. Gas chromatography just don't cut it. The more you know.......

http://www.imp.mx/investigacion/microscopia/en.php


SEM for sure has insufficient resolution for atoms and individual bond detection. Did you even read the link you pasted?

http://www.imp.mx/investigacion/microscopia/en.php?imp=lab2

If you can find some actual evidence to back your claim, we would all love to read it. Thanks.
 
Originally Posted By: Pablo


If you can find some actual evidence to back your claim, we would all love to read it. Thanks.


"There are several methods for the quantitative and qualitative analysis of elements in new
and used engine oils: inductively coupled plasma atomic/optical emission spectroscopy or mass
spectroscopy (ICP-AES/OES, ICP-MS), flame or graphite furnace atomic absorption
spectroscopy (FF-AAS/GF-AAS) or energy/wavelength dispersive X-ray fluorescence
spectroscopy (ED/WDXRFS). For the determination of the composition of tribofilms on different
test-pieces methods based on transmission or scanning electron microscopy (TEM/SEM), ultra
high vacuum tribometer (UHVT), Auger electron spectroscopy or scanning Auger microscopy
(AES/SAM), electron energy loss spectroscopy (EELS), X-ray or UV photoelectron
spectroscopy (XPS/UPS) are used."

http://www.vurup.sk/sites/vurup.sk/archi...2008_1_Sagi.pdf

http://www.slideshare.net/corematerials/chemical-analysis-in-the-electron-microscope

Like I have told you previously, knowing the elements in the oil is different than knowing their composition in the oil. Water has hydrogen and oxygen, but in what composition?
 
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Originally Posted By: azsynthetic

Like I have told you previously, knowing the elements in the oil is different than knowing their composition in the oil. Water has hydrogen and oxygen, but in what composition?

Water composition is 2 atoms of H and 1 atom of O. The O is in the center and the H atoms are covalently bonded to the O. The H atoms form a 104 degree angle with each other.

Waters composition is well known. I don't understand why this example was used or what you meant by it.
 
Last edited:
Originally Posted By: azsynthetic
Originally Posted By: Pablo


If you can find some actual evidence to back your claim, we would all love to read it. Thanks.


"There are several methods for the quantitative and qualitative analysis of elements in new
and used engine oils: inductively coupled plasma atomic/optical emission spectroscopy or mass
spectroscopy (ICP-AES/OES, ICP-MS), flame or graphite furnace atomic absorption
spectroscopy (FF-AAS/GF-AAS) or energy/wavelength dispersive X-ray fluorescence
spectroscopy (ED/WDXRFS). For the determination of the composition of tribofilms on different
test-pieces methods based on transmission or scanning electron microscopy (TEM/SEM), ultra
high vacuum tribometer (UHVT), Auger electron spectroscopy or scanning Auger microscopy
(AES/SAM), electron energy loss spectroscopy (EELS), X-ray or UV photoelectron
spectroscopy (XPS/UPS) are used."

http://www.vurup.sk/sites/vurup.sk/archi...2008_1_Sagi.pdf

http://www.slideshare.net/corematerials/chemical-analysis-in-the-electron-microscope

Like I have told you previously, knowing the elements in the oil is different than knowing their composition in the oil. Water has hydrogen and oxygen, but in what composition?


Do you even read the stuff you post? Like most of the "arguments" I see you get into, you don't seem grasp the core issue. In this case, you post a lab with a SEM as your evidence and when challenged - you don't even acknowledge that you were wrong. SEM does not have near enough resolution to resolve structure (in a vacuum mind you)of liquid organic molecules (in solution with other compounds, worse yet).

NOW you change the subject to TEM. Fine, but the first link is about XRF and AES. What does that have to do with EM? You basically just proved yourself wrong with your own link
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The second link is about crystalline structures and also proves that a TEM would be of limited use for mixed liquid organic molecules.

Sorry.
 
Originally Posted By: azsynthetic
For the determination of the composition of tribofilms on different
test-pieces methods based on transmission or scanning electron microscopy (TEM/SEM),


What part of this do you not understand? What part of electron microscopy using an electron microscope do you not understand?
 
Originally Posted By: volk06
[
Waters composition is well known. I don't understand why this example was used or what you meant by it.


I should have stated that a solution containing hydrogen and oxygen might or might not be water.
 
Originally Posted By: azsynthetic
Originally Posted By: azsynthetic
For the determination of the composition of tribofilms on different
test-pieces methods based on transmission or scanning electron microscopy (TEM/SEM),


What part of this do you not understand? What part of electron microscopy using an electron microscope do you not understand?


Please explain to us in detail what and how they are measuring in this case. You assume you get it, but some of us can see you clearly don't. Being flippant explains nothing, btw. Hint: they are not talking about base oil composition, which is the subject at hand, and even more precise a family of base oils, esters.
 
Neither SEM nor TEM will give you oil composition.

SEM and TEM can tell you if a film has been deposited on a surface. If you already know the composition of the oil, you may be able to make a good guess as to the nature of film based on its structure (amorphous, defined crystal shape, etc.) Neither SEM nor TEM alone can tell you the composition of the film. Crystal edges can sometime give you a lot of additional information.

@asxynthetic
Just accept that you have misunderstood something and try to figure out where you got lost.

@Pablo
I think that you know that you have requested an impossible task.

JAG's suggestion can give you a hint, but that strategy will also detect ketones, aldehydes, caboxyls, alcohols, ect.

The bottom line is there is not a shade-tree strategy to quantify ester base oil quantities.
 
Originally Posted By: Pablo

Please explain to us in detail what and how they are measuring in this case.


All you have to do is asked.

1. Obtain a base stock to be used in the test
2. Characterized the base oil using TLC method, IR and elemental analysis. Compare the results to OEM spec sheet if any.
3. Perform friction and wear test such as ASTM D-2783. Determine the wear scar and document as baseline. Also record the friction coefficient during the test.
4. Perform worn surface analysis. This usually done by X-ray photoelectrons spectroscopy (XPS)on the upper wear ball. A scanning electron microscope (SEM) and energy dispersive X-ray (EDX) are then used to study the rubbed surface morphology and the S, N elemental distributions in the worn steel surfaces. Document this as the baseline for the base oil.
5. Blend in the desire additives (This is where all the oil blenders such as Amsoil really do their things)
6. Repeat step 2 to 4 and document the results as the baseline for the end user products.

The XPS spectra were recorded to determine the chemical valence of the Fe, N, S and O elements on the worn surface with and without the additives. By comparing the binding energy of those elements a conclusion can be reached about the tribological reaction that has or has not occured between the lubricant and the metal surface during the friction process.

Without an electron microscope one would not know the adsorption of the decomposed lubricants and the structure of the elemental film that was formed. Amsoil does not do this for every batch of base oils that they buy.
 
Originally Posted By: GMorg
Neither SEM nor TEM will give you oil composition.

The bottom line is there is not a shade-tree strategy to quantify ester base oil quantities.


This is why I said all the blenders bought their base oils blind, yet Pablo think otherwise.

You might not know what the oil composition really is but at least you can tell if you are getting the same base oil as the last time.
 
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