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Tags Laclede primer , nanothermite , Niels Harrit , paint chips , tnemec , wtc

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Old 22nd August 2011, 02:49 AM   #241
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Originally Posted by Oystein View Post
Actually, we already know fairly well.
Analysis of the organic matrix is missing, and of course more work on the gray layer. Some better XEDS data, especially beyond 10keV, and with better resolution, would be helpful, but what we have is 90% of what we need.
Of course, XRD would show clearly and beyond any residual doubt that we are correct about hematite and kaolinite, but we are already sufficiently certain about that: The relative amounts of Si and Al are too good a fit for Al2Si2O5(OH)4, and the platelike crystal structure look so very much like kaolinite, that there really is no doubt here. We can also be very sure that there is no Si and Al in the mix outside of kaolinite, so there is no free (elemental) Al in these chips at all. We know that aluminiumsilicate, of which kaolinite is one form, are part of many paints, including one particular primer used on a great deal of WTC steel - it all falls into place.
I need to read again the several threads on this topic....that will take me several days.....

I'm just baffled that no truther insists that they submit the dust for independent testing.....
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Old 22nd August 2011, 05:26 AM   #242
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http://forums.randi.org/showpost.php?p=7484691&postcount=677

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Old 22nd August 2011, 05:27 AM   #243
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Originally Posted by newton3376 View Post
I need to read again the several threads on this topic....that will take me several days.....

I'm just baffled that no truther insists that they submit the dust for independent testing.....
This may help explain..

http://www.internationalskeptics.com...&postcount=677 hyperlink
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Old 22nd August 2011, 10:10 AM   #244
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Finally some (partial) info on the thermal degradation of epoxide resins (both under air and under inert gas)

Let me repeat (mostly for the accidental visitors):
Harrit et al. observed exothermic peaks on DSC curves of red-gray chips about 420 oC
Laclede primer paint contained epoxide binder cured/crosslinked/hardened by some polyamine. Our question therefore is: could this binder show the similar exotherms at these temperatures (between ca 380 and 450 oC?)

In the research of thermal behavior of polymers (like epoxides), two methods are widely used:
1) TGA (thermogravimetric analysis). Here, the sample (1-2 mg is enough) is slowly heated and the loss of material is observed as a function of temperature. The thermal degradation of polymers is always accompanied with such a loss, since polymer chains (or three-dimensional polymeric networks like in the case of epoxides) are gradually degraded/cleaved and low molar mass compound are formed which evaporate at such high temperatures. TGA is generally used for the measurements of polymer degradation.
2) DSC (differential scanning calorimetry). The sample is again slowly heated (few mg is enough) and the heat evolved/consumed by various procceses are again recorded with an increasing temperature. This method is excellent for the investigation of e.g. phase transitions in polymers (crystallization, melting), in which the overal amount of material remains constant, but... it is not very suitable for the degradation of polymers where the loss of material is substantial. Therefore, DSC measurements of the thermal degradation of polymers are not very common.

After some hour spent with our experts on DSC and TGA and after some literature search I can write here now:

The rapid thermal degradation of polymers as recorded by TGA (both purely thermal and oxidative) proceeds very frequently just in the range between 400 and 450 oC. The usual onset is slightly below 400 oC. You can find some typical examples here: http://depts.washington.edu/mseuser/.../TGA_Notes.pdf and there is also a TGA curve of some epoxide in Fig. 3 Even (quite complicated heteroaromatic) polymers synthesized by me show the same rapid degradation in this region, both under air and under argon, see corresponding figures in my/our recent papers: http://onlinelibrary.wiley.com/doi/1...24022/abstract http://onlinelibrary.wiley.com/doi/1...24780/abstract.

The same is valid also for epoxides. To my slight surprise, these highly crosslinked networks also rapidly degrade within the same "suspicious" temperature range even under inert atmosphere with a very substantial loss of mass, see e.g. these papers:
Polymer Degradation and Stability Volume 80, Issue 2, 2003, 383-391
Journal of Materials Science Volume 36, Number 18, 4405-4409
Polymer Degradation and Stability Volume 56, Issue 3, June 1997, Pages 291-299
Polymer Letters Vol.3, No.8 (2009) 501–509 etc.

Dr. L. Matejka from our institute explained me: the high temperature causes a cleavage of epoxide resin to shorter segments and volatile compounds like aromatic and aliphatic stuffs. If the air /oxygen is present, these segment/compounds are quickly oxidized and more heat is evolved. Roughly: the presence of oxygen usually lead to the degradation at slightly lower temperatures and with increased rate. This is, in fact, the manner how epoxides (and many other polymers) burn at temperatures between 400 and 500 oC.

So I still think that epoxide resins can thermally behave like red-gray chips. But, the degradation chemistry of epoxide resins is quite complicated and depends on many factors, including used hardener, the overal structure, the content of fillers (e.g. inorganics like Fe2O3 of aluminosilicates etc. Direct DSC measurements of more red-gray chips (best in the correlation with TGA) is still needed…

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Old 22nd August 2011, 11:42 AM   #245
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Originally Posted by bill smith View Post
Where on the attached chart do you think the grey material would fit ? From 0.001 to 100 ?
http://www-materials.eng.cam.ac.uk/m...s/IEChart.html
Towards the ceramics.


Originally Posted by Ivan Kminek View Post
Finally some (partial) info on the thermal degradation of epoxide resins (both under air and under inert gas)

Let me repeat (mostly for the accidental visitors):
Harrit et al. observed exothermic peaks on DSC curves of red-gray chips about 420 oC
Laclede primer paint contained epoxide binder cured/crosslinked/hardened by some polyamine. Our question therefore is: could this binder show the similar exotherms at these temperatures (between ca 380 and 450 oC?)


After some hour spent with our experts on DSC and TGA and after some literature search I can write here now:

The rapid thermal degradation of polymers as recorded by TGA (both purely thermal and oxidative) proceeds very frequently just in the range between 400 and 450 oC. The usual onset is slightly below 400 oC. You can find some typical examples here: http://depts.washington.edu/mseuser/.../TGA_Notes.pdf and there is also a TGA curve of some epoxide in Fig. 3 Even (quite complicated heteroaromatic) polymers synthesized by me show the same rapid degradation in this region, both under air and under argon, see corresponding figures in my/our recent papers: http://onlinelibrary.wiley.com/doi/1...24022/abstract http://onlinelibrary.wiley.com/doi/1...24780/abstract.

The same is valid also for epoxides. To my slight surprise, these highly crosslinked networks also rapidly degrade within the same "suspicious" temperature range even under inert atmosphere with a very substantial loss of mass,

Dr. L. Matejka from our institute explained me: the high temperature causes a cleavage of epoxide resin to shorter segments and volatile compounds like aromatic and aliphatic stuffs. If the air /oxygen is present, these segment/compounds are quickly oxidized and more heat is evolved. Roughly: the presence of oxygen usually lead to the degradation at slightly lower temperatures and with increased rate. This is, in fact, the manner how epoxides (and many other polymers) burn at temperatures between 400 and 500 oC.
Thanks Ivan - polymer chemistry isn't my strong point. It's interesting to have confirmation from experts that these materials will degrade in the exact region we are interested in. I suspected so. Look at these TGA thermograms

http://www.springerimages.com/Images...9-009-0052-0-6
http://www.springerimages.com/Images...9-009-0052-0-7
http://www.springerimages.com/Images...4-009-9991-3-4

I also wondered why it was so difficult to find DSC thermograms, thanks for the answer on that one.

I think there is plenty of evidence to suggest that this material is Laclede standard paint rather than thermite.

I'd be interested to see what your experts make of this truther video http://www.youtube.com/watch?v=t-pFb...layer_embedded

It's certainly not thermite.

Cheers.
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Old 22nd August 2011, 11:51 AM   #246
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Originally Posted by Oystein View Post
. I have a hunch that there was much more LaClede primer in the towers than Tnemec.
Good hunch. My in-head calculation is yes, unless I'm thinking of the floor system structure in the wrong way. (I'm assuming the steel floor deck would have been painted with LaClede).

ETA nevermind, I see you guys already covered that and decided the decks were probably galvanized...




Quote:
Another thing we should do is to ignore Bill Smith, unless he provides constructive critique and helpfull hints, rather than displaying his ignorance and trollishness.
I've had BS on ignore for a long time. I don't care whether he's a troll or not....makes no difference to me.
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Old 22nd August 2011, 11:54 AM   #247
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Originally Posted by Sunstealer View Post
Towards the ceramics.


Thanks Ivan - polymer chemistry isn't my strong point. It's interesting to have confirmation from experts that these materials will degrade in the exact region we are interested in. I suspected so. Look at these TGA thermograms

http://www.springerimages.com/Images...9-009-0052-0-6
http://www.springerimages.com/Images...9-009-0052-0-7
http://www.springerimages.com/Images...4-009-9991-3-4

I also wondered why it was so difficult to find DSC thermograms, thanks for the answer on that one.

I think there is plenty of evidence to suggest that this material is Laclede standard paint rather than thermite.

I'd be interested to see what your experts make of this truther video http://www.youtube.com/watch?v=t-pFb...layer_embedded

It's certainly not thermite.

Cheers.
Thanks for that. To me it looks like something inside the chip reacts causing the swelling and giving off gas. That's not metal I see inside is it ?

PS it also looks like the reactive substance inside the chip reacts and gives off gas before the main ignition,
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Old 22nd August 2011, 12:11 PM   #248
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Sunstealer are all the ingredients in the grey layer also present in the red layer ?
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Old 22nd August 2011, 12:20 PM   #249
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Originally Posted by Oystein View Post
Ivan, thanks for the interesting details on electrophoretic deposition!


Surely.
Phosphorus is next to Al (13), Si (14) and S (16) in atomic number, which are all clearly detectable by XEDS. It has the following edge energies:
K-alpha: 2.015 keV
K-beta: 2.136keV
K: 2.149
Fig. 6 of Harrit e.al. shows no discernable peaks above noise around 2.1keV.
Phosphating is a chemical process which converts a metallic surface to a non-metallic surface by chemically bonding a phosphate coating to the metal. The phosphate coating therefore forms an integral part of the surface composition.

I've no idea whether this P would show up in the gray layers. P is observed in a couple of the spectra in the paper. Fig 18 is labelled as such too.

Originally Posted by Oystein View Post
You should specifically ask if the process would oxidize a surface layer of the steel.
Depends if the steel structure is the anode or the cathode.

When I was at school there was a little phrase or saying to help you remember whether the anode or cathode was oxidised or reduced. Shame I've forgotten it!

The anode is oxidising and the cathode is reducing.

If the steel is the anode then you will get oxidisation and partial dissolution of the steel. Same as when you have a cell for electroplating. Remember metals form an oxide layer on contact with air so there will be a layer of oxidised material anyway.
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Old 22nd August 2011, 12:43 PM   #250
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LOL, I've had a guy on my channel telling me I don't understand DSC, or the thermite reaction. He's partially right, but then I'm not offering my personal opinion, but merely representing the criticisms made by those who DO understand these things.

If you guys would like to engage this fella (he's apparently married to a scientist, so he's not a typical truther - they're usually scientists dabbling outside their fields of expertise... ) go to:

http://www.youtube.com/all_comments?v=EY3nj728WPY

I think he's afraid to venture onto JREF discussions. As he should be..
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Old 22nd August 2011, 03:08 PM   #251
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Originally Posted by Sunstealer View Post
Towards the ceramics.



Cheers.
Ceramic,noun.. def..[ an artifact made of hard brittle material produced from from nonmetallic minerals by firing at high temperatures]
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Old 22nd August 2011, 03:18 PM   #252
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Originally Posted by bill smith View Post
Ceramic,noun.. def..[ an artifact made of hard brittle material produced from from nonmetallic minerals by firing at high temperatures]
towards [təˈwɔːdz tɔːdz]
prep 1. in the direction or vicinity of towards London
2. with regard to her feelings towards me
3. as a contribution or help to money towards a new car
4. just before towards one o'clock
5. Irish in comparison with it's no work towards having to do it by hand Also toward
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Old 22nd August 2011, 03:29 PM   #253
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Originally Posted by alienentity View Post
Good hunch. My in-head calculation is yes, unless I'm thinking of the floor system structure in the wrong way. (I'm assuming the steel floor deck would have been painted with LaClede).

ETA nevermind, I see you guys already covered that and decided the decks were probably galvanized...
Yes, but the floor trusses... I haven't had the time to look through construction details... how many trusses are there per floor?
I also need to learn the correct terminology. Each truss (joist?) consists of a top and a bottom "beam", connected by smaller diagonal pieces.

Looking at Figure 4-7 in NCSTAR 1-6 right now:
Floors were about 3.75m high on average; with 240 perimeter and 47 core columns, that's 416 meters of column per floor. However, a typical office floor had 1400 meters of primary trusses and 600 meters of bridging trusses. Columns are wider, but I guess that does not offset the fact that trusses were 5 times longer on aggregate than columns.
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Old 22nd August 2011, 03:34 PM   #254
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Originally Posted by Sunstealer View Post
Phosphating is a chemical process which converts a metallic surface to a non-metallic surface by chemically bonding a phosphate coating to the metal. The phosphate coating therefore forms an integral part of the surface composition.

I've no idea whether this P would show up in the gray layers. P is observed in a couple of the spectra in the paper. Fig 18 is labelled as such too.
Yep

Originally Posted by Sunstealer View Post
Depends if the steel structure is the anode or the cathode.

When I was at school there was a little phrase or saying to help you remember whether the anode or cathode was oxidised or reduced. Shame I've forgotten it!

The anode is oxidising and the cathode is reducing.

If the steel is the anode then you will get oxidisation and partial dissolution of the steel. Same as when you have a cell for electroplating. Remember metals form an oxide layer on contact with air so there will be a layer of oxidised material anyway.
Ivan wrote:
Originally Posted by Ivan Kminek View Post
...
More specifically, an epoxide paint (like Laclede primer under discussion) forms colloid particles, consisting mostly of pigment and adducts of epoxide oligomers with amine hardener. Such an hardener is basic (positively charged) so the colloid particles migrate to the cathode (painted steel) in this case.
...
Too tired now to check this for plausibility. But if you two are right, then the electropainting should not add to oxidation of steel.

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Old 22nd August 2011, 05:21 PM   #255
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Just the usual milling process produces a thin layer of oxided iron on steel bar stock. I have not seen any good photos of the assembled trusses before painting, but I would assume they were made by a rolling process, thus would be covered in the usual grey to black oxide layer. I have seen the angled parts begin fabricated, and they appear a bit lighter, thus may have been formed by a different process. This element was, of course a smaller percentage of the total surface area of the truss assemblies.

It was my impression that not all the chips were red/grey. I would expect there to be some relation between the number of red/grey and all red chips to the comparative surface areas of the two elements of the trusses, with the all red chips coming mostly from the angled ties.

(We need to establish the nomenclature of the parts of the truss assembly if we look any closer at this element.)
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Old 22nd August 2011, 10:44 PM   #256
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Originally Posted by bill smith View Post
Thanks for that. To me it looks like something inside the chip reacts causing the swelling and giving off gas. That's not metal I see inside is it ?

PS it also looks like the reactive substance inside the chip reacts and gives off gas before the main ignition,
I think (but cannot be sure) that this video show what might be expected for, e.g., a paint particle containing epoxide (see above): epoxide was first degraded by the flame and volatile degradation products (a fume visible) were then ignited by the still hot particle.
Remember: volatile compounds are what in fact burn even when you ignite a wood in your fireplace - this is the reason why it is not so easy to ignite it. On the other hand, a burning of this particular particle looks to be too slow for any thermite. (What about to buy some epoxy red primer, cure it and record some (micro)video of its burning? I am going to visit some hobby shop...) Concerning metallic or shiny appearence - photos and videos from the microworld are rather treacherous for our eyes - many things look shiny when magnified.

Originally Posted by bill smith View Post
Sunstealer are all the ingredients in the grey layer also present in the red layer ?
A strange question, after all this discussion. According to XEDS, gray layers contain just iron, oxygen a some carbon - and these elements were also present in the red layers of all chips.

Originally Posted by Oystein View Post
Yep Too tired now to check this for plausibility. But if you two are right, then the electropainting should not add to oxidation of steel.
After some more search I am quite sure that common epoxides hardened by amines are deposited on the cathode in the electrocoating process.

Originally Posted by Oystein View Post
Looking at Figure 4-7 in NCSTAR 1-6 right now:
Floors were about 3.75m high on average; with 240 perimeter and 47 core columns, that's 416 meters of column per floor. However, a typical office floor had 1400 meters of primary trusses and 600 meters of bridging trusses. Columns are wider, but I guess that does not offset the fact that trusses were 5 times longer on aggregate than columns.
Some (much) more thorough calculations are welcome Btw, we expect so far that the Laclede primer was stripped out from the steel joists during collapses to the quite high extent, since it can explain the abundance of paint particles in the dust. Looking again to some photos of the floor joist steel (post #206, link http://www.drjudywood.com/articles/JJ/JJ5.html Fig. 14) this steel looks more rusty than painted. But, this rusty color can be to some extent also a result of mixing of colours of iron oxide (red) and strontium chromate (yellow) in the paint. I would like to possess a piece of this widely twisted steel...

Last edited by Ivan Kminek; 22nd August 2011 at 11:01 PM.
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Old 23rd August 2011, 01:19 AM   #257
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Originally Posted by leftysergeant View Post
Just the usual milling process produces a thin layer of oxided iron on steel bar stock. I have not seen any good photos of the assembled trusses before painting, but I would assume they were made by a rolling process, thus would be covered in the usual grey to black oxide layer. I have seen the angled parts begin fabricated, and they appear a bit lighter, thus may have been formed by a different process. This element was, of course a smaller percentage of the total surface area of the truss assemblies.

It was my impression that not all the chips were red/grey. I would expect there to be some relation between the number of red/grey and all red chips to the comparative surface areas of the two elements of the trusses, with the all red chips coming mostly from the angled ties.

(We need to establish the nomenclature of the parts of the truss assembly if we look any closer at this element.)
There might be some useful pictures here Sarge.
http://www.youtube.com/watch?v=A5MRz...layer_embedded
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Old 23rd August 2011, 02:00 AM   #258
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Originally Posted by bill smith View Post
There might be some useful pictures here Sarge.
http://www.youtube.com/watch?v=A5MRz...layer_embedded
Thanks!
Source is here:
http://911datasets.org/index.php/NIS...g_-_Release_29
(That page links to Bittorrent download)
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Old 23rd August 2011, 02:25 AM   #259
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Originally Posted by Ivan Kminek View Post
I think (but cannot be sure) that this video show what might be expected for, e.g., a paint particle containing epoxide (see above): epoxide was first degraded by the flame and volatile degradation products (a fume visible) were then ignited by the still hot particle.
Remember: volatile compounds are what in fact burn even when you ignite a wood in your fireplace - this is the reason why it is not so easy to ignite it. On the other hand, a burning of this particular particle looks to be too slow for any thermite. (What about to buy some epoxy red primer, cure it and record some (micro)video of its burning? I am going to visit some hobby shop...) Concerning metallic or shiny appearence - photos and videos from the microworld are rather treacherous for our eyes - many things look shiny when magnified.



A strange question, after all this discussion. According to XEDS, gray layers contain just iron, oxygen a some carbon - and these elements were also present in the red layers of all chips.



After some more search I am quite sure that common epoxides hardened by amines are deposited on the cathode in the electrocoating process.



Some (much) more thorough calculations are welcome Btw, we expect so far that the Laclede primer was stripped out from the steel joists during collapses to the quite high extent, since it can explain the abundance of paint particles in the dust. Looking again to some photos of the floor joist steel (post #206, link http://www.drjudywood.com/articles/JJ/JJ5.html Fig. 14) this steel looks more rusty than painted. But, this rusty color can be to some extent also a result of mixing of colours of iron oxide (red) and strontium chromate (yellow) in the paint. I would like to possess a piece of this widely twisted steel...
Thanks Ivan. Would you say that the amount of oxygen present in the grey layer is surprisingly high ?
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Old 23rd August 2011, 02:44 AM   #260
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Originally Posted by bill smith View Post
Thanks Ivan. Would you say that the amount of oxygen present in the grey layer is surprisingly high ?
No. That layer has less O than rust, rust is part of thermite, and the red layer is not thermite. Where is the thermite?

Would you say there is a lot of carbon in thermite? Got any ideas? Got chemistry?

Last edited by beachnut; 23rd August 2011 at 02:56 AM.
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Old 23rd August 2011, 03:35 AM   #261
Ivan Kminek
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Burning of epoxide under air - a macroscopic approach

Introduction:
I have visited two big hobby markets this morning. It seems that no red epoxy primers are easily available here, such specialty paints can be probably found in some big paint shops only. Anyway, I have no electrophoretic facility to apply it to the steel…

Meanwhile, I bought some epoxy adhesive/sealant (clear, i.e. without any filler), with the amine hardener (as can be judged from its fishy smell). Here is a description of my very first “experiment” on its burning. I decided to use aluminum oxide as filler here since this non-reactive stuff should not significantly change the epoxy thermal/oxidative behavior. I added 20 wt % of this powder to the epoxy.

Experimental:
Epoxy used: Pattex Repair Universal Epoxy (Henkel Co, 5 min hardening time)
Filler: Aluminum oxide, basic, very fine particles (20 wt%)

Preparation of “epoxy macrochip”: both components of epoxy were weighed and thoroughly mixed with a weighed amount of Al2O3. The resulting viscous mixture was cast on polyethylene substrate. After hardening (1h), the white layer of the filled epoxy resin was stripped out from the substrate.

Burning experiment: the macrochip (irregular shape, ca 5x7 mm, thickness about 0.2 mm) was placed on the microscopic slide and ignited with an ordinary lighter (manufacturer unknown).

Filming device: mobile phone Nokia E52. Method of picture stabilization: trying to keep my old fingers not trembling too much.


Results and discussion:
You can see the video of this burning here http://www.youtube.com/watch?v=zfCclPpYSvU. I am therefore proud that I also added one more blurred video to the countless row of them in Youtube…
As you can see, the epoxide chip was easily ignited and burned with some bright flame for some seconds. Horrible smell was evolved as well.

Conclusion:
Chip of this cured epoxide resin filled with aluminum oxide (20 wt%) easily burns under air when ignited with an open flame. Dark (charred, brittle) residue can be observed as a result of this burning.

Last edited by Ivan Kminek; 23rd August 2011 at 04:51 AM.
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Old 23rd August 2011, 10:45 AM   #262
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Originally Posted by bill smith View Post
Thanks Ivan. Would you say that the amount of oxygen present in the grey layer is surprisingly high ?
What do you mean by high? What level is just right or expected? What level is high? Please show your calculations. Why are you even asking this?
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Old 23rd August 2011, 11:27 AM   #263
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Originally Posted by Sunstealer View Post
What do you mean by high? What level is just right or expected? What level is high? Please show your calculations. Why are you even asking this?

I'm just following a harmless train of thought Sunstealer. I know that the oxygen levels were very high. I want to find out if there is any reason why such high levels might be unexpected.
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Old 23rd August 2011, 11:31 AM   #264
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Originally Posted by bill smith View Post
I'm just following a harmless train of thought Sunstealer. I know that the oxygen levels were very high. I want to find out if there is any reason why such high levels might be unexpected.
How high were they? How high are they in rust? Looks like you don't know what you are talking about? Please how high were the oxygen levels? Compare that to rust, Fe/iron rust for us. What conclusion do you make?
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Old 23rd August 2011, 11:55 AM   #265
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Originally Posted by bill smith View Post
I'm just following a harmless train of thought Sunstealer. I know that the oxygen levels were very high. I want to find out if there is any reason why such high levels might be unexpected.
You know that the oxygen levels were very high do you? OK. How do you know this? What is your baseline? How are you working out that oxygen levels were high? Show your working. Show your evidence for high oxygen levels. I expect some work not a one word answer.
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Old 23rd August 2011, 12:29 PM   #266
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Originally Posted by Sunstealer View Post
You know that the oxygen levels were very high do you? OK. How do you know this? What is your baseline? How are you working out that oxygen levels were high? Show your working. Show your evidence for high oxygen levels. I expect some work not a one word answer.
From the peer reviewed paper...

''..indicate that the gray layers are consistently characterized
by high iron and oxygen content including a smaller amount
of carbon.''
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Old 23rd August 2011, 12:35 PM   #267
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Originally Posted by bill smith View Post
From the peer reviewed paper...

''..indicate that the gray layers are consistently characterized
by high iron and oxygen content including a smaller amount
of carbon.''
Now that's an even funnier answer than I expected..........nice troll!
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Old 23rd August 2011, 12:44 PM   #268
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Originally Posted by bill smith View Post
From the peer reviewed paper...

''..indicate that the gray layers are consistently characterized
by high iron and oxygen content including a smaller amount
of carbon.''
Give me strength. /facepalm.
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Old 23rd August 2011, 01:30 PM   #269
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Originally Posted by Sunstealer View Post
Give me strength. /facepalm.
So ?...is the amount of O surprising ?
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Old 23rd August 2011, 02:33 PM   #270
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Originally Posted by bill smith View Post
So ?...is the amount of O surprising ?
Not to someone competent enough to understand X-ray spectral analysis and materials science.
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Old 23rd August 2011, 03:24 PM   #271
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Originally Posted by bill smith View Post
So ?...is the amount of O surprising ?
Bill: I'm a laymen here but, Would you consider the O level in rust high?
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Old 23rd August 2011, 03:37 PM   #272
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Why do you allow Bill to derail this thread so easily? It is obvious that he is trolling! There is no point to his question. Do not reply, unless he manages to reasonably link his question, or work, to the topic of this thread, which is still "can we identify the type of paint?"
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Old 23rd August 2011, 03:49 PM   #273
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Structural steel contains about 0.5% carbon. The gray magnetic material is iron oxide from the surface of the steel . Jones separated based on magnetic properties for some reason.
The solvent he used, MEK, is a poor solvent for cured paint and he didn't think to look at what was in paint stripper [CH2Cl2] to do a proper job. The aluminum and silicon elemental maps overlap [Fig 10 in his paper, as I remember] which says to me that there is no elemental aluminum to speak of. What he neglects to mention is that standard SEM stages are aluminum and shine through of sample is always a possibility. A carbon stage is used if one wants to see aluminum metal.
A simple XRD will show the truth but apparently that is what Jones wants to avoid.
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Old 23rd August 2011, 03:50 PM   #274
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Originally Posted by Oystein View Post
Why do you allow Bill to derail this thread so easily? It is obvious that he is trolling! There is no point to his question. Do not reply, unless he manages to reasonably link his question, or work, to the topic of this thread, which is still "can we identify the type of paint?"
I hope you didn't direct this totally at me. I was trying to make a subtly dig.


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Old 24th August 2011, 01:42 AM   #275
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Originally Posted by pteridine View Post
Structural steel contains about 0.5% carbon. The gray magnetic material is iron oxide from the surface of the steel . Jones separated based on magnetic properties for some reason.
The solvent he used, MEK, is a poor solvent for cured paint and he didn't think to look at what was in paint stripper [CH2Cl2] to do a proper job. The aluminum and silicon elemental maps overlap [Fig 10 in his paper, as I remember] which says to me that there is no elemental aluminum to speak of. What he neglects to mention is that standard SEM stages are aluminum and shine through of sample is always a possibility. A carbon stage is used if one wants to see aluminum metal.
A simple XRD will show the truth but apparently that is what Jones wants to avoid.
Hi pteridine,
I don't think I have seen you around here, so happy to see you in my thread, especially since you seem to have a good grasp on the topic!
The information about Al stages is news to me. Not sure if anybody has thought of this before, and if and how we can eliminate that as a problem. I think I remember that C coating of ...whatever... poses a problem for determining C content. Does that ring a bell?

Anyway, the goal here is not to identify all the flaws that Jones, Harrit and co committed on their way to a moronic conclusions, but to make the best of their work and identify the paint. I think we are already quite certain that the gray layer is oxidized, flaked-off steel. If we could identify the type of steel ... but I think data resolution is too bad for that. As a second best option, we should formulate a theory about the gray layer ("it's Axx steel that oxidized when... and spalled off such and such..."), then, using literature, make predictions about how that would look like in the experiments that were in fact done: EDS spectra, microscopic appearance, electrical resistance, magnetism, ... If we find our predictions are a good fit with experiment, our theory is viable - and the only theory out there, afaik.
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Old 24th August 2011, 01:59 AM   #276
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Thanks, Pteridine)
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Old 24th August 2011, 02:06 AM   #277
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Burning of Laclede primer paint imitation and other epoxide samples under air – still macroscopic approach

Introduction:
I found yesterday (see post #256) that chip of the cured epoxy resin “Pattex Repair Universal Epoxy” filled with 20 wt% of aluminum oxide can be ignited very easily and burns with a bright flame for some seconds.

Then, I decided to prepare some imitation of Laclede primer paint used for the corrosion protection of WTC1 and WTC2 floor joists. Such imitation can serve not only for simple macroscopic burning tests, but also for: a) measurements of its TGA, DSC properties; b) microscopic study of its appearance during/after heating/burning; c) as a sample of typical epoxy resin suitable for the determination of a typical carbon, nitrogen and hydrogen content in epoxides by elemental analysis. Other uses of this paint imitation might be found later.
All these experiments could serve as a supporting info for the hypothesis that chips (a) to (d) in the paper of Harrit et al. were particles of Laclede primer.

In this contribution, my intention was not only to prepare such “Laclede imitation”, but also to compare its (macroscopically observed) burning with burning of previously prepared epoxy resins filled with aluminum oxide (“Al2O3 resin”) and with the pristine (non-filled, “pristine resin”) epoxy as well.

Declared composition of Laclede primer paint was (NCSTAR1-6b report of NIST, Appendix B):

Pigment: (21 % of total weight of dry/cured paint)
Iron oxide 55 % (wt%)
Aluminum Silicate 41 %
Strontium Chromate 4 %
Total Pigment 100 %


Vehicle:
Unmodified Epoxy Amine 45 %
Deionized Water and Amine 55 %
Total Vehicle 100 %


I gathered powdered iron oxide and a form of aluminosilicate called Nanoclay. Since I was not able to get strontium chromate, I decided to replace it with potassium chromate. Although there was not very much of chromate in the Laclede paint, the paint imitation should also contain some chromate, since chromates are generally strong oxidizing agents and can influence thermal/oxidative/burning behavior of the original paint as well as of its imitation.

Experimental:
Preparation of “Laclede imitation” layer:
Used chemicals
- Epoxy: Pattex Repair Universal Epoxy (Henkel, 5 min hardening time), 2.45 g
Fillers:
- Iron oxide, particle size between 1 and 3 μm; dark red-brownish powder (Lachema), 0.55 g
- Nanoclay, an aluminosilicate (hydrophilic bentonite) in the very fine platelet form (Sigma Aldrich), whitish powder, 0.41 g.
- Potassium chromate, yellow powder (Lachema), 0.04 g (molar masses of strontium chromate and potassium chromate are similar – 203.6 vs 194.2, so this amount of potassium chromate is adequate).

The sum of component weights in this epoxy composite is 2.45 + 0.55 + 0.41 + 0.04 g = 3.45 g and its composition should be in a good accordance with the composition of the real Laclede paint. The wt. ratio between epoxy resin and inorganic fillers is 2.45 : 1.

You can see the collection of starting chemicals on this Fig. 1: http://bobule100.rajce.idnes.cz/epox..._imitation.jpg .

Potassium chromate was first thoroughly grinded in a grinding mortar in order to achieve fine particles of this chemical.

Then, all chemicals were thoroughly mixed with a spatula (as usual in the preparation of epoxy adhesives/sealants) and the resulting viscous dark red matter was casted by spatula on polyethylene substrate. After curing (1 h) the tough (but flexible) dark red layer of the “Laclede imitation” was stripped from the substrate.


Preparation of “Al203 resin” layer
It was described in the post #256, but new layer (thicker) was prepared for better comparison here.

Preparation of “pristine resin” layer
It was prepared like in other cases but no filler was added.

All layers were about 0.5-0.8 mm thick.


Macroscopic burning experiments:
The epoxy “macrochips” (irregular shapes, ca 6-8x10-12 mm), were placed on the microscopic glass slides and ignited with an ordinary lighter. Some typical burning experiments were filmed and links to videos are given in the next section.
After burning, chips were again filmed and video is available (see later).


Results and discussion:
You can see typical burning of epoxy chips under study here:
http://www.youtube.com/watch?v=9SGc8..._order&list=UL (pristine resin);
http://www.youtube.com/watch?v=Uhh2w..._order&list=UL (Al2O3 resin);
http://www.youtube.com/watch?v=Pdzr2..._order&list=UL (Laclede imitation).

I can judge from this:
All epoxy samples are easily ignited with an ordinary lighter and burn with the bright flame for ca 30 s to 90 s.
The most flammable is “pristine resin” – the flame was the brightest and lasted for the longest time.
“Laclede imitation” burns better, longer and with the brighter flame than “Al203 resin”. This could be caused (at least partially) by the presence of chromate as oxidizing agent. Also iron oxide might play some role (?).

Chips after burning can be seen here:
http://www.youtube.com/watch?v=ET4gs..._order&list=UL
From the left to right:
“Pristine resin”: molten dark matter as a result, almost whole chip was burned.
“Al2O3 resin” some minor part was burned, this part was dark and brittle.
“Laclede imitation”: about half of the chip was burned, dark brittle matter resulted.

Conclusion:
Generally, fillers in epoxy resins seem to “quench” the burning to some extent, but even both filled resins ignite easily and burn with the bright flame.
In the case of Laclede imitation, it can serve as some hint that the real Laclede primer paint can be easily oxidized, e.g., during DSC measurements under air (as performed by Harrit et al.). This oxidation can be a source of exotherms observed by Harrit et al. for chips (a) to (d).
Further measurements on Laclede imitation (TGA, DSC, some microscopy on burned/heated resin, elemental analysis) will follow soon (I hope).

Thank you for your kind attention)

Last edited by Ivan Kminek; 24th August 2011 at 03:25 AM.
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Old 24th August 2011, 02:28 AM   #278
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(Remark: sorry, I accidentally removed the first video of epoxy burning from yesterday in Youtube. Although I have added this video again to Youtube, the original link in the post #256 probably will not work. But does not matter so much, since the burning of this kind of chip is presented again in the post #277 just above)
Anyway, a question for administrator: can I edit again the post #256 somehow?

Last edited by Ivan Kminek; 24th August 2011 at 02:34 AM.
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Old 24th August 2011, 04:17 AM   #279
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This thread is a good example of the obvious reasons why Jones doesn't want independent verification of his experiments...
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Old 24th August 2011, 04:33 AM   #280
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Originally Posted by Ivan Kminek View Post
Some (much) more thorough calculations are welcome Btw, we expect so far that the Laclede primer was stripped out from the steel joists during collapses to the quite high extent, since it can explain the abundance of paint particles in the dust.
Given that the floor elements all took the express route down the inside of the towers, you shouild expect nearly all of it to have been ground away. This was the devil's own rock tumbler, with multi-ton pieces of grit slamming into the metal elements. I doubt that much paint was left on any of them by the time they reached the end of that maelstrom.

Quote:
Looking again to some photos of the floor joist steel (post #206, link http://www.drjudywood.com/articles/JJ/JJ5.html Fig. 14) this steel looks more rusty than painted.
I am certain that it is mostly rust. If you look at the end of that top rail next to the bunched-up laces on the left edge, you will see that there is a dark area with slightly rusty margins. The paint has been stripped completely away, exposing the black oxide that coated the steel before it was painted. Heat and steam converted most of this black oxide to the red form (will some chemist help me out here? I am looking at it from the background of a casual construction and foundary worker.)

Quote:
But, this rusty color can be to some extent also a result of mixing of colours of iron oxide (red) and strontium chromate (yellow) in the paint. I would like to possess a piece of this widely twisted steel...
On the other hand, it is also a good match with the sort of colors you will see in steel recovered from a really hot fire scene days afterward.

I really doubt that any great amount of the pigment remains on the steel.
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