Tuesday, July 1, 2014

Dr. Harrit´s Aluminum Data

John-Michael Talboo and Ziggi Zugam cover the whole Harrit VS Millette debate in an essay written for Mark Basile´s fundraising effort: http://911debunkers.blogspot.com/2013/06/why-you-should-make-donation-at.html

Part IV: The Elemental Aluminum. So, how does Dr. Millette justify the lack of replication? He essentially states that further testing is unnecessary because there is "no evidence of individual elemental aluminum particles of any size in the red/gray chips, therefore the red layer of the red/gray chips is not thermite or nano-thermite." Millette claims that the plates of silicon and aluminum inside the chips are kaolin, which is a clay material that happens to be a common ingredient in paints. But as we have previously noted, Millette is probably not studying the same material as Harrit et al. - and in this case Millette may have found kaolin because he is focusing on the paint chips also present in the dust, despite Kevin Ryan´s specific warning. Kaolin plates may look very similar to coated aluminum platelets, but Millette finds kaolin plates as thin as 6 nm while Harrit et al. report consistent platelets "approximately 40 nm thick." Millette and his sponsors should have known that they could expect to find the aluminum in the correct chips hidden inside a protective coating based on silicon. They have failed to read the excellent references that Harrit et al. cite, including this one which explains that the coating is "essential to protect aluminum nanopowder.." and that it "leads to better dispersion...and more uniform mixing." The protective layer not only promotes efficiency, it also prevents air-oxidation and humidity from deactivating the elemental aluminum, which explains how the chips could remain active for so many years.

Harrit et al. agree that their chips contain aluminum and silicon together in the same space, but how do they determine whether or not the two chemicals are separate or chemically bound together as kaolin? As we note in Part II, when you compare the signals for Al/Si before and after ignition, you see that the peaks no longer have the same ratio after ignition and that the aluminum is relatively depleted, which is not consistent with a compound. And the team discovered that MEK paint-solvent induces swelling in their chips that segregates the silicon from the aluminum, which proves that they are not chemically bound together, so the plates in their chips are not kaolin. This is confirmed with chemical analysis and clear visual representations, but the "debunkers" ignore this important result. They claim that the main chips studied (chips "a to d" depicted in fig.7) are LaClede primer-paint that contains kaolin, and that the MEK chip is another type of paint (Tnemec) that does not have kaolin. Adam Taylor notes in his March 2011 article that the source for this MEK hand-wave is Sunstealer´s March 2011 post where he announces that the XEDS spectrum for the MEK chip (fig.14) looks very similar to the spectrum for Tnemec primer-paint. But as Taylor explains, the XEDS spectrum for the MEK chip represents the unwashed and contaminated surface, while the spectra for the other chips represent clean surfaces. The contaminants happen to make the unwashed MEK chip look like Tnemec, but Sunstealer´s rationale is essentially pretending that there is no contamination. 
ScootleRoyale´s excellent March 2012 article also demolishes Sunstealer´s premise for this theory, because the unwashed surface of all the studied chips had a spectrum similar to the unwashed MEK chip according to one of the authors of the study, including the chips featured in the paper (in figure 7). ScootleRoyale also demonstrates to Oystein how untenable the MEK hand-wave is by noting the fact that the MEK solvent does not dissolve or soften the chip, unlike confirmed Tnemec chips: "The reason Harrit et al. soaked a chip in MEK was to compare the result to Tnemec primer!" 

Talboo and Weathers also demonstrate in their May 2011 article that Sunstealer´s MEK Hand-wave is an obvious failure because there is no elemental aluminum in Tnemec, only aluminum bound to calcium. Tnemec also contains zinc, but the MEK chip only has Zn and Ca as surface contaminants which disappear after the wash in the MEK. Talboo and Weathers respond to Oystein´s objections to Taylor´s article, including his claim that Harrit et al. simply could not register Zn and Ca with their equipment settings for the recorded spectra after the MEK soak. Unfortunately for Oystein, his fellow JREF´er has debunked his claim and confirmed that Harrit´s equipment would have registered the Zn and the Ca. Talboo and Weathers also note that Dr. Farrer debunks Oystein´s claim that they mislabeled Zn as sodium(Na). According to Farrer, the sodium "peak that is found in fig 18 was confirmed by the absence of the Zn k-alpha peak at 8.637keV (and yes, the same exact spot was analyzed at a beam energy of 20kV and the Zn k-alpha peak is still not present)." Farrer goes on to say that "while it is true that the Na k-alpha peak (1.04keV) overlaps the Zn L-alpha (1.012keV), it is pretty simple to confirm which element is present."

After soaking the MEK chip, Harrit et al. focus on an area with a lot of aluminum to figure out if there is elemental aluminum present. They confirm the presence of elemental aluminum with the XEDS spectrum in figure 17, stating that "a conventional quantification routine" demonstrates "that the aluminum significantly exceeded the oxygen present (approximately a 3:1 ratio)." Figure 17 also demonstrates that the post-soaking MEK chip has a very strong aluminum signal without any Ca or Si present for bonding, so the MEK chip cannot be Tnemec or LaClede, and the conclusion of elemental aluminum is inescapable. See the articles Listening to Debunker Arguments is Like Watching Paint Dry..., Listening to Debunker Arguments is Like Watching Two Coats of Paint Dry..., Millette Versus Harrit et al: The MEK Test, and Oystein's Contamination Denial for more information, and keep in mind Dr. Jones´s message to Sunstealer et al.:
Look, Oystein, why don't you put a sample of Tnemec primer in MEK and soak it, and see whether it becomes limp (as I say) or remains very hard under forceps? Do debunkers ever do experiments? I say, do the experiment and let us know what you find! Experiments are much more convincing in science than hand-waving arguments.
Denis Rancourt has suggested that the XEDS sample-holder provides the aluminum signal, but Harrit notes that their control experiments prove that "the electron beam couldn’t even penetrate the carbon conductive tab used as substratum..." In other words, "the Al/Mg scaffold was never hit in any of the spectral recordings published in the article." Harrit also mentions that they have unpublished TEM analysis where "the samples were mounted on a copper holder and these measurements also confirm the presence of aluminum." According to Dr. Jones, their unpublished analysis via TEM and XRD is consistent with their previous (MEK test) conclusion of ruling out kaolin, but he notes that the new tests have not resulted in conclusive identification of pure aluminum - According to Jones, the aluminum might be in an amorphous form that is difficult to detect.

Basile plans to introduce one new test method (ESCA small spot technique with argon ion sputter) to directly establish the presence of unbound aluminum. Basile also plans to confirm aluminum by having an independent laboratory repeat the ignition tests, in air and inert atmosphere. He notes in a December 2012 interview (at 37m.55s.) that the chips will most likely also ignite in an inert atmosphere, and that even if they do not, that this test will still reveal any elemental aluminum since it will melt and leave a signature endothermic peak at a certain temperature. ScootleRoyale notes in his March 2012 article that that two of Harrit´s air-ignited samples have an endothermic peak around the 660 degree(C) melting point of aluminum, which is another strong indication of elemental aluminum:

"Notice how two of the traces go into the negative at around 620-670 degrees celsius. A small endothermic peak in this temperature range is characteristic of aluminium melting. This suggests that even after the reaction, there was still some elemental aluminium left over in those chips, which then melted." - Scootle
The fact that the chips actually work when ignited is also a very strong indication of elemental aluminum, according to one of Harrit´s co-authors, Dr. Frank Legge. Dr. Legge, who holds a PhD in chemistry, has stated that:
...The existence of elemental aluminium in the red chips is proven by the formation of the microspheres in the DSC, largely iron. What else can start to rip the oxygen out of iron oxide at below 400 deg C, then have a runaway temperature increase at least to the melting point of iron? Those who dispute this on the grounds that oxygen was present, and that the energy came from the combustion of organic material, must provide an explanation for why such special conditions are required in a blast furnace to produce iron. The idea that you could heat a little kaolin and coke and iron oxide to a mere 400 deg C and see it suddenly run away and produce molten iron is clearly a fantasy. http://www.thepotteries.org/shelton/blast_furnace.htm