me356: Photos of AURA control unit

I know little about mass spectroscopy. However, years ago, people who know a lot told me that EDX does not work reliably with samples of material such as powder or other particles not compact or electrically conductive. Here is an on-line discussion that confirms this:

https://www.researchgate.net/p…analysis_of_powder_sample

I learned this when I saw results from an EDX analysis of powder that seemed to be off the wall and useless. That was my impression, and that is what the mass-spec people confirmed.

The photos from Me356 appear to show fractal material that seems to be loose or not even attached to the substrate, so the results may be questionable. I cannot judge, but I think another method would have to be used to confirm the analysis.

Quote from axil

Me356 is using a scanning electron microscope (SEM) to look at his fuel

Apparently it is an SEM with an EDX built in.

https://steemit.com/science/@m…l-and-nickel-foil-samples

The link contains scanning electron microscope (SEM) images of the cavitaion prepared fuel used by the indian reactor (ECCO) kindly taken by me356.

me356 must have his own SEM.

There look to be whole ecosystems in there and even beautiful fractal structures.

This micrograph is very close to the ones that em356 has already shown us depicting his fuel. The ECCO reactor fuel also shows transmutation of carbon in fractal patterns,

The light ovoid decoration patterns that contains the fractal metal transmutations looks like carbon isotope change from subatomic particle (muons, pions?) emissions from the process that is producing the metal nanowire tracks.

me356 has his own SEM/EDX

I guess there are a few nanotools out there that can be bought for korunas

Lots of research labs have closed down.

Quote from JedRothwell

I know little about mass spectroscopy. However, years ago, people who know a lot told me that EDX does not work reliably with samples of material such as powder or other particles not compact or electrically conductive.

I think that is an unfair characterization of EDX. If you can image with the microscope, avoiding charge build-up, then EDX will in general be a reliable indicator of what elements are present. EDX will only provide an approximate measure of composition ratios and really provides no information on molecular structure - just what elements are present. To deal with charge build-up, many SEMs will have the chamber at an air or argon pressure of about 7 torr, compared to the normal ultra-high vacuum that must be maintained in the column. This prevents measurements of secondary electrons, and of course, you may detect oxygen, argon, and nitrogen in the x-ray spectrum.

Most samples are placed on a conductive carbon sticky tape which will cause carbon to show up in every analysis - sometimes a lot. This makes it difficult to determine if carbon is really in the spot probed by EDX or not. Generally, you have to ignore the carbon in the analysis.

Also, EDX works by having the electron beam knock off electrons from the atom and when the electrons are restored, it gives off the characteristic photon spectrum of the element. The characteristic photons of low atomic weight elements are very low energy and don't make it through the window on the x-ray sensor. You need a special x-ray sensor window (polymer) to be able to detect down to boron (Be windows are more common). Seeing Be or Li is nearly impossible with any sensor window - you need a sensor without a window and a high vacuum system to seen Be or Li.

There is a caveat: if your sample is radioactive, it can generate spurious lines in the acquired x-ray spectrum that are not the characteristic lines of anything. The analysis software may not deal with these extra lines gracefully and may say that an element is present that is not actually there. I have never seen this happen.

Quote from BobHiggins

There is a caveat: if your sample is radioactive, it can generate spurious lines in the acquired x-ray spectrum that are not the characteristic lines of anything. The analysis software may not deal with these extra lines gracefully and may say that an element is present that is not actually there. I have never seen this happen.

The EDS however has such fine resolution that I'm not sure how it might react. I would lean towards the detector being swamped with decay-related X-rays in some channels if the specimen has appreciable radioactivity.

I have seen the decay-related peaks many times using XRF for bulk concentration analyses. The lines due to radioactive decay are not spurious, however. They are consistent. One might (uncautiously) say they are characteristic of the radioactive source, but that is too easy confused with the Characteristic X-rays that the system normally relies on. In moderate and higher concentrations of a given element there are typically a large alpha and also a smaller beta peak channel located right next to the alpha channel, on the higher energy side. The smaller beta peak is absent in the decay-related lines, which helps to distinguish them from the elemental characteristic lines. Rhodium is one element that often reports in uranium-rich samples tested by XRF results, for example, and is due to a decay peak and not the actual presence of the element.

Smaller "shoulder peaks" sometimes also occur on either side of the main peak, when some elements in a sample have very high concentrations, which the detector software often falsely interprets as being related to some other element.

Quote from BobHiggins

I think that is an unfair characterization of EDX. If you can image with the microscope, avoiding charge build-up, then EDX will in general be a reliable indicator of what elements are present.

I wouldn't know, but years ago Mizuno sent a powder sample to two or three different labs for mass spec analysis. I recall they used EDX. The answers were COMPLETELY different for the same sample. So obviously it did not work. They advised him that an analysis of non-conductive material is problematic.

Ed Storms also told me that. He has an SEM with a built in mass spec, in his house. He has a lot of stuff.

"He has a lot of stuff"

Does Ed the nano builder have a gold coating nanotool?

Does the 5-10 nanometer layer interfere with good EDX of LENR catalysts?

https://www.microtonano.com/TI…an-SEM-sputter-coater.php

Quote from bocijn

Does Ed the nano builder have a gold coating nanotool?

Yup. That is essential for some kinds of samples. Such as flies. (Insects; a biologist told me that.) However, it does not work with powder.

Mizuno found that surface oxygen increased with excess heat.

Perhaps surface oxygen is a better assay for LENR activity than excess heat

But the assay still requires gold sputtering on his nickel wires.

Without somebody like Ed these EDX analyses might cost a yen or two

Quote from JedRothwell

Yup. That is essential for some kinds of samples. Such as flies. (Insects; a biologist told me that.) However, it does not work with powder.

Gold coating is not required for analysis of non-conductive samples in all SEMs. Modern SEMs have a charge reduction mode that puts ~7 torr of air or argon in the sample chamber to allow charge to bleed off a non-conductive sample. The column of the SEM is still kept at ultra-high vacuum. In charge reduction mode, gold coating is not required for a conductive or non-conductive sample (or your fly). There is no problem with analyzing powder on EDX, but EDX only provides an approximate quantitative atom analysis. SIMS would be much better and would use a mass spectrometer.

A SIMS is probably a bit north of $10.000.

I guess they pick up isotopes like O-18, C-13.

If one were to go for Helium-4 as a routine signature for LENR activity

perhaps a $2000 visible region spectrophotometer would suffice?

Quote from bocijn

If one were to go for Helium-4 as a routine signature for LENR activity

perhaps a $2000 visible region spectrophotometer would suffice?

MKS sells a high resolution mass spectrometer RGA for the mass range of 1-6. It is probably in the $15k range. It is the same quadrapole mass filter as their regular RGA, but run at a higher frequency. Mass spectroscopy of these gasses has to deal with the other molecular interferences in the measure. For example, measuring 4He, one has interferences of 2D2, and HT (and there are others) which have masses of ~4, but not exactly the same as 4He. A high resolution 1-6 m/e RGA can separate the 4He from the interferences.

How about Xenon as signature for some kinds of LENR.

Mizuno,1996, found

"Gaseous Xe was noteworthy because it was so abundant. Xenon is particularly unlikely to be a contaminant because

metals do not absorb noble gases, and because the cathode was degassed in a vacuum at 473K for 20 hours."

lenr-canr.org/acrobat/MizunoTanomalousia.pdf

I think Xenon has a distinctive UV emission at 236 nm wavelength.

Anything new from me356?

He seems to be more competent and productive than Rossi. Hope he makes it first to the market...

I also wanted to ask if me356 is aiming for large units that are more suitable for electrical production rather than many small units assembled together?

If possible is me356 getting COPs near or better than Rossi?

I still believe that Ni, and Ni powder in particular, is a likely key to higher power LENR. I have not been idle in the last 4-5 months. I am getting setup for treating of Ni powders in an RF H2 plasma (13.56 MHz, 5-40W) - sort of like what is being done by Mizuno and probably me356 (since what he does is just a guess). The changes in the Ni granules will be documented over the course of treatment with SEM observation (I am bringing an SEM online in my lab in about a week). This has required new lab hardware and reworking of some lab facilities. Hopefully plasma treating will begin before the end of the year.

After doing some maintenance aperture replacements in the column of my SEM, it is working pretty well. I have taken a first set of survey images of the as-supplied Hunter Chemical AH-50 grade Ni powder that I have been using. I made a Ted Pella pin stub sample holder adapter, and hopefully this afternoon I am going to take comparative images of the Ni powder A. Parkhomov uses. My SEM is a Hitachi TM3030plus. It doesn't have EDS yet, but I hope to add that in January if I can scrape together the funds. Enclosed are some of the AH-50 images. The images are taken at 15kV using both the SE detector and Backscatter detector in a combined image mode in high vacuum within the sample chamber (since everything was conductive). The powder is adhered to the aluminum sample pedestal with conductive black tape. While this SEM doesn't have the ultimate resolution of late model full size SEMs, for a tabletop SEM, the resolution is adequate for this work - the resolution is better than the 20 year old physically large full size SEM we had at the company I worked for previously. The only facility requirements for this SEM are a sturdy tabletop and an ordinary wall plug (~500W).

I have looked as EDS options and I find that IXRF (http://www.ixrfsystems.com/cat…s-elemental-analysis.html) has an excellent solution. Their hardware is as good as Bruker and their software is better. Plus, IXRF provides free lifetime software updates but you have to pay a lot for updates from Bruker. The cost of the IXRF EDS option for the TM3030plus is 2/3 of the cost of Bruker's EDS option.

Thanks for the link. I bought my SEM from the regional Hitachi field representative - it was her demo model; so not new. Hitachi is introducing their 4000 series and she will be demonstrating that model beginning in 2018.

We should put clearly, that fancy pictures of various "ash" samples present in no way substitute for serious LENR research involving calorimetry.