Are excess heat and isotope changes in e-cat LENR reactor real? Part 2

Are excess heat and isotope changes in e-cat LENR reactor real? – Part 2

Part 1 of my analysis of the Lugano report[1] covered the e-cat evolution, energy measurements, melting miracles and the chemical compound that was suggested as the source of hydrogen.

In part 2, I will look deeper into the issue of the isotope changes in nickel and lithium, reaction kinetics and the implications of the Lugano report for Industrial Heats´ patent situation.

Isotopic changes in nickel and lithium

Apart from the excess heat, the most remarkable claim is the finding of isotope changes in nickel and lithium.

Samples from the fuel and ash were analysed by state of the art analytical methods such as ICP-MS, ICP-AES, SEM/EDS and TOF-SIMS. The methods are explained in Appendix 1.

The fuel contained three different types of particles. Based on the analytical methods applied (SEM/EDS, pages 43-44), the particles are characterised as

• a first particle is mainly Ni, but it contains also C,O, and Al
• a second particle contains mainly Al and O, with traces of Ni, C and Cl
• a third particle contains Fe and O, with traces of Cr, Mn, Si and Cr

The fuel was found to be basically Ni, in natural isotope abundance (for which partly incorrect numbers are given in the report), and some other particles which contain substantial amounts of iron oxide and aluminium oxide. The contents of Li and H in the particles cannot be detected by this method. They are probably included in the second particle, and the oxygen could be (partly) due to improper handling of LiAlH₄ (see part 1).

In the fuel, according to ICP-MS / ICP-AES analysis, the total Ni content was found 55%, Al content was found 4.4% and Lithium was found 1.1%.

The ash, extracted from the reactor after the test was finished, has two different types of particles, characterised as

• a first particle is mainly Ni, but it contains low trace amounts of O, C, Si and Al
• a second particle contains C,O and Si

Remarkably, the total non-Ni content of the ash was found only ~ 4%! So, the ash was found to be basically pure nickel, but in a much higher concentration than the fuel – the total Ni content of the ash was found ~ 96 % – and Fe completely disappeared, along with some other elements.

In the Ni particle of the ash the authors found what would be a scientific sensation: A remarkable isotopic change from Ni-58 (67% found in the fuel; 68% is the natural abundance, reduced to 0.8% in the ash) to Ni-62 (98.7% found in the ash; 3.6% is the natural abundance).

Also, Li-7 (91.4% found in the fuel; 92.5% is the natural abundance) shifted to Li-6 (92.1% found in the ash; 7.5% is the natural abundance).

A change of neutrons betweens elements, as it is indicated for Li and Ni, and transmutation of Fe and Al to other elements would be a nuclear reaction. Neither Cu, nor Zn could be detected, in contrast to earlier claims by Andrea Rossi. The data with respect to Li and Ni isotopic changes are shown in the following table.

The original theory of a Ni to Cu transmutation, basis of Rossi´s patent application, is not supported by the experimental data, as it was never supported by earlier results.

Today´s knowledge of nuclear physics cannot explain these results, and unfortunately a new theory was not offered by Rossi and the Italo-Swedish research association.

Ni-62 is a stable (non-radioactive) isotope of nickel. It is both naturally occurring and produced by fission. Ni-62 is the most stable Ni isotope, and it is the most tightly bound nuclide, with a binding energy of 8.7945 MeV per nucleon[2].

What happened to the disappeared elements?

Very interestingly, the analysis of the fuel revealed additional elements which disappeared in the ash: C, Ca, Cl, Fe, Mg and Mn. Especially the disappeared high Fe content is unbelievable. This observation strongly suggests that the samples were not representative. The disappeared elements could be due to non-uniform composition of the ash, but even then traces would probably still be detectable. Or there could be other explanations.

As mentioned in part 1, Rossi changed the reactor to alumina (Al₂O₃ ). But alumina has some further implications. Sintered alumina is porous and has a permeability to gases which many play a role at extreme conditions, such as in the case here with high pressures and high temperatures in the range of 1200-1400 °C. Oxygen diffusion[3], hydrogen permeability[4] and inclusion of elements such as Ti in the defect structure of the Al₂O₃ corundum structure[5] are known properties.

Hydrogen may stay in the reactor by forming a nickel hydride faster than diffusing out. This may be a reason why a hydride was applied as a source of hydrogen, as suggested in the Lugano report, rather than hydrogen gas.

The porosity of alumina may explain the partial disappearance of some elements. But it cannot explain the complete disappearance of all the other elements.

So, are we supposed to believe that all the other elements of entirely different chemical and physical properties- C, O, Cl, Mg, Mn, Fe – would have converted to Ni-62, the nucleus with the highest binding energy, without any detectable radiation? This is totally unrealistic and absurd. Other cases of reported transmutation typically describe a mixture of newly formed elements but not a uniform conversion to only specific isotope of one element. It sounds like the alchemists are back. Too bad that Rossi could not make something more useful such as gold.

Of course, there is another explanation which seems to have a higher probability: Samples of fuel and ash came from different sources. Either the ash is not the real ash, or the fuel sample wasn´t the fuel that was used in the experiment. But that would mean the samples had been manipulated.

Handling of the samples

The ash sample contained 98.7% pure Ni-62, similar to commercially available material. Both Ni-62 and Li-6 can be procured from specialist chemical suppliers.

Critics have raised their concern that the sample could have been manipulated. On page 7 the report clarifies that the Andrea Rossi, a controversial character and inventor of the e-cat device, actively participated in the experiments:

“Rossi intervened to switch off the dummy, and in the following subsequent operations on the E-Cat: charge insertion, reactor startup, reactor shutdown and powder charge extraction.”

 It is a mystery why the examiners compromised the integrity of their research by allowing the inventor to intervene in the experiment. On this basis the Lugano report can hardly be considered as „third party independent“. Critics believe that Rossi´s magic hands are vital for the success of the experiment and he could have switched samples or salted the ash of the reaction. It could be also conceivable that the analysed fuel was not the same material as the fuel that was put in the reactor.

In this context it is important who attended the procedure of handling samples. Rossi was involved and as it seems, and only one of the scientists. On page 7 the report says

”the powder …..had been….weighed (about 1 g) and then transferred to a test tube so that Bianchini could perform radioactivity measurements on it,……..lastly the contents of the test tube were poured inside the reactor, in the presence of a member of the experimental team”.

If phrased correctly, this sounds as if only one of the scientists attended and witnessed the important step of introducing the fuel into the reactor.

Does this means that all the other scientists did not attend and cannot witness how the fuel was introduced before the reaction started? It does not say who was the “member of the experimental team”. But it would be interesting to know who is the only witness.

On the same page it is stated “all phases of the test were monitored directly by the collaboration”. In this case, “the collaboration” would refer to one individual witness only. I would not be totally surprised if this particular individual was the same person who provided the equipment to measure energy input and output. This means that for a manipulation it would not require a grand conspiracy involving all the scientists.

I am stressing the point because Rossi manipulated samples before when providing ash samples to Prof. Kullander of Uppsala University for elemental analysis. Rossi admitted:

“AS THESE SCIENTISTS CORRECTLY SAY, I SUPPLIED THOSE SAMPLES, IN 2011 (TO PROF. SVEN KULLANDER), AND I GAVE A SAMPLE FROM WHICH THE COMPONENTS, THAT AT THOSE TIMES WERE NOT DISCLOSABLE, HAD BEEN EXTRACTED, BECAUSE NOT YET PATENTED. I CLEARLY WARNED PROF. KULLANDER OF THAT. SO WE ALL KNEW THAT TOSE ANALYSIS COULD NOT BE TAKEN AS COMPLETE, BUT JUST AS A FIRST APPROACH TO THE PROBLEM. THE COPPER FOUND WAS PROBABLY AN IMPURITY AND I MADE CLEAR THIS SUSPECT OF MINE . IN THAT CASE THE SAMPLE HAD NOT BEEN WITHDRAWN FROM A REACTOR BY A THIRD PARTY AND I HAVE NO DIFFICULTY TO SAY, AS I DID WHEN I DELIVERED IT, THAT I HAD TAKEN OFF FROM IT THE PARTS THAT I WANTED NOT TO DISCLOSE.”[6]

Kullander found nickel and copper in natural isotope ratios which contradicted the claims of nuclear reaction. Unfortunately, Sven Kullander deceased and cannot further comment on the issue.

Prof. Stephan Pomp of Uppsala university, a known critic of his alma mater peers from Uppsala university, and their favourable endorsement in previous papers, made the point „it is totally inexplicable to me, how the authors cannot see the most obvious and by far most likely conclusion of the fuel analysis; that they simply have been fooled.”[7]

More Issues related to isotopic changes

Provided that the isotope shifts would be real, there are many questions unanswered such as

• why did Ni-64, a stable isotope and a heaver isotope than Ni-62, disappear ? (from 1% to 0%)
• as intermediate stages, radioactive isotopes of Ni (and other elements) would have been expected. Why are no such elements found and why is no radiation measured?
• is Ni-62 really the end product of the process?

Finding almost pure Ni-62 at the end of the experiment has further implications.

Unexplained reaction kinetics

Providing that the sample of the ash would be representative, this would strongly suggest that Ni-62 is the product of the reaction, not the reagent. However, if Ni-62 would be the product of the reaction, and the conversion would be almost completed, then the question is, why does the reaction rate still accelerate, and not decline, as it would be expected towards the end when almost the entire fuel is consumed (see chart below: power production).

Either the net power production chart is wrong, or Ni-62 is not the product of the reaction.

This is basic reaction kinetics. A reaction rate is proportional to the concentration of the rate determining reagent. With almost complete conversion, providing that Ni-62 is the end product, the concentration of whatever is rate determining must be very low. In other words, the fuel almost burned out, but the power production was still increasing. This is impossible, unless the sample was not representative (in this case the conversion could have been considerable lower than it appeared) and other particles (remaining fuel or intermediates) were unaccounted for. Or other reactions could be rate determining involving other reagents and products.

Possibly there could be other fusion reactions, involving hydrogen and helium, which is more difficult to detect and no attempts have been made to detect it. Hypothetically, these alternative reactions could run faster in presence of Ni62-hydride, and this could explain why the reaction rate did not decline. But unfortunately these elements were not analysed further in the Lugano e-cat report (why not?); only a general remark is given that no deuterium was found. The state of hydrogen in metal hydrides, for example, can be analysed by ¹H-solid state NMR spectroscopy[8]. Helium would have escaped from the reactor, under the given circumstances.

Since the sample was very small (several mg of a total 1 g fuel charge), it is possible that the finding of the Ni is not representative for the whole fuel, and there may be other particles, still active fuel, with lower degree of Ni isotope conversion,. On the other hand, the report also states on page 29 that “the spent fuel was found inactive”, but it is not clear on what basis this judgment is founded, since the reaction was not continued subsequently.

On page 54 (fuel and ash was analysed by ICP-MS / ICP-AES) reveals not only the obvious difference in appearance of the ash, and it shows only one sample from the ash in the table.

Apart from the question what happened to the third sample which is mentioned but no data are shown, we must remember that the ash was not homogeneous. It is disappointing why the scientists did not examine further samples of the ash, to get a better view of the entire picture, considering the questions raised above, in the view of the extraordinary claims. But is seems, in this study, they got “only a few granules” to examine. It is inexplicable that the scientific team stopped at this point and would have accepted such constraints, and this weakens the scientific value of the whole report.

It is even more disappointing that more tests are not planned. Science is always about replication, if no repetition of experiments happen, no good science can ever be established.

Of course, sample manipulation could be an alternative explanation for the reaction kinetics, the disappeared elements and the isotopic shifts.

Why did the role of Ni-62 change?

It should not be forgotten that three years ago Mr. Rossi made totally contradicting statement regarding the role of Nickel-62. He wrote in his blog

December 6th, 2011 at 3:45 PM

„As I have explained many times, we use Ni enriched of 62 and 64 Ni, which are the sole to react, and 63 and 65 Cu are stable. Our process has been developed upon a theory that became stronger in time, based on the results of the thousands of our tests we made with our apparatuses. At this point we have a solid theory which is leading our R&D, making progress by the day. The problem is that the theory leads directly to the industrial confidential IP and since we have not a granted patent we deem opportune not to disclose the theory.”

But now there is no evidence for Cu is found in the ash. No evidence for enriched Ni-62 and Ni-64 in the fuel is found either.

October 21st, 2011 at 3:22 PM

„We enrich Ni 62 and 64 isotopes, but this is not an effect of the operation of the reactor.“

Mr Rossi seems to be surprised himself. He said in an interview[9]

“This report is no doubt very interesting and we are studying it because, as you probably know, there is a surprising result regarding the Nickel-62 in particular, and we are studying it because we are strongly directed, under a theoretical point of view, to understand these kinds of results that was unexpected.”

October 25th, 2014 at 3:10 PM

“As a matter of fact, the enrichment system is the process made by means of the ECat. Nevertheless the results from the test have gone well Beyond what we found before during our internal R&D. As I said, now we are studying how to reconcile……”

Absence of radiation

No radiation, neither alpha, beta nor gamma rays have been detected.

Levi et al. [1] ruled out a transmutation to copper which is the proposed process of Rossi´s patent. They wrote on page 29 “for example the reaction p + ⁵⁸Ni -> ⁵⁹Cu + g and ⁵⁹Cu decaying back to ⁵⁹Ni via ß⁺ emission releases 3.4 MeV. Even if that particular reaction is excluded, since no gammas are observed……………the absence of any nuclear radiation from the burning process is presently an open question, and has to be understood.”

Bound neutron tunnelling?

The scientists of the Lugano report [1] did not offer a theory to explain isotope changes and excess energy. But a physics student from Uppsala university, Carl-Oscar Gullström, proposed “bound neutron tunnelling” to explain how the e-cat works[10], a theory which was eagerly absorbed in e-cat related internet forums.

Prof. Pomp of Uppsala University commented“to claim that this explains the E-Cat is, hmmm, pretty far-fetched to use a slight understatement”.

Tunnelling is a well understood basic principle of quantum mechanics. The question is how large is the probability for tunnelling. Not going into the theoretical aspects and various mistakes of the paper, Gullstöm´s calculations obviously do not explain the claimed excess energy, they are orders of magnitude off. He wrote:

“this suggest that approx. 2 g nickel was burned during the test…..using the nickel weight abundance in the fuel gives an approx. amount of nickel of 100g. This means that 2% of the Ni in the fuel was burned.”  

But the total fuel was only 1 g, according to the report.

The Lugano report does not support the e-cat patent

Some people may interpret the contradictory statements as intentional misdirection. But there are a few problems with this theory.

Ni-62 now “surprisingly” seems to shows up as the sole reaction product. However, Ni-62 is an essential reagent in claim 1 of the sole patent, and affects all patent claims. A reagent is not a product. This is a show stopper for the patent.

More specifically, Rossi changed in 2013 the claims of his European patent application[11], the only known patent family in the field by the inventor, which claims now (the US patent claims are different and more general) [12]

“….exothermal reaction of nickel and hydrogen,…..and that said nickel powder of a nickel isotope having a mass of 62”

This means the inventor assumed Ni-62 to be the reagent, not the product. If Ni-62 would be the product of the reaction, the European patent claims of the sole patent known would be useless.

But there are more serious problems with the patent, not even stressing the fact that the patent outlines a transmutation to copper without any evidence. The main issue is: The current models of the hotcat are operating clearly outside the claims of the patent, in several aspects:

1. The main claim of the particular patent assumes a metal (US) or copper (EP) tube as reactor which isn´t used anymore. The Lugano hotcat[1] is made of alumina (Al₂O₃), a ceramic material. Alumina ceramic is not a metal, and certainly not in any way related to copper.
David French, a retired patent attorney who frequently contributed to a cold fusion website, correctly commented on Rossi´s US patent examination[13] “these independent claims stipulate for the presence of a metal tube. In the absence of such a component, a competing construction would not infringe these claims. For example, if a ceramic tube were employed, it would not fall under the language of the claim”. This is the case in the Lugano-hotcat.

2. Temperature: at 1200-1400 °C a copper tube (mandatory reactor material in EP patent claim) would melt. The melting point of copper is 1085 °C which would per se limit the upper temperature level to this level. Besides, the preferred temperature range is given as 150-500 °C; the current hotcat device is far above this range.

3. No hydrogen gas is injected in the reactor tube as it is requested by the patent claims

4. Nanometric nickel is mandatory, too. The particle size of the fuel looks larger than 50 micrometers (Fig.1 on page 43 of [1]), though with some smaller substructures. “Nanometric” normally means a range of 1-100 nm; 100 nm are 0.1 micrometer.

All these points together, there is no doubt that the Lugano test is outside the scope of Rossi´s patent. So, if the thing is real, the developers would need urgently fresh patent applications with fundamentally reworked descriptions and claims.

In other words, the purpose of this testing was certainly not to defend the said patent, since the operating conditions were clearly outside the scope of it. This means the Lugano hotcat[1] will not provide any support for ongoing patent examinations, at least not for the sole patent what is known till date.

But according to Industrial Heat´s press announcement[13], more patents may be in the pipeline. They claimed „since acquiring Rossi’s technology, IH has engaged in a broad-based effort to protect it by preparing numerous patent applications related to the core technology as well as associated designs and uses.“

Of the “numerous patent applications “ not even one is known till date. Time will tell. It is strange enough that till date no further patents have been disclosed, after years of “improvements”, and 17 months after the publication of [2] – patent applications are laid open to the public 18 months after filing.

As pointed out, the Lugano test is not supporting Rossi´s patent. To achieve this, IH should have provided a device that is inside the claims of the patent, and operate it under conditions as specified in the patent. They clearly failed to do so.

On the contrary, things are now getting worse. All published papers, demonstrations, presentations and blog contributions, including own ones, set a prior art which is potentially critical for new patent applications. Rossi and Industrial Heat face patent risks which will make it more difficult to file new patents in the future.

Another issue of concern for IH should be that the involvement of Li-6 in alleged LENR processes is not new. It is prior art since 2011, linked with the patent disclosure of Rossi´s competitor Piantelli[14].

Summary

Overall, the Lugano report [1] is not convincing, and the circumstances remain suspicious.

1. The Lugano report contains various loopholes, technical weaknesses and lacks experimental details, which undermine the credibility of the whole report.

Even Michael McKubre, a long time LENR advocate makes this point “There is curious inattention to detail—surprising for a document as delayed, anticipated and important as this……… this report has problems at several levels that render direct interpretation difficult or impossible without further information and clarification. This is a shame and undoubtedly a source of great frustration …..”[25].

25 years after the Fleischmann and Pons announcement of a table top cold fusion, the established scientific community largely considers the field of LENR as pseudoscience. With the Lugano report this is not very likely to change.

2. No truly independent test was ever allowed. The fact that Rossi and his associates were always involved in all experiments, is highly suspicious.

Some may say the reason for being so secretive is intellectual property. But what I see is a patent application contradicting the experimental data, and no serious intention of the patent holder to establish the operability of the invention.

3. Rossi never allowed testing of the same device twice. The design of the device, obviously R&D prototypes, always changed. Replications of previous experiments were never intended. Why not test the device that is offered in the market since 2011, such as a module of the 1MW industrial e-cat?

4. No convincing theory is provided that would explain the experimental findings. It is unconceivable that regulators would give green light to a nuclear device which is not even understood.

It is disappointing that no further research is allowed by IH and Rossi. But science always includes replication, and without replication, no science can be established.

These things combined, one may ask what is the purpose of these papers [1,15] ? It´s not science, it doesn´t help the patent, so why are they doing this? To support sales and marketing activities? To attract more investor funds?

Prof. Pomp called his post [6] „The cat is dead“. BUT CATS HAVE NINE LIVES.

Appendix 1: Analytical methods

	Technology explained	Detection of hydrogen /deuterium	Detection of lithium
ICP-MS	Inductively coupled plasma (ICP) mass spectrometry (MS) is an analytical technique used for elemental determinations.Light elements such as C,H,O,He cannot be detected by ICP-MS[16].	No	Yes
ICP-AES	Inductively coupled plasma (ICP) atomic emission spectroscopy (AES) is an analytical technique used for the detection of trace metals in which the intensity of this emission is indicative of the concentration of the element within the sample.Light elements such as C,H,O,He cannot be detected by ICP[14]	No	Yes
SEM/EDS	scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDS) provides qualitative, or with adequate standards, quantitative analysis of elemental composition with a sampling depth of 1-2 microns.The detection of light elements such as C,H,O,He is difficult to obtain with standard energy-dispersive X-ray spectrometry (EDS) and usual proceedings for SEM	No	No
TOF-SIMS	Time-of-Flight Secondary Ion Mass Spectrometry provides is used to determine the elemental composition and molecular species on a surface of a particle. All the elements in the periodic table, including hydrogen, can be detected	Yes	Yes

 

References and footnotes

[1] Levi, G. et al. Observation of abundant heat production from a reactor device and of isotopic changes in the fuel

[2] M. P. Fewell: The atomic nuclide with the highest mean binding energy, American Journal of Physics, (1995), DOI 10.1119/1.17828.

[3] Hine,N. et al. , Electronic Structure Discussion Group, 3.7.2009: Bulk Diffusion in Alumina: Solving the Corundum Conundrum

[4] Roberts,R. et al., : Hydrogen permeability of sintered aluminium oxide, Journal of the American Ceramic Society 62 , No. 9-10, 495

[5] Hine,N.D.M. et al: Point Defects and Diffusion in alpha-Al2O3, International conference on QMC (2009)

[6] Prof. Stephan Pomp´s blog: Mr Rossi, I admire you

[7] Prof. Stephan Pomp´s blog: The e-cat is dead

[8] Ell,J.M. Dissertation Universität Darmstadt (2007)

[9] Coldfusionnow.org: Andrea Rossi on 3rd-Party Report, Industrial Heat, & 1MW Plant — New Interview

[10] Gullström,C.O.: Low radiation fusion through bound neutron tunneling

[11] European patent EP08873805

[12] Claims of the European patent application EP08873805, currently under examination, revised in 2013::

1. A method for carrying out an exothermal reaction of nickel and hydrogen, characterized in-that said method comprises the steps of providing a copper tube, introducing into said copper tube a nanometric particle nickel powder and injecting into said copper tube a hydrogen gas having a temperature much greater than 150 °C and a pressure much greater than 2 bars, and that said nickel powder is a powder of a nickel isotope having a mass number of 62.

2. A method according to claim 1, characterized in-that said hydrogen temperature varies in the range of 150 to 500 °C

3. A method according to claim 1, characterized in-that said hydrogen is injected into said tube under a pulsating pressure.

…….

The US patent claims are

CLAIMS

1. A method for carrying out an isothermal reaction of nickel and hydrogen, characterized in -that said method comprises injecting hydrogen into a metal tube filled by a nickel powder, even of nanometric dimensions, or nickel granules or bars, in a high temperature and pressurized hydrogen gas saturated environment, thereby generating energy.

2. A method according to claim 1, characterized in that in said method catalyzer materials are used.

3. A method according to claim 1, characterized in that said high temperature is preferably from 150 to 500⁰C. 4. A method according to claim 1, characterized in that said hydrogen is injected into said nickel powder filled metal tube at a pressure preferably from 2 to 20 bars.

…….

[13] French,D.: Status Report – Rossi Pending US Patent Application

[14] Patent application US2014/0098917, claim 2, priority 26.4.2011

[15] Levi, G. et al: Indication of anomalous heat energy production in a reactor device containing hydrogen loaded nickel powder

[16] The ions formed by the ICP discharge are typically positive ions, M+ or M+², therefore, elements that prefer to form negative ions, such as Cl, I, F, etc., are very difficult to determine via ICP-MS