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Saturday, April 27, 2019

Red/Gray Chips, 10 Years Later

Paper on Active-Thermitic Material Remains Unchallenged

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April 3, 2019 marked the tenth anniversary of the publication of the landmark paper, "Active Thermitic Material Discovered in Dust from the 9/11 World Trade Center Catastrophe," by Dr. Niels H. Harrit, along with Dr. Steven Jones, chemist Kevin Ryan and others.  This is one of the key scientific studies that was ignored by the FBI’s 9/11 Review Commission, which underscores the need for a court-overseen review of the 9/11 related evidence that was not included in the 2004 9/11 Commission Report.  This study is so significant that it was included as Exhibit 1 of the Department of Justice Grand Jury Petition filed with the office of the U.S. Attorney in Manhattan, New York, by The Lawyers’ Committee for 9/11 Inquiry. Over the last decade, it has mostly been criticized in the blog-o-sphere.  There was one attempt by James R. Millette, Ph.D., Executive Director of MVA Scientific Consultants, to develop a technical paper refuting the findings of Harrit et al, but upon receiving feedback from his preliminary draft report, the project was abandoned and the analysis was not rehabilitated.  Because Millette's preliminary draft study has been used by many in the blog-o-sphere, who have limited technical competency, a discussion of some of the shortcomings, with the Millette report, is included as an addendum. 


An investigative team, originally lead by Dr. Stephen Jones and Jeff Farrer, discovered distinctive red/gray chips in samples of the dust produced by the destruction of the World Trade Center.  Detailed examination of the chips was then performed by a larger group of experts.  They examined four samples of dust that had been collected from separate sites and reported the results in their paper, "Active Thermitic Material Discovered in Dust from the 9/11 World Trade Center Catastrophe."    One sample was collected by a Manhattan resident about ten minutes after the collapse of the second WTC Tower, two the next day, and a fourth about a week later.

Harrit 10Years Chips 35737 tn
Figure 1: Photomicrographs of red/gray chips from samples 1-4 of the WTC dust involved in this study, shown in (a)-(d) respectively. The inset in (d) shows the chip edge on, which reveals the gray layer. Click image to enlarge.

Naked-eye and microscopic examination revealed numerous tiny metallic, magnetically attracted, spheres and quite distinctive red/gray chips in the dust samples.

The properties of the red/gray chips shown in Figure 1 were analyzed using Optical Microscopy, Scanning Electron Microscopy (SEM), X-ray Energy Dispersive Spectroscopy (XEDS), and Differential Scanning Calorimetry (DSC).

The red material contains grains approximately 100 nano-meters across, which are largely iron oxide, while aluminum is contained in tiny plate-like structures. Separation of components using methyl ethyl ketone demonstrated that elemental aluminum is present. The iron oxide and aluminum are intimately mixed in the red material. When ignited in a DSC, the chips exhibit a large, narrow exothermic event occurring at approximately 430 °C.  The ignition temperature is far below the normal ignition temperature for commercial thermite which consists of large particles of iron and aluminum that have significant distances between the elements (on an atomic scale) .

The paper notes that numerous iron-rich spheres are clearly observed in the residue following the ignition of these peculiar red/gray chips. The red portion of these chips is found to be an unreacted highly energetic thermitic material.

This article briefly summarizes some of the tests presented in the paper.  Please consult the paper, or the videos below, for a more complete discussion.

X-ray Energy Dispersive Spectroscopy (XEDS)

 X-ray Energy Dispersive Spectroscopy is an analytical technique used for the elemental analysis or chemical characterization of a sample. This test relies on the interaction of a narrow beam of X-rays with the atoms in a sample. The characterization capabilities result from the fundamental principle that each element has a unique atomic structure creating a distinct pattern of energy absorption and re-emission as the atoms are excited by x-rays with varying amounts of energy. This process allows identification of the presence of specific atoms in a very precise area.Harrit 10Years XEDS 349e2 tnFigure 2: XEDS spectra obtained from the gray layer (top) and red layer (bottom) for specimen (a) of the WTC dust sample. Click image to enlarge.

In order to carefully observe the characteristics of the red and gray layers, and to eliminate the possibility of surface contamination from other dust particles, the red/gray chips from each of the four WTC dust samples were fractured to expose areas free from contamination. The clean, cross-section surfaces at the fracture were then studied.

As shown for sample (a) in Figure 2, the atoms, comprising the gray layer, are mostly iron and oxygen, with a small component of carbon.  The red layer has a significant amount of carbon with smaller amounts of oxygen, aluminum and silicon.  Subsequent tests confirmed that the aluminum and the silicon are not chemically bound together and that the aluminum is, effectively, suspended in the carbon material as elemental aluminum.  The fact that the aluminum is in an elemental form is important because it is free to react without breaking chemical bonds with other elements, such as silicon.

NOTE: Many critics in the blog-o-sphere will point to the XEDS trace [Harrit et al, Figure 14] that contains zinc, calcium and other elements not found in the clean cross section.  They frequently assert that the presence of these other elements proves the sample was primer paint.  However, this trace [Harrit et al, Figure 14] is from an entire chip (not a clean, fractured face) that would have surface contamination.  For example, the US Geological Survey investigated samples of the WTC dust to determine which elements and compounds were present in the dust.  Their analysis showed that the WTC dust had a geometric mean concentration of 1004 PPM for zinc.  Figure 14, in the  article Review of Atomic Elements Found at the World Trade Center, compares the concentration of zinc in the WTC dust with national averages.

Differential Scanning Calorimetry (DSC)

Differential scanning calorimetry is a thermo-analysis technique in which a known amount of heat is continually added to two similar containers – one with a sample of interest and another that is inert.  During the test as heat is input to the samples, the increase in temperature is observed in both samples and the difference in the change in temperature is noted (using the second sample as a reference). Any difference in the temperature of the sample indicates thermal reactivity (exothermic – energy producing, or endothermic – energy consuming).    

Harrit 10Years DSC 83d2f tnFigure 3: Differential Scanning Calorimeter (DSC) traces for four red/gray chip samples found in World Trade Center dust collections.Click image to enlarge.

When the red/gray chips were heated to about 430 °C, they ignited, releasing relatively large amounts of energy very fast as shown in Figure 3. The residue of the ignited red/gray chips included iron-rich spheres, indicating that a very high temperature reaction had occurred – since the iron-rich product clearly must have been molten to form spheres.

The DSC traces demonstrate that the red/gray chips react vigorously at a temperature below the melting point of aluminum and below the ignition (oxidation) point of ultra-fine grain (UFG) aluminum in air.


Comparison to Published Nanothermite DSC Characteristics

The exothermic properties of the red/gray chips that were shown in the DSC tests were consistent with a DSC trace of a material identified as "super-thermite" in a paper published by researchers associated with Lawrence Livermore National Laboratories ( Tillotson et al., 2001). Figure 4 compares a DSC trace obtained from a WTC red/gray chip with the DSC trace by Tillotson et al.

Harrit 10Years Tillotson 86520 tnFigure 4: DSC trace of sample 1 (blue line) compared with DSC of xerogel Fe2O3/UFG Al nanocomposite (from Tillotson et al.  Both DSC traces show completion of reaction at temperatures below 560 °C.Click image to enlarge.

Both samples begin to demonstrate the start of exothermic behavior at about 400 °C.  A comparison of the two curves shows that WTC sample begins significant exothermic behavior at a lower temperature and reacts more quickly than the Tillotson sample. The higher energy peak for the WTC sample completes at a lower-temperature which suggests a more intimate mixing of the aluminum and iron elements than was present in the Tillotson sample. 

This comparison reinforces the hypothesis that the thermitic material found in the WTC dust is a form of nanothermite, not ordinary commercial thermite. Ordinary commercial thermite ignites at a much higher temperature (about 900 °C or above) and gives a significantly broader trace than the super-thermite.

Formation of Iron Spheres

One of the results of the DSC test was the conversion of the red/gray chips into heat and the production of numerous iron spheres.  The iron spheres from the DSC had the same chemical properties and appearance of the iron spheres that were described by the US Geological Survey and RJ Lee Group during their analysis of WTC dust.

Harrit 10Years IronSpheres 9a594 tnFigure 5: Spheres from: WTC dust (top left); commercial thermite (top right); DSC residue (bottom left), with corresponding DSC XEDS spectrum (bottom right). Click image to enlarge.

Figure 5 compares the iron spheres from three sources: Those found in the WTC dust, commercial thermite and post-DSC spheres.  The Harrit et al paper provides an XEDS comparison of the spheres from these three sources and shows their similarity.  The observations reinforce the hypothesis that the iron spheres have the similar mechanisms of creation.

Methyl Ethyl Ketone (MEK) Reveals Elemental Aluminum

The initial objective of this test was to compare the behavior of the red layer with paint when soaked in a strong organic solvent known to soften and dissolve paint.  Methyl Ethyl Ketone (MEK) is very useful in paint, rust, varnish, lacquer, and grease removers. Paint chips subjected to MEK softened and partly dissolve.  The red layer only swelled when soaked in MEK.

Harrit 10Years MEK Swollen 83e5f tnFigure 6: Photomicrograph of the MEK treated chip. Compare to side view shown in the inset for (d) in Figure 1. Click image to enlarge.

After soaking, the red/gray chips showed significant swelling of the red layer, and apparently, without dissolving any part of the chip. In Figure 6, the red layer and gray layer are shown side by side. The gray layer is on the right – the swollen red layer is on the left.  By visual inspection, the red layer swelled approximately five times its original thickness. 

It was discovered in this process that a significant migration and segregation of aluminum away from other elements had occurred in the red-chip material. This allowed an investigation to determine whether some of the aluminum was in elemental form.

An XEDS spectrum analysis was performed at various locations within the swollen red layer.  A location with a high concentration of aluminum was further analyzed and showed that the amount of aluminum significantly exceeded the oxygen present – by approximately a 3:1 ratio. Given the very high surface area to volume ratio of the aluminum particles and aluminum's propensity to have a layer of aluminum oxide, it is reasonable to find significant amount of oxygen along with the aluminum. However, this low 3:1 ratio means that while some of the aluminum may have been oxidized, a significant amount of the aluminum could not be chemically bound to oxygen.  Therefore, some of the aluminum must exist in elemental form in the red material. This was considered a key observation.

Flame/Ignition Tests

Because the DSC studies did not allow for visual inspection of the energetic reaction, visual tests were performed with a small oxyacetylene flame. The flame was applied to both the red/gray chips and several paint samples. When the samples were heated in the flame:

Red Gray PostFlameIgnition Sphere 9446cFigure 7: Silvery-gray spheroids are seen after the ignition test of red/gray chip. Some of the porous red material remains.

  • The paint samples were immediately reduced to fragile ashes by the hot flame,
  • After a few seconds of heating the first WTC red/gray chip, a high-speed ejection of a hot particle was observed. This was accompanied by an intense light.  The bright orange color of the particle attests to its high temperature. The ejected, small end-product of this visual test reaction was not found.
  • In a second flame-ignition test, the end product was recovered and is shown in the photomicrograph in Figure 7. Once again, the formation of iron-rich semispherical shapes shows that the residue had been melted, enabling surface tension of the liquid to pull it into spherical shapes.

The authors note that the evidence obtained in the DSC analyses is more compelling that a thermitic reaction actually occurred than the supporting/confirming visual observation in the flame ignition test.

A short video clip of the test (including slow-motion) is available here:

Dr. Niels Harrit at "The Toronto Hearings on 9/11: Uncovering Ten Years of Deception"

In 2011, experts and scientists from around the world gathered in Toronto, Canada to present new and established evidence that questioned the official story of 9/11. This evidence was presented to a distinguished panel of experts over a 4 day period. This presentation discussed the research performed with Dr. Harrit's colleagues regarding the active thermitic materials. This presentation is 84 minutes.

Interview with Jeff Farrer

Physicist Jeff Farrer - one of the scientists who found thermite in the World Trade Center dust discusses in depth his process of discovery using the scientific method.  This interview is 34 minutes.

Addendum: The Millette Paper

In early 2012, Dr. James R. Millette, Ph.D., Executive Director of MVA Scientific Consultants, distributed a technical paper that purported to refute the findings of Harrit et al.  However, upon receiving feedback from those who reviewed it, the effort was abandoned.  Subsequently, no other person or entity elected to address the criticisms and the analysis was never furthered or rehabilitated.  Because this preliminary, draft study has been used by many people in the blog-o-sphere, who have limited technical competency, a discussion of some of the issues with the Millette report has been extracted from an article by Kevin Ryan at his Dig Within website.

Millette is well known for having helped create the official reports on the analysis of WTC dust. He was responsible for creating the form that was used to pre-screen all materials found in the dust prior to any analysis by official investigators. Those official reports did not mention any of the evidence listed above, in particular failing to report the abundant iron microspheres scattered throughout the WTC dust. Additionally, Millette’s official report team did not find any red-gray chips, let alone nanothermite.

As he worked to debunk the WTC thermite research, Millette was still unable to find any iron microspheres. But he did claim to have finally found the red-gray chips. Curiously, he did not attempt to replicate the testing that would determine if those chips were thermitic.

Claiming to have found the chips, Millette perfomed an XEDS analysis for elemental composition but failed to do any of the other tests including BSE, DSC, the flame test, the MEK test, or measurement of the chip resistivity. Having inexplicably “ashed” the chips at 400 °C in a muffle furnace, thereby proving that they were not the materials of interest (which ignite at 430 °C), Millette ignored the remainder of the study he had set out to replicate. Because he did not do the DSC test, he could not do XEDS of the spheres formed from the chips. Since he had still not found spheres in the dust, he could not test those and this allowed him to ignore the testing of spheres from the thermite reaction.

KevinRyan ftir911 10b3c

Millette rested his case on Fourier-transform infrared spectroscopy (FTIR), which I have also performed on chips from WTC dust but with a much different result. Like Millette’s paper, my FTIR work is not yet part of a peer-reviewed publication and therefore should not be taken as authoritative evidence. There has been less urgency to this supplemental work because what has been done to date has received no legitimate response from the government or from much of the scientific community. That sad fact should be the central point of discussion today.

In any case, Millette attempted only one tenth of the tests in his struggle to replicate (or refute) one tenth of the evidence for thermite at the WTC. His un-reviewed “one percent approach” was nonetheless very convincing to many people, including some of the people who produced the official reports for 9/11. But it is obvious to others that Millette’s work was not a replication in any sense of the word.

I’m looking forward to the peer-reviewed scientific article that finally does replicate the nanothermite paper or any of the other peer-reviewed scientific papers that document the evidence for thermite at the WTC. Hopefully, we can approach those efforts without concerns about the sources and without recalling all the deception and manipulation that preceded them.

Until then, it is important to recognize the difference between the superficial appearance of science and the actual practice of science. Ignoring 90 percent of the evidence is not scientific. And replication of the 10 percent means actually repeating the work. If thermite debunkers and alternate hypothesis supporters can find the courage and focus to step through that challenge, maybe they can begin to add to the discussion.

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