| NOTE:
The 9,600 pages of FBI documents released to the National Academy of
Sciences include solid evidence that "mysterious crystals" found in the
Daschle powder by Battelle Memorial Institute were calcium carbonate crystals from the
growth media. The facts indicate that the crystals observed by
AFIP are the same material. Here is an image from the Battelle report showing the element percentages (from Batch 2, Module 13, page 41 of the FBI documents):  Here is what calcium carbonate looks like:  Here's how they look in a form very similar to what was observed in the New York Post powder:  |
| On December 26, 2010, I
printed out a copy of the
February 5, 2010 "report" by the Armed Forces Institute of Pathology
(AFIP) showing their 2001 spectral analysis of the Daschle and New York
Post
powders, along with never before seen images of particles from those
powders. Conspiracy theorists had been using the report for many
months to argue that the New York Post powder contained solid proof of
"weaponization" in the form of inexplicably large amounts of the
element
Silicon. They bizarrely argued that the spectra provided by AFIP
seemed
to show that
the New York Post powder was almost pure Silicon.
To the conspiracy theorists this somehow indicated "weaponization"
because it meant the Silicon must have been deliberately
added. To me, it merely indicated that there was an error or
misunderstanding somewhere, and I never dug into it any further - until
the day after Christmas. It then occupied much of my attention
for the
next week and more. THE
AFIP "PACKAGE"
The so-called "AFIP report" actually contains 2 reports. It appears to be a "package" of documents assembled on February 5, 2010, shortly before the FBI and the DOJ closed the Amerithrax investigation on February 19. Page 1 is the cover page with the Feb. 5 date and a description of the contents of the "package." Pages 2-24 contain a stack of "Scanning Electron Microscopy (SEM) images and Energy Dispersive X-Ray (EDX) spectra aquired 25-26 October 2001." Each unique SEM image page provides the date and time it and the related spectra readings were acquired:
It's clear that the Daschle
samples were analyzed first, then the New York Post samples were
analyzed. And
the next day, some samples from an archive were analyzed for comparison
purposes
- probably for comparison to the New York Post samples.
Pages 25-29 contain "Scanning Electron Microscopy (SEM) images/photographs acquired 25-26 October 2001," according to the cover page. But all the SEM images on those pages are dated 25 October 2001. Significantly, the SEM photographs on those 4 pages are larger than the related images in the previous group, they have different scales which are automatically generated by the SEM, and they contain several fascinating images which were not part of the EDX spectra analysis. (There will be more about those extra images later in this analysis.) Page 30 is a "Certification of Inactivation" that USAMRIID supplied to AFIP to guarantee that the specimens being submitted do not contain any live bacteria. Page 31 is a "Certificate of gamma radiation" showing how the materials were sterilized. Page 32 is a note FAXed from AFIP to USAMRIID with the preliminary results of the tests done on 25 October 2001. It contains just 3 paragraphs. The first paragraph is about the equipment used and its reliability. The second and third paragraphs are as follows (with key sentences highlighted in red): Significant findings for the SPS02-57-03 [Daschle] sample include the presence of silicon and oxygen, which is indicative of silica (SiO2) or silicates (SiO4, etc.). It is not possible to distinguish between silica and silicates (clays). Other components, which are not expected to be signigicant to the question at hand were sulfur, phosphorous, sodium, calcium, and chlorine. It is worthwhile to note that there was no evidence of aluminum in the specimen. The SPS02-88-01 [New York Post] sample had regions which exhibited the same set of elements found in SPS02-57-03 [Daschle], but these tended to be on "large" pieces within the sample. Many of the smaller pieces within the sample exhibited the main peak associated with silicon. It appears that silicon (not bonded to oxygen or other elements) is present in many areas of this sample. Pages 33-41 are a "Memorandum" for the FBI, sent via the Pentagon and dated 26 November 2001. It consists of a 2 page letter and seven attachments. The attachments are less-readable copies of documents that are on pages 6, 7, 11, 17, 19, 21, and 15 of the AFIP "package." The letter to the FBI contains a paragraph that is mostly identical to the first paragraph of the note FAXed to USAMRIID on October 25, 2001, describing the equipment used, but significantly includes a couple additional sentences, the first of which may be very significant. Here is the entire paragraph: 2. Elemental analysis was
conducted using a Thermo-Noral "Vantage" energy-dispersive X-Ray
analysis (EDXA) accessory attached to a Hitachi model S3500N scanning
electron microscope (SEM). The basis for this methodology is that
the electron beam of the SEM induces X-Ray emission from the "inner
core" electrons of the atoms. The energies of the X-rays are
characteristic of the elements from which the X-rays were emitted, so
the identification of the elements in the specimens can be
unequivocal. Typically,
samples are coated with a thin layer of carbon to assist with the
conduction of electrons away from the sample and prevent buildup of a
charge; consequently, all the EDXA data (spectra) exhibit a peak for
carbon. Representative EDXA plots are included.
It appears that AFIP is rationalizing the cause of the carbon peaks, assuming the carbon is a carbon coating on the samples applied by USAMRIID and not actually an element that is part of the original samples. The paragraph describing the Daschle sample is identical to what was sent to USAMRIID, except that they don't say that "It is not possible to distinguish between silica and other silicates (clays)," they say: Distinguishing among the various
possibilities would require additional work with standard materials.
Between October 25 and November 26, AFIP scientists appear to have learned that is is possible to distinguish between silica and other silicates -- if you have "standard materials" to use for comparisons. The paragraph describing the first group of three New York Post samples is worded somewhat differently from what was sent to USAMRIID: The SPS02-88-01 [New York
Post] sample had regions which exhibited
the same set of elements found in SPS02-57-03 [Daschle], but these were generally on the larger
aggregates within the sample. Many
of the smaller pieces within the sample exhibited the main peak
associated with silicon with very little oxygen
as shown in the attached data sheet.
The "attached data sheet" is a copy of page 7 of the AFIP "package." There is no mention of the second sample of 5 particles and data sheets from pages 8 and 9 of the AFIP "package." It's also important to note that the report to the FBI says there was "very little oxygen" associated with the sample, while the note to USAMRIID said, "It appears that silicon (not bonded to oxygen or other elements) is present in many areas of this sample." It appears that the scientists at AFIP had reason to rethink their wording between the writings of the two different reports. The report to the FBI was somewhat less definite about the AFIP findings, and they appear to be a bit concerned about what the carbon peaks may really indicate. The report sent to the FBI also includes three paraphraphs of description for the archive samples sent to AFIP on October 26, 2001. These descriptions are on page 34 of the AFIP package. Most of the archive samples contained aluminum, which was not present in the attack anthrax. Mystery
#1
The Daschle Particles The first thing that jumped
out at
me as I looked at the printed copy of the AFIP report was that the
sample of the
Daschle powder (SPS02-57-03) examined
by AFIP seems to consist of
just five particles of various sizes, none
of which is any smaller that approximately 20 microns by 20 microns.
There
are NO individual spores
visible in any
of the particles. Nor
does any sample look much like a cluster of pure spores (although it's
possible they all
could be clusters of spores). This
is very different from the
way the Daschle powder was described in
Richard Preston's book "The Demon In The Freezer." In that book,
what Tom
Geisbert saw inside his Transmission Electron Microscope (TEM) was
described this way: The view was wall-to-wall spores. The spore were ovoids, rather like footballs but with more softly rounded ends. The material seemed to be absolutely pure spores. Preston's book also says that the sample that Tom Geisbert of USAMRIID took to AFIP for examination in their EDX was already mounted on a "special cassette." Did Geisbert only take unusual clumps to AFIP for examination? Page 25 of the AFIP "package" shows four of the five Daschle samples that AFIP analyzed:  In the AFIP report, the first Daschle particle (P-25-A above) has four (4) spectra readings. Readings 1, 2 and 3 are focused on random areas on the particle, but reading #4 seems to be focused on an area outside of the particle, as if it is a calibration reading for the background. Here is another view of the sample in question with the point test location numbers enlarged and an arrow pointing to the point that was measured outside of the spore:  Mystery
#2
What is being measured? In the spectral diagrams that
accompany the image above, that
fourth reading gives very different results than the first three
readings, but
silicon is still
present, and the reading for Calcium seems to skyrocket.
Is it a calibration reading to determine the elements in the
background? If so,
what does it indicate? If it's not a calibration reading, what is it? Here are the spectral
readings from point #1 (in the center of the sample) and point #4
(below the sample):
Mystery #3 On page 33 of the AFIP package
is
the explanation letter that
AFIP sent to the FBI on November 26, 2001. It says that
“Typically, samples are
coated with a thin layer of carbon to assist with the conduction of
electrons away from the sample and prevent the buildup of a charge;
consequently, all the EDXA data (spectra) exhibit a peak for
carbon.”
This seems to indicate that AFIP didn't prepare the sample and didn't
know how USAMRIID prepared the
sample on the cassette. Was it prepared with a coating of carbon
or
not? Typically
that
would be the case. It appears that AFIP was only asked to analyze
the
samples without really knowing what the samples represented - or even how
they were prepared. And there's no indication that AFIP personnel even knew
what they were analyzing, although they might probably have assumed it
was the powder found in the Daschle anthrax letter. Mystery
#4 Page 25 contains larger
images of
the Daschle particles examined earlier in the report. I also
noticed that the larger image of the D-1 particle above is
identified differently. Instead of being sample SPS02-57-03, it's identified as
sample SPS01-57-03.
The 2 is changed to a 1. Is
it a typo? There's no way to tell. It could represent
a different test number. Mystery
#5  Note the number of the
sample: sps01-57-03.
It also seems significant that there is no spectra information in the
AFIP report about this particle. There are no numbers in the
image to indicate that they even did spectral readings. It's the
most unusual particle among the five Daschle particles, yet there is no
information about it, no mention is made of it, and there is no spectra
of it. If this is truly a picture of
a
particle from the Daschle powder, it is very different
from anything
described in Preston's book. Perhaps it's something neither
Geisbert
nor Jahrling wished to share with someone writing a book. The
only explanation that comes to my mind for
this particle is that it's a piece
of dried agar. If so, then it's confirmation that all the
powders originated as spores grown on agar. If not, what is
it? It looks like
material that is rubbery and somewhat flexible. That is how agar
has been described to me. In a conversation I had with
an
anthrax expert on November 5, he said that scraping bacterial growth
off of agar plates is aways a problem because you always get pieces of agar.
However, later, he also wrote: When you scoop the bugs [spores & bacteria], you slide along the perfect smooth agar surface. I suspect he meant that you always get small pieces of agar, but you occasionally get LARGE pieces of agar. The particle looks like it might be a very small broken piece of agar. But it's a mystery. Mystery
#6
The "Normal" New York Post Particles Pictures of the New York Post powders have been previously shown to the public at the National Academy of Sciences (NAS) presentations in September of 2009. Here is a Scanning Electron Microscope (SEM) image of some of the chunks found in the New York Post letter:  It's these particles which seem to resemble the fifth AFIP image of the Daschle powder. The fuzziness and lack of detail in the AFIP SEM image could explain most differences. Here's a closeup of one chunk from the New York Post powder:  And here is a closeup of the closeup:  There can be no doubt that these images show spores embedded in some kind of material. So, Mystery #6 is: What is the material in which the spores are embedded in the New York Post particles? Pages 27, 28 and 29
of the AFIP package contain
images of some NY Post
(SPS02-88-01) particles. Some of the pictures show particles that look
very much like the particles seen
above in earlier images. For example, image P-28-B below is from
page 28 of the AFIP package. This particle looks like it has
a rough
surface that could
consist of dried spores and/or dried bacteria.
But, it also looks chair-shaped, and I'm not sure what that indicates:
Image P-29-B below (from
page 29 of the AFIP package) might be a particle of similar
components. But, based upon the scale, it is a much larger
particle.
It
seems to show a very solid chunk
of something - probably anthrax spores. But, there also appears
to be layering in the material. It resembles a chunk of fatty
bacon with some slices removed, but it's actually smaller
than the
head of a pin:
It seems very possible that if AFIP had
the ability to produce the finely detailed SEM images seen in the other
images of the New York Post powder particles, the two images above
would show spores embedded in some unknown material, just like the
earlier pictures. Mystery #7 Image P-27-C below is from page
27 of
the AFIP report and is by far the strangest particle in the New York
Post images. Initially, I had no
clue as to
what it was supposed to
represent. It appears to show crystals.
But the crystals are also
stuck together. Or it might just be a pile of
crystals. Could it be that the centrifuge caused all these
crystals to accumulate in one spot? At first glance, I thought
they
might be Bacillus
thuringiensis
spores, but they're too irregular to be Bt spores. And,
the NY Post material
was contaminated with Bacillus subtilis spores, not Bt spores.
Bacillus subtilis spores look very
much like anthrax spores. What could the crystal-like
particles be as seen in this SEM image from AFIP?
On Lew Weinstein's web site, "BugMaster" has been arguing (without providing any detailed explanation) that the spectra indicates there must be Silicon Carbide in the New York Post samples. I tend to agree. Here's an image of Silicon Carbide crystals that I found on the Internet:
There are other images of silicon carbide crystals HERE, HERE and HERE. Here is an image showing the cluster of (presumably) silicon carbide crystals from the New York Post powder along with an image of spores. Both images are at the same scale.  Obviously the crystals have nothing to do with "weaponization," particularly with enabling the spores to more easily aerosolize. The crystals are many times larger and many times heavier than the spores. If there were crystals of silicon carbide in the New York Post powder, why has no one mentioned it during the past nine years? And, why are the crystals so easily distinguishable from the other New York Post powder particles? Why don't we have pictures where the silicon carbide particles are together with the other kinds of particles known to be in the New York Post powder? Or do we? Mystery
#8
The AFIP fibers As inexplicable as the cluster of crystals in picture P-27-C seems to be, things get even more weird in two other AFIP images which are also supposed to be of some kind of material in the NY Post powder. This time we see what looks like frayed pieces of string or fiber amid more particles of silicon carbide:
Could those "threads"
possibly be
pieces of
paper fiber from the envelope or the letter? For all I know,
paper fiber could be a hundred times as thick as what is visible in
these
SEM photographs. Interestingly, however, the shape of the
"silicon carbide"
pieces in
picture P-27-D look very much
like what's in the cluster of "silicon carbide" pieces in picture
P-27-C. And
the scale is the same! Mystery #9
Comments by Bruce Ivins Pondering what these particles and fibers might be, I recalled some comments by Bruce Ivins in a February 12, 2003 interview with an FBI agent. The interesting part of the interview is on page 27 of FBI pdf file #847443: IVINS was recently at Home Depot and
saw the many different grades of sandpaper that they sell which made
him think
about the use of sand in purifying B.a. A pasty block of
spores can be shaken with
sand of varying coarseness to achieve very pure or fine spores.
IVINS advised that 1 - “Specifically, the silicon
carbide surfaces are hydrophilic with hydroxyl termination,”
SOURCE 2 - “Silicon carbide is a hydrophilic substrate, which is a surface that forms hydrogen bonds with water molecules.” 3 - ”it has been recognized that silicon carbide whiskers and silicon carbide particles are both hydrophilic” Ivins was presumably trying to point the finger at Iraq when he made his comments about sandpaper. And mentioning how "Iraq has very fine sand" could be a way of explaining why the crystals in the New York Post powder are so fine (in sandpaper terms, about "1000 grit"). Perhaps more significantly, his comments also prove that he knew of a simple way to dry anthrax spores, a non-USAMRIID way to purify anthrax spores, and he saw a connection to sandpaper.However, I did some tests with fine-grit silicon carbide sandpaper and found that the paper is far too thin to absorb much moisture, and the moisture doesn't seem to be absorbed by the silicon carbide crysals but is more likely caught in cracks and crevices between the crystals. So, the crystals are somewhat hydrophilic but of little use for drying materials via desiccation. Mystery #10
The piece of paper in the New York Post powder To confuse matters a bit, below is an image of what the New York Post Powder looked like to the naked eye:  Note that there is a small piece of paper inside the tube and atop the New York Post powder. It appears too thin to be sandpaper. The best suggestion seems to be that it is a folded piece of "weighing paper" used to scoop the last remaining particles out of the New York Post envelope. It may have been left in the vial with the New York Post powder because microscopic particles from the New York Post powder could be clinging to its surface. It's not much of a mystery and it doesn't seem to have anything directly to do with the AFIP report, but there is no official explanation, so the piece of paper is a mystery. What is most important about this image is that the particles look too coarse to have been created by sanding larger particles. Mystery #11
What was AFIP analyzing? Something is definitely amiss
with the lack of information about the particles in the New York Post
powder which look so much like silicon carbide.. It makes no
sense that the New York Post powder would
contain so much silicon carbide, but no one ever mentioned it
before - unless
it was considered to be evidence that only the anthrax
mailer could explain. And, after Bruce Ivins' death, there was no
one left to explain it. (The police often withhold
information from the public about specific aspects of a case which they
can use to sort out the nutcase publicity seekers who frequently show
up claiming to be the person behind some sensational crime.)  At first glance, it might look like the three points are just randomly selected points on the rough surface of some object. But, there's another view of the same points on page 27 of the AFIP report. And there is an image of a single crystal on page 28. When the scales are made the same, and when combined into a single photograph, this is what you get:  Clearly, AFIP was not examining three random points on a sample, they were analyzing three of the mysterious crystals which, in the image above, appear to be stuck to some unknown, much larger object. But we still do not know for certain exactly what those mysterious crystals are. Nor do we know for certain what the larger object is. It might only be the tape or chip upon which the crystals were placed for SEM viewing, although the background seems far too irregular for that, and there are cracks and crevices in the background material large enough for the crystals to fall into. That makes no sense. Mystery
#12
What are the crystals? The spectra for the three crystals appear to show that they are almost pure silicon:  However, the spectra is misleading due to the different atomic weights of the elements. A scientist who calls himself "Anonymous" on Lew Weinstein's web site put the data from the first chart above into a program that converted the chart data into net weights and atomic weights, and he got this:
So, while the graph seems to show almost pure silicon, in this interpretation the data actually shows that the elements in crystal #1 appear to be only 32.75% silicon by dry weight and 61% Carbon. The difference is even greater when you look at the atomic percentages. As I understand it, the atomic percentages are the percentages of the individual atoms in the crystal. It says there are more than 4 times as many carbon atoms in the crystal as there are silicon atoms. But silicon carbide consists of 1 carbon atom for each silicon atom. So, the crystals cannot be silicon carbide. Or can they? Could the difference be explained by the coating of carbon that AFIP mentioned might be on the samples? People familiar with EDX readings say no, the coating is so thin - just a few nanometers - that it cannot explain the difference. That seems to leave only one other possibility: Mystery #13
What is the background? The AFIP report to the FBI dated November 26, 2001, doesn't even mention the other five particles in the New York Post powder that AFIP tested on October 25, 2001. But the AFIP package includes pictures of those five particles and their spectra. Here's the image of the five particles examined as shown on page 8 of the AFIP package:  And here is the same cluster of particles as shown on page 29 of the AFIP package:  Notice that there is a nearly straight line "crack" running from the upper left corner towards the center. Notice that the surface on the left seems more regular than the surface on the right, and the image from page 8 seems to have a far rougher background than the image above, so "lighting" appears to be a factor. Notice that there appear to be brighter areas at the bottom left corner and particularly on the bottom right corner. This suggests that the background is not a mounting chip or mounting tape. Here are the "slab of bacon" particle along with the two images containing the crystals AFIP examined, with all three images converted to roughly the same scale:  Note that the background in image P-27-B could be part of the rough top-left surface of the large "slab of bacon" particle. And the background in image P-29-C could be part of the smoother surface seen in the center of the "slab of bacon" particle. There's even a crack in the surface where the P-29-C image seems to belong on the "slab of bacon" image. And there's a very long crack in the "slab of bacon" on that same surface. Note, too, that the slab of bacon has a bright edge where the "bacon" would have been sliced off. And image P-29-C has similar bright areas at its bottom corners. But the sizes do not quite match. Could the two lower images be closeups of sections of the upper image? It certainly seems possible - if the problem of size differences can be explained. And it seems very likely that AFIP would have been asked to determine the elements in tiny crystals which seem to be stuck to large particles known to contain spores embedded in dried agar or the clumps of spore material. And, if the background is a large particle of spores and growth material, then it is mostly carbon. Here is what the Daschle particles consisted of:
But the key point is that there is a massive amount of this material in the background compared to the elements in the crystals, therefore the readings for the three crystals in P-27-B could be for the crystals and some of the background. That would explain why there seems to be too much carbon for the crystals to be silicon carbide. There isn't too much carbon in the crystals, there is too much carbon in the area being tested because some of the test area is outside of the crystal and is actually part of the background. But, without confirmation that's just an hypothesis. So, the background is still a mystery, and so is the actual composition of the crystals. Mystery #14
Why are there crystals in the NY Post powder? The crystals are too large to have anything to do with aerosolization or some other form of weaponization using silicon. The composition of the crystals seem to show that the silicon in them has nothing to do with the silicon in the spore coats. So, why are there crystals in the New York Post powder? I don't know. My original hypothesis was that silicon carbide sandpaper was used as a desiccant to dry the spores. But tests done on silicon carbide sandpaper show that it is far too thin to absorb much moisture, and it doesn't seem to readily absorb moisture. It seems to hold water. If you dip a piece of the sandpaper into water, water will get inside the paper and between the silicon carbide particles, but it will not make the entire piece of sandpaper wet via capillary action. It doesn't act like a blotter. The New York Post powder doesn't appear to have been sanded to get smaller particles and to break the spores loose from the growth material. The particles in the powder are far too large for that to have happened. The New York Post material may have been dried on a piece of silicon carbide sandpaper, but, if that was done, the reasons for doing it remain unknown. It's pure speculation. The culprit may have rubbed two pieces of silicon carbide sandpaper together to cause some of the grit to drop into the anthrax material. He may have done that to suggest some Iraqi weaponization process, or he may have done that to add a mysterious "signature" to the powder in order to confuse investigators. Or, he may have done it as another signature like the "hidden message" in the media letters, creating another "signature" he could use if necessary to prove he was the one who created the anthrax letters to the media to warn America of the dangers of a bioweapons attack. I suppose it's also possible that there's an error somewhere, and the crystals weren't really in the New York Post powder when it was mailed, but were accidentally added sometime later at USAMRIID or AFIP or sometime between finding it at the New York Post offices and the time the letter was delivered to USAMRIID. It's also possible that the crystals aren't really silicon carbide. I have an expert telling me I'm wrong in my conclusions about that, but he won't tell me how and where I'm wrong nor how he determined I am wrong. I suppose it's possible that information about those crystals might be the subject of some peer reviewed article for a scientific journal that is still making its way through that process. If I wanted to spend the time on it, I could probably dream up a bunch of other possibilities. *
As always, I'm looking for any information that may help clarify the matters discussed above. I'm also looking for any information which may prove I was right or wrong in some statement or conclusion. |
