WTC Dust Study Feb 29, 2012 by Dr. James Millette

[pgimeno]

I don't want to derail this thread any further. The full article about Marie-Paule Pileni is in this thread, we can continue there if you want: http://www.internationalskeptics.com/forums/showthread.php?t=141353

 

[Africanus]

fe -nope
al- nope
o- nope
c- maybe its a diamond!!!!!!
si- ? duh

Just provide the data for this assertion!

 

[gabeygoat]

and who are apparently too chicken**** to use their real names.

Is your name really "Ergo"?
Not that that would be bad. I actually kind of like it as a name. It could fit both a girl or a boy.

 

[Sunstealer]

got a question for ya. some people think that laclede is the primer paint that jones and crew tested. how do you think those silicon rich microspheres were formed when they did the dsc test? millette heated his to 400C and in the ash found kaolin plates. if one does think that jones' chips are laclede, how does the silicon from the kaolin form into silicon rich microspheres which appeared "transparent or translucent when viewed with white light" according to the bentham paper????

Silicon rich means nothing. Iron rich means nothing. The word rich is stupid because it does not describe quantity nor does it allude to any other element in the composition. It's so ambiguous as to be meaningless, which is why you truthers love to jump all over it with silly iron-rich quotes when you could just as easily say oxygen rich and be more correct. See figs 25-27 in Harrit et al.

How do you know the silicon was from kaolin? We already know that the samples tested in the DSC where not characterised. Oystein showed this. There is no correlation between what was tested in the DSC and samples a)-d). We also know calcium silicates were present in the Tnemec paint.

To answer your question.

Dehydroxylation is a reaction of decomposition of
kaolinite crystals to a partially disordered structure.

http://www.szte.mtesz.hu/06journal/2007_1/pdf/epa_2007_1_2.pdf

A disordered structure is a glass.

You also think that anything spherical must have been produced by a melting process. This is incorrect. In fact there are many papers that describe the manufacture of iron-oxide nano-sized round particles from non-spherical material way below the melting point of iron oxide for example.

Millette did low temperature ashing with the express purpose of NOT destroying the hexagonal platelet particles. He didn't want to destroy them because he wanted to analyse their crystal structure in order to characterise them. A far more sensible method than DSC.

I have an idea with regard to the Harrit et al DSC curves and the formation of the spheres produced.

FeOOH undergoes calcination and subsequent mass loss upto 270°C due to removal of water which could explain the rise to around 270°C. The exothermic peak is likely to be burning of epoxy or other organic material. There's also an endotherm that starts at 520°C for two of the curves which is potentially a phase change. Phase changes will easily account for spheroidisation of particles below the melting point of the material. Annealing of FeOOH and the transformation to Fe₂O₃ is a mechanism that will produce spheres at temperatures observed in the DSC. If you couple that with the fact that these spherical particles contain large proportions of Si/Al/Ca and sometimes Ti/S/K along with their respective sizes then there is no way that anyone can say that to produce spheres you need temperatures of 1500°C plus.

You do not need to melt a sample to produce spheres.

If you look up powder metallurgy you can see that you can form nearly fully dense metals from powder without melting using a sintering process with temperatures well below the melting point of the material.

If the sample had experienced 1500°C then there wouldn't be any sample left. We can clearly see from the Harrit et al paper that large proportions of the red layer remain even after reaching 700°C. (but the gray layer doesn't) Not very efficient thermite if not all of it reacts at the claimed 430°C is it?

 

[Sunstealer]

fe -nope
al- nope
o- nope
c- maybe its a diamond!!!!!!
si- ? duh

Stop being so childish. It's pathetic and makes you look stupid.

4. Observation of Iron-Rich Sphere Formation Upon
Ignition of Chips in a Differential Scanning Calorimeter

In the post-DSC residue, charred-porous material and
numerous microspheres and spheroids were observed. Many
of these were analyzed, and it was found that some were
iron-rich, which appear shiny and silvery in the optical microscope,
and some were silicon-rich, which appear transparent or translucent when viewed with white light; see photographs
taken using a Nikon microscope (Fig. 20).

Again - silicon rich. It means nothing. So where is the analysis? Where are the figures for the composition of these translucent spheres? Oh that's right there isn't one.

So Africanus was correct and you were wrong - wrong as usual. Grow up.

 

[Oystein]

... We also know calcium silicates were present in the Tnemec paint ...

We also know silica proper (diatomaceous as well as amorphous) was present in Tnemec paint. Silica and silicates are both quite common in paints, so Tnemec is not the only candidate, just the only one we know of. It is a total certainty that many more red paints were present in the towers.

 

[Ivan Kminek]

FTIR spectra in Appendix C, Millette's report

Thank you, Sunstealer Still, only experiments could convince any truther.

And now for something completely different, (to Chris and especially to JREFres who undestand IR spectroscopy):

Poseidon pointed in Oystein's blog, that in epoxy resins cured with amines, no IR band of carbonyl groups (at ca 1670 to 1680 cm^-1 should be present. He is right and it represents some problem for us, Laclede primer proponents, who claim that Bentham chips (a) to (d) are Laclede primer particles. The problem is that in both epoxy coating used in comparison and red chips in Millette's Appendix C, some bands corresponding to carbonyl groups are apparent (at wavenumbers ca 1706-1731 cm ^-1. And, Laclede primer was cured with some amines. Is there any explanation?

Let me repost my answer to Poseidon:

"Poseidon: you noted above that FTIR spectrum DGEBA-based epoxy resin cured with amine/polyamine should not contain band corresponding to carbonyl at ca 1670-1760 cm-1. You are right, in this range no other characteristic bands should appear (perhaps with the exception of weak/broad band “overtones”). Thanks again.

Since Jim Millette’s spectrum of epoxy coating shows a strong band at 1731 cm-1, this should be basically some epoxy cured with e.g. anhydride or other curing agent containing carbonyl groups (or leading to the formation of that groups).

I have just found this fine paper http://www.sciencedirect.com/science/article/pii/S0141391005004234 dealing with DGEBA-based epoxies cured with both amine and anhydride. As you can see in Fig. 1, FTIR spectra of freshly cured samples are very similar and they basically differ only in the carbonyl band (appearing at 1740 cm-1) for “anhydride epoxy”.
Otherwise, they both contain distinct bands (among others) at ca 1605, 1510, 1460, (ca 1350) 1250 and 1190 cm-1. I’m not qualified to decide if the spectra of Jim Millette indicate clearly epoxy resin, but let me consider just carbonyl bands again.

The mentioned paper studied thermal and photochemical aging of epoxy samples and in “amine-epoxy”, the carbonyl band is developed during aging. This is quite expected, since carbonyl compounds are normal products of polymer oxidation.

From this point of view, I would suggest the following hypothesis:

Epoxy coating measured by Jim Millette can be DGEBA epoxy resin cured with anhydride or other curing agent containing/leading to the formation of carbonyl groups."

Red-gray chips measured by Jim Millette can be strongly oxidized chips of epoxy resin in Laclede primer (cured with amines). Anyway, no wonder that they can be strongly oxidized after more than 40 years)


Well, in this way, carbonyl bands in red chips in Appendix C can be explained, even if they are Laclede primer.

Still, I would have some questions to Jim Millette (if you read it, Chris):

- Is a formulation (especially curing agent) of epoxy coating in Appendix C known?
- In which way Jim Millette identified epoxy in red chips? Using just this comparison of FTIR spectra, or using some additional info from some FTIR database?

 

[Oystein]

...
Poseidon pointed in Oystein's blog, that in epoxy resins cured with amines, no IR band of carbonyl groups (at ca 1670 to 1680 cm^-1 should be present. ...

Thanks to you, Ivan, for engaging Poseidon on the FTIR issue in my blog, and for being open and honest about the possible problems for our theory that he raises.
I will respond to the XEDS arguments he has posted in recent days. Basically, I want to settle with admitting that Fig 17, which shows Al in abundance, has no definitive explanation within the framework of a "Tnemec" hypothesis for the MEK-chip; but that thermite is also not a valid explanation, because the chip as a whole contains much too little Al (Fig 14). I see four possibilities for the apparent presence of elemental Al in some undefined little spot of the MEK-chip in Fig 17:

1. Measurement error (incompetent handling of probe, wrong device parameters...))
2. Contamination of chip with actual Al from different source
3. Signal is picked up from sample holder (remember the apparent concentration of Al only at the steep edge of the chip, adjacent to an area where indeed Al-signal is shown outside of the chip, coming most likely from the sample holder))
4. That spectrum is not from that chip (mix-up or fraud)

Still, I would have some questions to Jim Millette (if you read it, Chris):

- Is a formulation (especially curing agent) of epoxy coating in Appendix C known?
- In which way Jim Millette identified epoxy in red chips? Using just this comparison of FTIR spectra, or using some additional info from some FTIR database?

About the second question "(how did) Jim Millette identified epoxy in red chips?" I'd propose that his equipment has software that does the matching with database. If so, I propose that such software not only provides the best match, but also provides some numerical/statistical measure of how good the match is. If this is so, details and a bit of explanation would be great (such as: "software identified epoxy plus kaolin with 94% confidence, second best match is X+Ywith 37% confidence" or "correlation coefficient from method Z is 0.71, generally a value above 0.50 is considered probable, above 0.6 good, above 0.75 definitive").

 

[chrismohr]

I just copied off Ivan and Oystein's posts to Jim. Jim was out of town most of last week so we haven't been in contact for awhile.

 

[chrismohr]

Sunstealer,

You wrote, "You also think that anything spherical must have been produced by a melting process. This is incorrect. In fact there are many papers that describe the manufacture of iron-oxide nano-sized round particles from non-spherical material way below the melting point of iron oxide for example."

I think you've linked us to these papers before, but can you give me a couple links to some good papers that show nano-particles of iron oxide being created at sub-melting temps? I want to post these on our Gage debate website. Richard Gage just told me personally last Friday that nano-sized iron oxide particles in the red-grey chips are strong evidence for thermite and very high temperatures.

 

[Oystein]

@ Chris Mohr:

Please forward the following to Jim:


In the Progress Report, under "Notes on the Source of the Red/Gray Chips", Jim writes, refering to [16] (a product sheet for Tnemec 69 and 99 column paints):

"small EDS peaks of zinc and chromium were detected in some samples but the amount detected was inconsistent with the 20% level of zinc chromate in the primer formula"​

This "20% level in the primer formula" is not quite correct. According to the product sheet for Tnemec 69 and 99, zinc chromate is about 20% of the primer pigment. The formulation, as tabulated by Sramek, has four pigments, which add up to 100%, and 7 ingredients of the vehicle, which also add up to 100%. However, the pigments are only a certian proportion of the dry paint. Assuming that pigments are about 30% by weight of the dry paint (for comparison, the LaClede formula has 28.5% pigment), then zinc chomate is not 20%, but only about 6% of the "primer formula". By elemental composition then, zinc would be 2.4% by weight and chromium 1.9%.

(The Zn-peak in graphs like 9119-4795L1560-red(2) would still tend to be a little low, and there is always too little Cr, except in 9119-5230M3451B-red-gray(9), which however appears anomalous, with a very low C-peak. So I am not sure if any chip can reliably be identified as Tnemec 69/99, even if a lower Zn/Cr content is taken into account).

 

[Miragememories]

"... Iron rich means nothing. The word rich is stupid because it does not describe quantity nor does it allude to any other element in the composition. It's so ambiguous as to be meaningless, which is why you truthers love to jump all over it with silly iron-rich quotes when you could just as easily say oxygen rich and be more correct ..."

So if I am to understand your reasoning correctly, the word rich fails because it is too imprecise?

And that with that reasoning, iron poor would be understood as meaningless, stupid, needing quantification, incomplete, and ambiguous beyond meaningless?

Iron-rich conveys significant meaning.

The conditions necessary to form those high-purity iron microspheres, requires temperatures high enough to melt iron.

MM

 

[Oystein]

So if I am to understand your reasoning correctly, the word rich fails because it is too imprecise?

Yes. If you disagree, perhaps you could give us some quantitative idea of how precise that term is?

And that with that reasoning, iron poor would be understood as meaningless, stupid, needing quantification, incomplete, and ambiguous beyond meaningless?

Would be, yes, if anybody used the term. Does anybody? Where?

Iron-rich conveys significant meaning.

Care to explain what that meaning is?

The conditions necessary to form those high-purity iron microspheres,

Can you point out which "high-purity iron microspheres" you are talking about? Can't find any in the Harrit-paper.

requires temperatures high enough to melt iron.

No.

 

[Dave Rogers]

Iron-rich conveys significant meaning.

The problem with "Iron-rich" is that it conveys vague and imprecise meaning. In particular, it fools the gullible into believing that the microspheres in question are not some unknown mixture of chemical compounds which includes some or all which contain iron as a constituent, but rather that they are iron spheres containing some level of impurity...

The conditions necessary to form those high-purity iron microspheres...

...or, on occasion, the extremely gullible will jump to an even more bizarre conclusion.

Dave

 

[Senenmut]

Silicon rich means nothing. Iron rich means nothing. The word rich is stupid because it does not describe quantity nor does it allude to any other element in the composition. It's so ambiguous as to be meaningless, which is why you truthers love to jump all over it with silly iron-rich quotes when you could just as easily say oxygen rich and be more correct. See figs 25-27 in Harrit et al.

iron rich means iron rich and it does mean someting. for example when jones spoke with greening concerning the iron microspheres:
"Dr. Farrer and Danny and I have looked at many of these post-DSC spheres, many do NOT contain Al. See for example Fig 21 in our paper....."

"Look again at the data (fig 21) -- there is no Al in evidence. Furthermore, the amounts of Si and Ca and especially S here is trivial. The melting points of iron and of iron oxide are both above 1200 C, yet the DSC reached only 700 C, insufficient to cause melting of iron or iron oxide."

How do you know the silicon was from kaolin? We already know that the samples tested in the DSC where not characterised. Oystein showed this. There is no correlation between what was tested in the DSC and samples a)-d). We also know calcium silicates were present in the Tnemec paint.

i dont know that. as you and i and everyone knows, the chips vary from chip to chip and from site to site on the chips.you and oystein can say whatever you want but the point is they jones chips reacted around 430C and procuced iron and silicon rich microspheres. has he ever done a dsc and came up with NO iron and silicon microspheres???? i cant answer that question. jones chips might contain a silicon matrix whereas millettes contain kaolin. some belive jones chips are laclede, then those silicon rich spheres must have come from kaolin.

A disordered structure is a glass.

this sure looks like spheres and glass to me:

You also think that anything spherical must have been produced by a melting process. This is incorrect. In fact there are many papers that describe the manufacture of iron-oxide nano-sized round particles from non-spherical material way below the melting point of iron oxide for example.

yeah, did millette find any at 400C. i know jones went up to 700C.
now do you think the kaolin plates that were around 40nm by 1 micron reacted to produce transparent and translucent microspheres that look to be around 10 microns? do the plates come together when they turn to metakaolin or would the plates independantly turn to metakaolin?
from the bentham paper: the line represents 50 microns. the microspheres in question are the ones at the bottom right.
[/url]

Millette did low temperature ashing with the express purpose of NOT destroying the hexagonal platelet particles. He didn't want to destroy them because he wanted to analyse their crystal structure in order to characterise them. A far more sensible method than DSC.

sure..

I have an idea with regard to the Harrit et al DSC curves and the formation of the spheres produced.

FeOOH undergoes calcination and subsequent mass loss upto 270°C due to removal of water which could explain the rise to around 270°C. The exothermic peak is likely to be burning of epoxy or other organic material. There's also an endotherm that starts at 520°C for two of the curves which is potentially a phase change. Phase changes will easily account for spheroidisation of particles below the melting point of the material. Annealing of FeOOH and the transformation to Fe₂O₃ is a mechanism that will produce spheres at temperatures observed in the DSC. If you couple that with the fact that these spherical particles contain large proportions of Si/Al/Ca and sometimes Ti/S/K along with their respective sizes then there is no way that anyone can say that to produce spheres you need temperatures of 1500°C plus.

im confused? are you saying the chips contain feooh particles before reacting? oystein says they are hematite. fe2o3 not feooh? again note jones' email to greening above and see fig 21 in the bentam paper when you speak about the spheres contain large proportions of si/al/ca and sometimes ti/s/k.

You do not need to melt a sample to produce spheres.

If you look up powder metallurgy you can see that you can form nearly fully dense metals from powder without melting using a sintering process with temperatures well below the melting point of the material.

If the sample had experienced 1500°C then there wouldn't be any sample left. We can clearly see from the Harrit et al paper that large proportions of the red layer remain even after reaching 700°C. (but the gray layer doesn't) Not very efficient thermite if not all of it reacts at the claimed 430°C is it?

the dsc is NOTHING like the sintering process.....

 

[Senenmut]

Stop being so childish. It's pathetic and makes you look stupid.

Again - silicon rich. It means nothing. So where is the analysis? Where are the figures for the composition of these translucent spheres? Oh that's right there isn't one.

So Africanus was correct and you were wrong - wrong as usual. Grow up.

what is the makeup of those chips.... predominately iron, carbon, aluminum, oxygen, and silicon. so what is the most likely candidtate for a translucent or transparent microsphere. you dont have to think too scientifically here. silicon rich does mean something. it means its silicon rich. your right, i would like to see a fig for the compostion of these spheres. jones thinks his chips contain a silicon matrix whereas millete's matrix is carbon and oxygen and is an epoxy resin. im not wrong, i just ruled out the obvious....

 

[Sunstealer]

So if I am to understand your reasoning correctly, the word rich fails because it is too imprecise?

And that with that reasoning, iron poor would be understood as meaningless, stupid, needing quantification, incomplete, and ambiguous beyond meaningless?

Iron-rich conveys significant meaning.

Here are some Oxygen rich spheres!

Do you now see why calling these spheres "iron-rich" is misleading? Why iron rich and not oxygen rich? Hell you could even claim they are silicon rich with validity.

The conditions necessary to form those high-purity iron microspheres, requires temperatures high enough to melt iron.

MM

Source? Citation? And no don't bother with any truther crap I want a proper source that says only melting causes spherical particles to form preferably from a scientific paper.

 

[Sunstealer]

what is the makeup of those chips.... predominately iron, carbon, aluminum, oxygen, and silicon. so what is the most likely candidtate for a translucent or transparent microsphere. you dont have to think too scientifically here. silicon rich does mean something. it means its silicon rich.

Which means what? 43% Silicon? 90% Bearing in mind how truthers wrongly refer to iron-rich spheres as I have proven using Harrit's own data (see above post) then claiming Silicon rich for another unknown particle with no data is silly.

Yes such a transparent particle is likely to contain silica but you've moved the goalposts because you know that Oystein has shown that no truther can show where that silicon comes from because no one including Farrer knew what material was tested in the DSC.

your right, i would like to see a fig for the compostion of these spheres. jones thinks his chips contain a silicon matrix whereas millete's matrix is carbon and oxygen and is an epoxy resin. im not wrong, i just ruled out the obvious....

No he doesn't...

It is also shown that within the red layer there is an intimate mixing of the Fe-rich grains and Al/Si plate-like particles and that these particles
are embedded in a carbon-rich matrix.

Page 15

We make no attempt to specify the particular form of nano-thermite present
until more is learned about the red material and especially about the nature of the organic material it contains.

Page 25.

...unless he's going against the paper he continually refers to.

Why do you spout such nonsense? Why don't you actually read Harrit et al before claiming such easily refuted rubbish. You look sloppy.

So yes Millette's findings correspond with the data in the Harrit et al paper and the authors of that paper state the material is organic.

Instead of posting nonsense here why don't you ask the paper's authors why they didn't characterize the organic material? Why don't they release the FTIR data which would characterize this material.

 

[Sunstealer]

iron rich means iron rich and it does mean someting. for example when jones spoke with greening concerning the iron microspheres:
"Dr. Farrer and Danny and I have looked at many of these post-DSC spheres, many do NOT contain Al. See for example Fig 21 in our paper....."

"Look again at the data (fig 21) -- there is no Al in evidence. Furthermore, the amounts of Si and Ca and especially S here is trivial. The melting points of iron and of iron oxide are both above 1200 C, yet the DSC reached only 700 C, insufficient to cause melting of iron or iron oxide."



i dont know that. as you and i and everyone knows, the chips vary from chip to chip and from site to site on the chips.you and oystein can say whatever you want but the point is they jones chips reacted around 430C and procuced iron and silicon rich microspheres. has he ever done a dsc and came up with NO iron and silicon microspheres???? i cant answer that question. jones chips might contain a silicon matrix whereas millettes contain kaolin. some belive jones chips are laclede, then those silicon rich spheres must have come from kaolin.



this sure looks like spheres and glass to me:
[qimg]http://www.internationalskeptics.com/forums/imagehosting/thum_285444fccc98889ee0.jpg[/qimg]


yeah, did millette find any at 400C. i know jones went up to 700C.
now do you think the kaolin plates that were around 40nm by 1 micron reacted to produce transparent and translucent microspheres that look to be around 10 microns? do the plates come together when they turn to metakaolin or would the plates independantly turn to metakaolin?
from the bentham paper: the line represents 50 microns. the microspheres in question are the ones at the bottom right.
[/url][qimg]http://www.internationalskeptics.com/forums/imagehosting/thum_285444fcccc08a5e9d.jpg[/qimg]

sure..



im confused? are you saying the chips contain feooh particles before reacting? oystein says they are hematite. fe2o3 not feooh? again note jones' email to greening above and see fig 21 in the bentam paper when you speak about the spheres contain large proportions of si/al/ca and sometimes ti/s/k.



the dsc is NOTHING like the sintering process.....

I'm not even going to bother with this nonsense. You are all over the place. Your contradicting yourself in the same post regarding Millette's ashing at 400°C. Write coherent sentences.

 

[Senenmut]

Which means what? 43% Silicon? 90% Bearing in mind how truthers wrongly refer to iron-rich spheres as I have proven using Harrit's own data (see above post) then claiming Silicon rich for another unknown particle with no data is silly.

Yes such a transparent particle is likely to contain silica but you've moved the goalposts because you know that Oystein has shown that no truther can show where that silicon comes from because no one including Farrer knew what material was tested in the DSC.

you know exactly what was tested with small variation from chip to chip and from location to location on those chips. your just saying that to get out from trying to explain how kaolin transformed into those silicon rich microspheres if you believe it is laclede primer.

No he doesn't...

from the bentham paper:

"Further, we have shown that the red material contains
both elemental aluminum and iron oxide, the ingredients of
thermite, in interesting configuration and intimate mixing in
the surviving chips (see Results, section 1). The species are
small (e.g., the iron oxide grains are roughly 100 nm across)
in a matrix including silicon and carbon, suggesting a superthermite
composite."

ok so carbon and silicon.......my bad, i didnt mean just silicon...sorry.

So yes Millette's findings correspond with the data in the Harrit et al paper and the authors of that paper state the material is organic.

jones is silicon with carbon and millette's is epoxy.

Instead of posting nonsense here why don't you ask the paper's authors why they didn't characterize the organic material? Why don't they release the FTIR data which would characterize this material.

that would be nice. what non sense are you referring too?