To recapitulate:
In the 2008 article "Extremely high temperatures during the World Trade Center destruction." by: Steven E. Jones, Jeffrey Farrer, Gregory S. Jenkins, Frank Legge, James Gourley, Kevin Ryan, Daniel Farnsworth, and Crockett Grabbe.
http://www.journalof911studies.com/articles/WTCHighTemp2.pdf Jones et Al found Iron rich spheres prompting further research.
While looking for more evidence about the source of the iron rich spheres a red substance with remarkable exothermic properties was discovered in the 9/11 dust. Published under the title, "Active Thermitic Material Discovered in Dust from the 9/11 World Trade Center Catastrophe." By: Niels H. Harrit, Jeffrey Farrer, Steven E. Jones, Kevin R. Ryan, Frank M. Legge, Daniel Farnsworth, Gregg Roberts, James R. Gourley and Bradley R. Larsen.
https://benthamopen.com/contents/pdf/TOCPJ/TOCPJ-2-7.pdf
These findings have since been dismissed as not the only possible source of iron spheres. Namely, the spheres likely came from 'fly ash' and blast furnace slag.
(Image from post in this tread)
Yet this is not characteristic of the Iron spheres in question.
(Image from Harrit et Al)
I would like to now reexamine the findings of Millette in his 2012. Progress Report on the Analysis of Red/Gray Chips in WTC Dust.
https://www.metabunk.org/attachment...ysis-of-red-gray-chips-in-wtc-dust-pdf.37907/
From Methodology:
The analytical procedures used to characterize the red/gray chips were based on the criteria for the particles of interest in accordance with the recommended guidelines for forensic identification of explosives and the ASTM standard guide for forensic paint analysis and comparison.
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.
Chips of interest were ashed in a muffle furnace using a NEY Temperature Programmable furnace operated at 400o C for 1 hour.
Samples of red/gray chips were placed in several solvents overnight and then subjected to ultrasonic agitation to determine if the solvents could dissolve the epoxy binder and liberate the internal particles. The solvents included methylene chloride, methyl ethyl ketone (MEK), and two commercial paint strippers used for epoxy resins. The commercial paint strippers, Klean-Strip KS-3 Premium Stripper and Jasco Premium Paint and Epoxy Remover, contain methylene chloride, methanol and mineral spirits. One red/gray chip was subjected to 55 hours of submersion in MEK, then dried and coated with a thin layer of gold for conductivity.
From Results:
Red/gray chips that had the same morphology and appearance as those reported by Harrit et al., and fitting the criteria of being attracted by a magnet and having the SEMEDS x-ray elemental spectra described in their paper (Gray: Fe, Red: C,O, Al, Si, Fe) were found in the WTC dust from all four locations examined. The red layers were in the range of 15 to 30 micrometers thick. The gray layers were in the range of 10 to 50 micrometers thick (Appendix B).
The FTIR spectra of the red layer were consistent with reference spectra of an epoxy resin and kaolin clay (Figure 9) (Appendix C).
The SEM-EDS and backscattered electron (BE) analysis of the cross-sections of the gray layer in the red/gray chip showed it to be primarily iron consistent with a carbon steel. The cross-sections of the red layer showed the presence of equant-shaped particles of iron consistent with iron oxide pigment and plates of aluminum/silicon consistent with reference samples of kaolin. The thinnest kaolin plates were on the order of 6 nm with many sets of plates less than 1 micrometer thick. Small x-ray peaks of other elements were sometimes present. The particles were in a carbon-based matrix (Figures 10 through 15) (Appendix D).
TEM-SAED-EDS analysis of the residue after low temperature ashing showed equantshaped particles of iron consistent with iron oxide pigment and plates of kaolin clay. Small numbers of titanium oxide particles consistent with titanium dioxide pigment were also found (Figure 16) (Appendix E).
PLM also found possible clay present based on a microchemical clay-stain test. TEM-SAED-EDS analysis of another portion of the same muffle furnace residue showed equant-shaped particles of iron consistent with iron oxide pigment, plates of kaolin clay and some aciniform aggregates of carbon soot consistent with incomplete ashing of a carbon-based binder (Figure 18). The SAED pattern of the kaolin particles (Figure 19) matched the kaolin pattern shown in the McCrone Particle Atlas (Appendix E). The values for the d-spacings determined for the diffraction patterns matched those produced by reference kaolin samples.
TEM-SAED-EDS analysis of a thin section of the red layer showed equant-shaped particles of iron consistent with iron oxide pigments and plates of kaolin clay (Figures 20 and 21). The matrix material of the red coating layer was carbon-based. Small numbers of titanium oxide particles consistent with titanium dioxide pigment and some calcium particles were also found (Appendix F).
The solvents had no effect on the gray iron/steel layer. Although the solvents softened the red layers on the chips, none of the solvents tested dissolved the epoxy resin and released the particles within. SEM-EDS phase mapping (using multivariate statistical analysis) of the red layer after exposure to MEK for 55 hours did not show evidence of individual aluminum particles (Appendix G).
In summary, red/gray chips with the same morphological characteristics, elemental spectra and magnetic attraction as those shown in Harrit et al. were found in WTC dust samples from four different locations than those examined by Harrit, et al. The gray side is consistent with carbon steel. The red side contains the elements: C, O, Al, Si, and Fe with small amounts of other elements such as Ti and Ca. Based on the infrared absorption (FTIR) data, the C/O matrix material is an epoxy resin. 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. There is no evidence of individual elemental aluminum particles detected by PLM, SEM-EDS, or TEM-SAED-EDS, during the analyses of the red layers in their original form or after sample preparation by ashing, thin sectioning or following MEK treatment.
FROM DISCUSSION:
The Encyclopedia of Explosives describes thermite as essentially a mixture of powdered ferric oxide and powdered or granular aluminum. There are two sets of ingredients listed for thermite in Crippen's book on explosives identification. The first is iron oxide and aluminum powder and the second is magnesium powder, ferric oxide, and aluminum powder. Nano-thermite (thermitic nanocomposite energetic material) has been studied in the Lawrence Livermore National Laboratory in California. A TEM image of a thin section of that material was published by R. Simpson in 2000 and shows material that is made up of approximately 2 nanometer iron oxide particles and approximately 30 nanometer aluminum metal spheres (Figure 22)
According to the Federation of Societies for Coatings Technology, kaolin (also known as aluminum silicate or china clay) is a platy or lamellar pigment that is used extensively as a pigment in many segments of the paint industry. It is a natural mineral (kaolinite) which is found in vast beds in many parts of the world. Iron oxide pigments are also used extensively in paints and coatings. Both kaolin and iron oxide pigments have been used in paints and coatings for many years. Epoxy resins were introduced into coatings in approximately 1947 and are found in a number of specially designed protective coatings on metal substrates.
In forensic studies, paints and coatings often must be broken down so that the components of the entire coating product can be studied individually. Epoxy resins are formed from the reaction of two different chemicals which produces a polymer that is heavily cross-linked. Epoxy resins can be especially difficult to dissolve. Organic solvents, including those sold commercially for epoxy paint/coating stripping, were found to soften the red layer of the red/gray chips but did not dissolve the epoxy resin sufficiently so particles within the coating could be dispersed for direct examination. In this study no organic solvent was found to release particles from within the epoxy resin and it was necessary to use low temperature ashing to eliminate the epoxy resin matrix and extract the component parts of the coating. The other procedures generally used to examine component particles within a coating without extraction (cross-sections and thin sections) were also applied in this study.
FROM NOTES:
At the time of this progress report, the identity of the product from which the red/gray chips were generated has not been determined. The composition of the red/gray chips found in this study (epoxy resin with iron oxide and kaolin pigments) does not match the formula for the primer paint used on iron column members in the World Trade Center towers (Table 1). 16 Although both the red/gray chips and the primer paint contain iron oxide pigment particles, the primer is an alkyd-based resin with zinc yellow (zinc chromate) and diatomaceous silica along with some other proprietary (Tnemec ) pigments. No diatoms were found during the analysis of the red/gray chips. Some 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.
Material Safety Data Sheets (MSDS) contain some information about product materials. According to the MSDS currently listed on the Tnemec website,17 55 out of the 177 different Tnemec coating products contain one or two of the three major components in the red layer: epoxy resin, iron oxide and/or kaolin (aluminum silicate) pigments. However, none of the 177 different coatings are a match for the red layer coating found in this study.
So Millette excludes the possibility of thermite or nano thermite based on the shape of the Al source: thermite and nano thermite both have granular Al powders (spheres) where as in the red substance the Al source is in plates. From the discussion, both the Encyclopedia of Explosives and Crippen's book on explosives identification define thermite and nano thermite as having powdered or granular aluminum as an ingredient. This substance does not match that description as the Al is found in plates supporting Millette's conclusion. This substance is not nano-thermite (2 nm iron oxide and 30 nm aluminum metal spheres).
(Image from Millette: Not Thermite)
The tests on the samples that underwent low temperature ashing and muffle furnace ashing both showed the Al source to be conveniently bonded supporting Millette's conclusion.
(Image from Millette)
However, if the epoxy were mixed with silicone similar results would be obtained with the presence of elemental Al at a scale micrometer scale (plates not spheres). Since the suspected silicone was not dissolved in the epoxy solvents the possibility of elemental Al can not be excluded.
From the notes, Millette also excludes the possibility of the results being explained by the primer used for the WTC buildings.
(Image from Millette)
Millette's conclusions of:
Kaolin: Al2Si2O5(OH)4
22.22Al
22.22SI
55.56O
or- (natural kaolin mixture)
18.67Al
19.26Si
0.53Ca
6.27Ti
10.24Fe
45.03O
Epoxy:
C21H25ClO5
40.38C
48.08H
1.92Cl
9.62O
and Rust: FeO3, could unarguably be formulated to produce the results of the red substance.
(Image from Millette)
However this same spectrum could be produced by a mixture of two paints.
A silver colored paint of 1 part Al (2um) with 20 parts silicone. (fire retardant)
A red primer paint of 2.2 parts FeO3 with 10 parts epoxy. (sealant)
This alone is not alarming.
The alarming detail is that the two paints appear to be electrostaticly painted together. Producing in this combination, something analogues to a nano version of an old solid rocket fuel.
https://patents.google.com/patent/US3309249A/en
The possibility of a high grade propellant found in the evidence of a fire that resulted in catastrophic building failure was not excluded by the findings of Millette. In pursuit of a larger theory of possible arson, I respectfully submit my research to be debunked. Please don't remind me of the OCT (I am well aware). Ad Homonym does not persuade me. The burden of proof was on Millette, and that we are still arguing over it a decade out is evidence that burden not met. I would love to test this further myself but I was informed that mixing these two paints could land me in a world of trouble with ATFB.
Evidence that kaolin not yet present before ashing can be found in Millette's own study.
(Image from Millette)
This is but a few examples where Al and Si are significantly mis matched in the assumed kaolin samples.
(Image from Millette)
Millette offers no explanation for why the Kaolin is so fine.
(Image from Millette)
Millette had conclusively shown that it is kaolin after ashing. But does not explain what looks like SiO2 in the soot, nor does it exclude the possibility of elemental Al (only state that none was found in ashed samples).
@Oystein @Marc Powell