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

[Senenmut]

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.

of coarse your not. with regards to millette's ashing, a "skeptic" posted a link speaking about melting of nanoparticles at low temps. well, at 400c, there was no microspheres formed from his fe2o3 particles. no contradiciton, just science from millette's study.

 

[Senenmut]

found the quote and link:
post 546
"For example, the melting temperature of iron particles in the range of a few nanometers lies approximately between 200~400°C compared to 1538°C for bulk iron."

http://www.ifm.eng.cam.ac.uk/pp/projects/laserprintforming.html

thats why i brought up millette's ashing and the lack of iron microspere formation.

 

[Oystein]

...
as you and i and everyone knows, the chips vary from chip to chip and from site to site on the chips.

Exactly. So be careful, and don't lump them all together. Some chips contain kaolin, others don't. Some contain silica, others don't. Some contain titanium oxide, some don't. Some contain zinc chromate, others don't. Some contain calcium silicate, others don't. Some contain epoxies, some may not. Some may even contain aluminium or alumina (but neither has been shown by anyone at all), but most do not.

It is obvious that different types of chip will behave differently in different tests. If chip X shows behaviour x, you can't assume that chip Y would show the same behaviour, unless you first show that X and Y have the same composition.

Do you comprehend that, Senemut?

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.

Senemut: Which of the at least six different kinds of chips reacted at 430°C? And which produced iron-rich microspheres? And which produced silicon-rich (glassy) microspheres?
(Answer: no one knows)

has he ever done a dsc and came up with NO iron and silicon microspheres????

What would you conclude if a Millette chip did produce this or that kind of spheres?
What would you conclude if a Millette chip did NOT produce this or that kind of spheres?

i cant answer that question. jones chips might contain a silicon matrix whereas millettes contain kaolin.

Nothing in Jones's data points to a silicon "matrix".
Everything in Jones's data on chips (a)-(d) points to kaolin in an organic matrix.

some belive jones chips are laclede, then those silicon rich spheres must have come from kaolin.

No.
Some believe that one of the at least six different kinds of red-gray chips are LaClede, and the other at least 5 are NOT LaClede.
It follows then that no one believes that silicon rich spheres must have come from kaolin when Jones e.al. heated some UNKNOWN kind of chip, because at least 5 of the different kinds of chips may not contain kaolin.

im confused? are you saying the chips contain feooh particles before reacting? oystein says they are hematite. fe2o3 not feooh?

Yes, you are confused.

Oystein says that the red matrix contains red hematite pigments, i.e. grains Fe2O3 that are about 100 nm small. Run-of-the-mill cheap red pignents.

Sunstealer says the chips contain FeO(OH) - but not as nano-sized pigments in the red matrix. Rather, such phases are normal constituents of mill-scale - i.e. the gray layer, wich is corroded steel surface.

There is no conflict between his and my claims.

You are just confused.

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.

Earlier, you spole about "high-purity iron".
Does Fig 21, or any other Jones data, show such a thing?

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

Not? Why not? Please explain! (this shall be funny )

 

[Oystein]

you know exactly what was tested with small variation from chip to chip

You know this how? Where does "small" begin and end?

We know from the Harrit paper that they had at least six differend kinds of chips in their dust bags.
Only for two of these do they produce pre-ignition compositions: Chips (a)-(d), and the MEK-chip. I have shown in my blog that the difference between these two kinds are vast - 2/3 of the XEDS signal for the MEK-chip would have to get removed to make it look similar to chips (a)-(d). That variariation is not small, it is proof that we are dealing with two entirely different compositions, and that "contamination" is not an acceptable explanation.
As for the at least 4 other kinds of chips, we have no information at all to asses whether or not the variations are "small".

So how on earth do you know there was only "small variation from chip to chip"??

...if you believe it is laclede primer.

Sorry to rub this in, but:
We do NOT "believe" "it" is LaClede primer, with "it" being the substance from which any of the post-DSC spheres that they show were produced.
Rather, we KNOW that there were at least 5 different kinds of red-gray chips that were NOT LaClede primer, and no one knows which kind or kinds they DSCed. It follows that it is impossible to guess which base material gave rise to which spheres, and that LaClede / kaolin may very well not have been "it".

Do you understand by now that the variation between the chips is significant, because we know of only one that it did contain kaolin, but of five that may not have contained kaolin (one which we are pretty sure does not contain kaolin)?

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."

They have not in fact shown any of this, least of all a matrix including Si.
They have not shown that all of the chips contain elemental Al, however they HAVE shown that chips a-d contain NO free Al.

 

[Oystein]

found the quote and link:
post 546
"For example, the melting temperature of iron particles in the range of a few nanometers lies approximately between 200~400°C compared to 1538°C for bulk iron."

http://www.ifm.eng.cam.ac.uk/pp/projects/laserprintforming.html

thats why i brought up millette's ashing and the lack of iron microspere formation.

For the record: Some posters here think that melting point depression plays a significant role in our context, but I do not.

Melting point depression is significant only at particle sizes well below 100 nm, which is the smallest we see in Harrit e.al.'s samples.

I think Sunstealer's phase transitions within the gray layers are a better candidate especially since many of the spheric blobs that Harrit e.al. show appear to have originated from the gray layer, not the red layer; the gray layer is many microns thick, so melting point depression can't play a role.

 

[chrismohr]

For the record: Some posters here think that melting point depression plays a significant role in our context, but I do not.

Melting point depression is significant only at particle sizes well below 100 nm, which is the smallest we see in Harrit e.al.'s samples.

I think Sunstealer's phase transitions within the gray layers are a better candidate especially since many of the spheric blobs that Harrit e.al. show appear to have originated from the gray layer, not the red layer; the gray layer is many microns thick, so melting point depression can't play a role.

Oystein,
Last Friday Richard Gage told me personally that some of the iron-rich spheres found in the Bentham paper were only about 100 atoms across. Is this true? That would be ultra-nano if it were! He thinks Millette may not have looked at this closely enough.

 

[Senenmut]

Exactly. So be careful, and don't lump them all together. Some chips contain kaolin, others don't. Some contain silica, others don't. Some contain titanium oxide, some don't. Some contain zinc chromate, others don't. Some contain calcium silicate, others don't. Some contain epoxies, some may not. Some may even contain aluminium or alumina (but neither has been shown by anyone at all), but most do not.

i see that jones and crew has one type that varies from chip to chip and henryco and millette have another. remember henryco heated his to 900c i believe and no microspheres formed. so i still have my money for chris when he is ready for it concerning a dsc test of millette's chips.

It is obvious that different types of chip will behave differently in different tests. If chip X shows behaviour x, you can't assume that chip Y would show the same behaviour, unless you first show that X and Y have the same composition.

Do you comprehend that, Senemut?

that is soooo true. millette and jones' chips show similar sem and edx but will millttes react at around 430C and produce the iron and silicon rich microspheres!!

Senemut: Which of the at least six different kinds of chips reacted at 430°C? And which produced iron-rich microspheres? And which produced silicon-rich (glassy) microspheres?
(Answer: no one knows)

the chips that vary from chip to chip and spot to spot on the same chip that jones and crew have.

What would you conclude if a Millette chip did produce this or that kind of spheres?

if it took place in a dsc and it reacted around 430C and produced a similar spike and had similar edx data for the microspheres then i would conclude that that particular chip millette tested is similar if not equal to jones' chip makeup.

What would you conclude if a Millette chip did NOT produce this or that kind of spheres?

i think u know the answer to that.

Nothing in Jones's data points to a silicon "matrix".
Everything in Jones's data on chips (a)-(d) points to kaolin in an organic matrix.

ok, so you say. Jones says it does:
"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."

Some believe that one of the at least six different kinds of red-gray chips are LaClede, and the other at least 5 are NOT LaClede.
It follows then that no one believes that silicon rich spheres must have come from kaolin when Jones e.al. heated some UNKNOWN kind of chip, because at least 5 of the different kinds of chips may not contain kaolin.

it was not an unknown kind of chip. we know what it consisted of. you say we dont know, the bentham paper says they do know.

Oystein says that the red matrix contains red hematite pigments, i.e. grains Fe2O3 that are about 100 nm small. Run-of-the-mill cheap red pignents.

Sunstealer says the chips contain FeO(OH) - but not as nano-sized pigments in the red matrix. Rather, such phases are normal constituents of mill-scale - i.e. the gray layer, wich is corroded steel surface.

There is no conflict between his and my claims.

he never mention that he was speaking of the gray layer. so what percentage of that corroded steel would contain feooh? sounds like a BIG strech to me!

You are just confused.

i dont think so, i believe you are!

Earlier, you spole about "high-purity iron".
Does Fig 21, or any other Jones data, show such a thing?


Not? Why not? Please explain! (this shall be funny )

look at the edx fig 21. if you dont think it is, why not?

 

[Sunstealer]

of coarse your not. with regards to millette's ashing, a "skeptic" posted a link speaking about melting of nanoparticles at low temps. well, at 400c, there was no microspheres formed from his fe2o3 particles. no contradiciton, just science from millette's study.

Stop wibbling. Learn to write coherent sentences. You've been told why Millette used 400°C. He did not want to destroy the crystals. He simply wanted to remove the epoxy and separate the particles for further analysis. If you had read his report you would know this because he states it:

Low-temperature ashing (LTA) is an alternative to using solvents to extract inorganic constituents from an organic film or coating.⁶ LTA of the chips of interest was done using an SPI Plasma Prep II plasma asher. LTA was performed for time periods of 30 minutes to 1 hour depending on the size of the chip. The gray layer remained intact and the red layer residue was collected in clean water and drops of the suspension were placed on carbon-film TEM grids. After drying, the particulate was analyzed using a Philips CM120 TEM capable of SAED and equipped with an Oxford EDS system.

400°C over 30-60 mins is too lower temperature over too shorter time to produce spheres.

Again - far better not to destroy the sample and actually analyse what is there than do DSC which tells you nothing anyway.

You can cling to the DSC test and the spheres all you want, it still doesn't mean thermite is present.

 

[Oystein]

i see that jones and crew has one type that varies from chip to chip

Where do you see that?

...
if it took place in a dsc and it reacted around 430C and produced a similar spike and had similar edx data for the microspheres then i would conclude that that particular chip millette tested is similar if not equal to jones' chip makeup.

See, that would be an invalid conclusion.

i think u know the answer to that.

Tell me anyway

it was not an unknown kind of chip. we know what it consisted of. you say we dont know, the bentham paper says they do know.

Ok. Then quote the Bentham paper and tell us what the DSCed chips consisted of

 

[Sunstealer]

found the quote and link:
post 546
"For example, the melting temperature of iron particles in the range of a few nanometers lies approximately between 200~400°C compared to 1538°C for bulk iron."

http://www.ifm.eng.cam.ac.uk/pp/projects/laserprintforming.html

thats why i brought up millette's ashing and the lack of iron microspere formation.

A few nanometers now equals 100nm (for the rhombohedral Fe2O3 in the red layer) and 10 to 50 microns or 10000 to 50000nm (for the gray layer.)

So lets say a few equals 20, then at minimum you are out by a factor of 5 and at worst 2500.

Based on the optical and electron microscopy data, the Fe/O particles are an iron oxide pigment consisting of crystalline grains in the 100-200 nm range and the Al/Si particles are kaolin clay plates that are less than a micrometer thick.

The gray layers were in the range of 10 to 50 micrometers thick (Appendix B).

From Millette.

You obviously have no concept of the scales in the Harrit paper and Millette's progress report. Secondly the reason why papers have been quoted showing lower than bulk melting temperatures for nano-scale materials is to show truthers that they are incorrect when they state bulk material properties for materials on the nano-scale.

 

[Sunstealer]

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.


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.

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


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

No it's not a silicon matrix because silicon is not observed in the matrix material.

The XEDS maps, several of which are shown in Fig. (10b-f),
indicate by color, the degree to which the particular element
is present at or near the surface from point to point across the
area. The results indicate that the smaller particles with very
bright BSE intensity are associated with the regions of high
Fe and O. The plate-like particles with intermediate BSE intensity appear to be associated with the regions of high Al and Si. The O map (d) also indicates oxygen present, to a
lesser degree, in the location of the Al and Si. However, it is
inconclusive from these data whether the O is associated
with Si or Al or both. The carbon map appears less definitive, that is, it does not appear to be associated with a particular particle or group of particles, but rather with the matrix material.

Fig 10 shows this and it's self evident.

There is no silicon matrix if matrix is used in the correct way. You can tell that the report was written by many people due to such inconsistencies. These would have been picked up had the paper gone through a proper and rigorous peer review.

 

[Sunstealer]

Yes, you are confused.

Oystein says that the red matrix contains red hematite pigments, i.e. grains Fe2O3 that are about 100 nm small. Run-of-the-mill cheap red pignents.

Sunstealer says the chips contain FeO(OH) - but not as nano-sized pigments in the red matrix. Rather, such phases are normal constituents of mill-scale - i.e. the gray layer, wich is corroded steel surface.

There is no conflict between his and my claims.

You are just confused.

Exactly. The gray layer is consistent with rust from a low carbon steel. Rust contains different iron oxides. Some of these iron oxides exhibit different crystal structures/phases.

http://en.wikipedia.org/wiki/Iron_oxide

FeOOH is one of them. The reason I'm looking at the iron oxides is because the gray layer disappears post DSC and small metallic looking spheres are formed. It therefore makes sense that the gray layer forms the majority of the constituents of these spheres. It therefore makes sense to look at phase transformations and other reactions involving potential oxides that make up the gray layer.

Infact in the DSC there are endothermic troughs above 550°C. That's a potential phase change or localised melting occurring.

 

[Oystein]

Oystein,
Last Friday Richard Gage told me personally that some of the iron-rich spheres found in the Bentham paper were only about 100 atoms across. Is this true? That would be ultra-nano if it were! He thinks Millette may not have looked at this closely enough.

Let's see...

Iron oxide, Fe₂O₃, has a density of about 5.2 g/cm³ and a molar mass of 159.7 g/mol. So one mol occupies a volume of (159.7/5.2) cm³ = 30.7 cm³ = 3.7*10^-5 m³. The edges of cube of that volume are 0.031 m long (3.1 cm), that is 310,000,000 nm.

1 mole is about 6.0 ×10²³. The cubic root of that number, 84,343,266, would be the number of molecules along the edge if you arrange 1 mole in a cube.

So if iron oxide molecules were in a cubic crystal structure, you'd find 84,343,266 molecules per 31,000,000 nm, or 0.37 nm per molecule, or 37 nm per 100 molecules.

The iron oxide pigments in the red paint are typically 100-150 nm across, that would be 270-405 molecules.

This would be somehat different for different materials, but I think we get an idea here of the orders of magnitude that we are talking about.
Iron: 23 nm / 100 atoms.
Silica: 34 nm / 100 atoms
etc.

So Gage is claiming that there are microspheres in the Bentham paper that are about 20-40 nm across? Let me check...

Nope, I see none post-ignition spheres smaller than 1 micron, all are larger than 1,000 nm, or more than 2500 atoms/molecules across.

However, as I said, the iron oxide pigments are close to that order of magnitude, they are only a few 100 molecules across. Perhaps he (or you?) mixed up pre-ignition grains and post-ignition spheres?

100 nm iron oxide pigments have been state of the art for 100 years and are easily and cheaply produced on large industrial scales by entirely conventional means: Chemical reaction, grinding and sieving, and are thus found in millions of mundane products.

 

[Senenmut]

Where do you see that?

as far as i know, his red gray chips react around 430C. i dont think that he has ever stated that he tested a chip that didnt react.

See, that would be an invalid conclusion.

or the right conclusion.

Ok. Then quote the Bentham paper and tell us what the DSCed chips consisted of

"...indicate that the gray layers are consistently characterized
by high iron and oxygen content including a smaller amount
of carbon. The chemical signatures found in the red layers
are also quite consistent (Fig. 7), each showing the presence
of aluminum (Al), silicon (Si), iron (Fe) and oxygen (O), and
a significant carbon (C) peak as well"

i know your response will be blah..blah...blah..blah

 

[Senenmut]

A few nanometers now equals 100nm (for the rhombohedral Fe2O3 in the red layer) and 10 to 50 microns or 10000 to 50000nm (for the gray layer.)

So lets say a few equals 20, then at minimum you are out by a factor of 5 and at worst 2500.





From Millette.

You obviously have no concept of the scales in the Harrit paper and Millette's progress report. Secondly the reason why papers have been quoted showing lower than bulk melting temperatures for nano-scale materials is to show truthers that they are incorrect when they state bulk material properties for materials on the nano-scale.

you played the melting point depression angle for awile (yr or so ago). i remember getting a link awhile back from you when speaking about iron microspheres. i know the scales.

 

[Senenmut]

No it's not a silicon matrix because silicon is not observed in the matrix material.

Fig 10 shows this and it's self evident.

There is no silicon matrix if matrix is used in the correct way. You can tell that the report was written by many people due to such inconsistencies. These would have been picked up had the paper gone through a proper and rigorous peer review.

think what you want too.

it is interesting when mark basile talks of the matrix in this vid:
http://www.youtube.com/watch?v=h1VmaCl4HwU

at 3950 he speaks of a matrix with silica and then at 46 30 (post reaction), he speaks about a silicate material shell that was left over from the original matrix. he speaks about a silicate material all coated inside with "iron films"......interesting stuff.

 

[Oystein]

as far as i know, his red gray chips react around 430C. i dont think that he has ever stated that he tested a chip that didnt react.

This does not mean that the chips were significantly different from each other.

Since it clearly was the organic matrix that ignited arounf 400°C, and since many different organic matrixed will ignite in thar area, and since most the minerals will not burn at all, any of the following might show these general characteristic of reacting around 430°C:
- Oil paint with organic pigments
- Epoxy paint with iron oxide, kaolin and strontium chromate
- Epoxy and linseed oil based paint with silica, talc, iron oxide, calcium aluiminate and zinc chromate
- thermite in an epoxy matrix
- acrylic coating with clay and cadmium sulfide pigment
- etc.

All these are very different where it matters, one would even contain thermite, but DSC is unable to tell these apart.

or the right conclusion.

No.

"...indicate that the gray layers are consistently characterized
by high iron and oxygen content including a smaller amount
of carbon. The chemical signatures found in the red layers
are also quite consistent (Fig. 7), each showing the presence
of aluminum (Al), silicon (Si), iron (Fe) and oxygen (O), and
a significant carbon (C) peak as well"

THIS is blah blah blah.
"presence of Al" would be satisfied if you have aluminium, alumina, aluminium silicate or aluminates. All significantly different in context.
"presence of Al" would be satisfied if you have elemenal silicon, silica, silicates... All significantly different in context.
"presence of Fe" could be satisfied by elemental iron, various iron oxide and hydrocides, iron carbides, etc. All significantly different in context.
C and O are no brainers to start with, since we are obviously dealing with hydrocarbon matrixes, of which many are possible. All significantly different in context. And pretty much every compound in the context has oxygen.

i know your response will be blah..blah...blah..blah

It would be an appropriate response to your / Jones's blah..blah...blah..blah.

 

[Redwood]

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.

Furthermore, industrial-grade bulk chemicals will commonly contain traces of other, similar materials. There's no point in refining them to something like analytical reagent purity so long as it doesn't affect its intended use. I should expect that commercial aluminum silicate will contain certain amounts of magnesium silicate, potassium aluminum silicate, silica, etc., and that this will vary from batch to batch. Paint isn't exactly a high-tech item.

 

[Oystein]

Furthermore, industrial-grade bulk chemicals will commonly contain traces of other, similar materials. There's no point in refining them to something like analytical reagent purity so long as it doesn't affect its intended use. I should expect that commercial aluminum silicate will contain certain amounts of magnesium silicate, potassium aluminum silicate, silica, etc., and that this will vary from batch to batch. Paint isn't exactly a high-tech item.

Correct. "Aluminium silicate" is simply clay. Most clays for such purposes come from natural deposits and contain several other silicates besides Al-silicate. Silicate clays from Georgia, for example, have mainly impurities from Ti, but also Mg, Ca, Nl and K, as well as some Fe2O3.

 

[Redwood]

Correct. "Aluminium silicate" is simply clay. Most clays for such purposes come from natural deposits and contain several other silicates besides Al-silicate. Silicate clays from Georgia, for example, have mainly impurities from Ti, but also Mg, Ca, Nl and K, as well as some Fe2O3.

One might even say that silicates in general are <ahem> as common as dirt!