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First independent Isotopic results [UPDATE#2 - Second Earthtech Ni Isotopic report agrees with University of Missouri results]

Scritto da Robert Greenyer on .

Without too much comment so that you can all see it fast - the very first isotopic data sent to us of one of the independent testing parties.

Note we do not know which sample is what - but there is

- a sample of GS3 fuel

- a sample of GS3 ash

- a sample of GS2 ash

Ash samples were fully extracted and mixed before sample selection

before all the data is in and the index key is released - see what you think is what.

https://goo.gl/6bvbjl


UPDATE#1 - MURR, University of Missouri isotopic analysis of Ni and Li

The analysis is for Parkhomov Ni and LiAlH4 as well GS2 Ash and GS3 Fuel/Ash (which contained Parkhomov Ni) and was conducted at http://acg.missouri.edu

Results are

https://goo.gl/mfcNMf

We thank the University of Missouri for conducting this Assay.

We know from previous EDX that Parkhomov LiAlH4 contains Chlorine, but in terms of 7Li and 6Li, both US sourced and Parkhomov LiAlH4 both have near-natural isotopic ratios as given on wikipedia.

Both were 7Li 92.6 : 6Li 7.4 to 1dp

Here are the testers comments:

"Attached is a spreadsheet with isotopic results and approximate elemental concentrations.

The basic message of the results is that, to the ability of our quadrupole ICP-MS to measure, the Li isotope ratios are effectively the same in all four samples that contain major amounts of Li.  We do not have a “natural” Li standard with certified isotope ratios, and since Li is a light element, the ratios can vary a bit in nature.  Thus I had to assume a natural 7Li/6Li ratio in the standard and compare its isotope ratios with those from the samples, keeping the Li in the standard and sample solutions at an approximately constant concentration.  Effectively, it appears that (7Li/6Li) in all samples is a bit higher than the standard.

Also, the Ni in all samples appears to be isotopically natural.  All ratios measured are within one standard deviation of natural Ni, except for one (61Ni/58Ni) measurement in Vial 46, run 2, which was within two standard deviations of the natural ratio.

Please keep in mind that the elemental concentrations were measured without internal standard and may only be considered approximate.

Below are some method notes:

 

  1. The LiAlH4 sample (52.2 mg) was reacted with 1 mL ultrapure water (H2O).  The resulting suspension of white solids was dissolved by adding 1 mL of conc. HNO3 (Optima grade).

  2. To the aliquots of samples in brown vials (approx. 30 mg each) was added 1 mL of H2O, since they were thought to contain LiAlH4.  No reaction was observed.  2 mL of HNO3 was added and samples warmed to 90C for 30 minutes to digest solids.

  3. The sample Vial 38 still contained fine greyish solids after digestion.  It was heated for a longer period of time (about 1 hour) at 90C and no progress was seen in the dissolution of the solids.  The supernatant solution was analyzed regardless.

  4. The Ni carbonyl sample (112.2 mg) was digested in 2 mL HNO3, warming to 90C to speed the reaction.

  5. All samples were diluted with water and the exact mass of solution measured.

  6. Further dilutions were performed as needed using 3% HNO3, in order to make the concentrations of Li or Ni approximately equivalent to the concentrations in the standards.  Separate standards containing Li and Ni were prepared at varying concentrations.

  7. The isotope ratios were measured using bracketing standards in several separate analyses using a PerkinElmer NexION 300X:

    Ni isotopes were measured at ~250 ppb Ni in KED (Kinetic Energy Discrimination) mode.

    Li isotopes in LiAlH4 were first measured at 1 ppm Li in standard mode, with the deflector lens detuned to keep the signal measurable by the pulse counting detector.

    Li isotopes were measured in LiAlH4 and the Vial 34, 38, 46 samples at 100 ppb Li in standard mode, with the nebulizer gas flow detuned slightly to keep the signal measurable by the pulse counting detector.  Consistent results were obtained for the LiAlH4 sample using both methods.

  8. The general order of the analysis was standard-sample-standard-sample-standard-….  Each analysis consisted of 10 separate measurements of the signal at each mass.

The mass bias for each ratio was determined in each analysis of bracketing standard.  The average mass bias was used to correct the bracketed sample signals.  Each sample was run at least twice."


UPDATE#2 - Second Earthtech Ni Isotopic report agrees with University of Missouri results

https://goo.gl/tCMZ4g

Due to the unusual results from the first isotopic study by Earthtechs (ET) testing partners, where both Lithium and some Ni isotopes were studies, Earthtech commissioned another study from the independent testing lab. A separate portion of the blind samples sent was taken.

This time the results match those found at the university of Missouri (UOM), i.e. that Nickel was essentially natural isotopic ratio in all samples, fuel or ash.

The Independent testing lab said that trying to test for Li isotopes at the same time as some Ni isotopes most probably resulted in the unexpected results.

For the MFMP this is an easier result to understand, since whilst we still do not know which sample is which, the difference between UOM and ET did not inspire confidence in comparing analysis between different labs and techniques and also, was quite unexpected given the very short events that occurred in the GS3 runs.

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0 #45 Edwin Pell 2015-10-09 15:12
Exciting results for GS2. Would love to see same for a GS run that goes for 1000 hours, 40 days, 1.3 months.
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0 #44 Tom Clarke 2015-09-18 17:28
@Pete,

if you read it, that article is just saying that they cannot find significant electron screening in metal lattices. Uncontentious and accepted by pretty well everyone. It does not suggest lower loading is better, merely that electron screening as they measure it does not appear to be the mechanism behind LENR, if such exists.
Quote
 
 
0 #43 Peter Mobberley 2015-09-17 14:52
Electron Screening In Reaction Between Protons And ...
ol.ijs.si/~matej/sola/A4_6x9.pdf
by M Lipoglavšek - ‎Related articles
We have measured the cross section for the 1H(7Li,α)4He reaction at lithium beam ... Due to Coulomb repulsion the cross section σ for charged particle induced ...

Hi Ged,
Now I Know you are Jed because of an expression you use
'Oy vey'
You mignt want to add the above paper to your library
I think it is important
It suggests that high loading may not be advantageous
and that lower loading may ,in certain circumstances be
better. Pete.
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+2 #42 Ecco 2015-09-11 03:38
Songsheng Jiang reported observing slight changes in Li6 content and virtually no change in Ni isotopic ratios (1). This would be consistent with MFMP#21 and MFMP#59 being the fuel and the ash from GS3 as previously speculated.

(1) e-catworld.com/.../...
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0 #41 Ged 2015-09-11 03:17
Oh, nevermind, didn't see the very next comment about two week vacations. Oy vey!
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0 #40 Ged 2015-09-11 03:16
Quoting Robert Greenyer:
@All

Getting there - One party has said this

"I have run the analyses and am still working on the calculations. Should have some results soon.

The analyses that were contracted to be performed were a comparison of isotope ratios. Elemental concentration data from these analyses are limited and should be considered semi-quantitative.'


Aka, we can see changes by ratio, but can't extrapolate that with precision to absolute numbers. I.e. if 50% of the nickel is Ni62, that doesn't say if there is 5 grams of nickel or 10 grams, out of say a 15 gram sample.

Tis fine, just means we can't necessarily back calculate energy release reliably, -if- a change in isotope ratios is found.

Exciting that the data is coming along! Hopefully tomorrow will be our isotope day :D.
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0 #39 Robert Greenyer 2015-09-08 20:28
@All

Getting there - One party has said this

"I have run the analyses and am still working on the calculations. Should have some results soon.

The analyses that were contracted to be performed were a comparison of isotope ratios. Elemental concentration data from these analyses are limited and should be considered semi-quantitati ve.'
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+1 #38 Robert Greenyer 2015-09-07 12:36
@All

UPDATE:

One party says that the testing is still at the back of the queue and will not be done this week.

Another party says they are on holiday for two weeks!
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0 #37 Robert Greenyer 2015-09-07 12:36
@Tom

I am Cautiously optimistic myself. Confirmed isotopic / elemental shifts would allow me to move my position.
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+2 #36 Tom Clarke 2015-09-07 08:25
@Bob - I'm not making any assumptions about what comes from what - in fact my guess would be the two normal isotopic ratios both come from fuel+ash in GS3!

@Alan - thanks - so with that info we have a required excess power (under the hypothesis that such an isotopic change is happening from fuel to ash) of 160W over 30 hours. I'm still unclear what the effective total length of possible excess power in GS3 is.

@all - I like to try and join up as many dots as possible when looking at experimental results. This is mostly a skeptical exercise, because any given hypothesis can be knocked down (or at least shown to need radical modification) when it is inconsistent.

The area you guys are investigating is both very open (no clear theoretical expectations) and full of wild hypotheses. So the more filters you have for hypothesis-maki ng the better. Those hypotheses that survive filtering (as true ones will) are stronger, and waste of time hypotheses can be eliminated. This helps experimental design which is bound to some extent to be guided by plausible hypotheses.

The merit of filtering hypotheses with data is strong whether your initial approach to the question of "does an LENR+ effect exist" is highly skeptical (as me) or pretty convinced (as Bob).

Best wishes, Tom
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+1 #35 AlanG 2015-09-07 04:03
@ Tom Clarke

The GS3 fuel load was 0.30 g of Parkhomov Nickel and 0.03 g of LiAlH4 (Consolidated Chemical). The fuel was ground in a porcelain mortar before loading directly into the alumina cell.
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+1 #34 Robert Greenyer 2015-09-06 18:02
@Tom,

Bit premature - we don't know which sample is the ash and which is the fuel yet - an artefact of the robust double blind process we set up.
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+2 #33 Tom Clarke 2015-09-06 17:26
OK, so I note these results, and estimate the heat released from this conversion assuming (as does Bob) that 1H is the source of the extra nucleons needed to go from Ni58 to Ni62.

There is no uncertainty in this calculation, except the total mass of Ni in the reactor. I assume this is 2g.

Spreadsheet (how do i post this?) then gives:
Total heat release: 1.16E8J (this is equiv to a mass fraction conversion of 0.00031 on 2 H1 + Ni60 -> Ni62

This heat release corresponds to an average 1kW over 30 hours.

That would appear to be much larger than the possible excess heat from GS3?

It would be good to clarify:
(1) total energy in to GS3
(2) upper bound on total exergy excess of GS3
(3) mass of Ni (not total fuel, this contains LiAlH4 as well) in GS3


Best wishes, Tom
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+2 #32 Robert Greenyer 2015-09-06 10:19
@All

The New Fire MK1 - A controllable reaction driven and moderated by heat, pressure, element ratios, phase states and morphology...
by Bob Greenyer

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+2 #31 Robert Greenyer 2015-09-06 10:19
@Ecco

Yes - Cubic - with nano/sharp promentries

Yes - probably from contamination from transit/storage

C - will no from ICPMS, might be just surface.

In any case - the 200ºC treatment will remove the water (source of O) and C.
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+2 #30 Ecco 2015-09-06 04:08
@Robert Greenyer: I see, so perhaps the varying oxygen content might be mainly from moisture contamination.

I find odd that the Ni particles have in all cases consistently roughly 25-30% carbon content by atom percentage though. Is that really just from the background carbon tape? And is it usual for micro Ni particles to actually have a geometrically cubic appearance (with relatively "sharp" edges, even)?

EDIT: some more info.

Parkhomov's Ni powder is supposed to have 0.15% carbon (by weight), max:

i.imgur.com/EhHgpeJ.png
Source: docs.nevacert.ru/.../...

EDIT2: even less than that, according to newer standards (GOST 9722-97): eng.arsenal.dn.ua/.../poroshok

According to the same specifications, particle size for this Ni powder is supposed to be less than 20 µm, with larger particle sizes not exceeding 20% of the total powder content by weight.

This seems to be in agreement with the grain analysis submitted in late 2014:
e-catworld.com/.../...

(which apparently was from the "old" supplier, though)

EDIT3: have a look at this 2013 Rossi powder analysis:
Source: pesn.com/.../11-Askanalys.pdf


i.imgur.com/eoTs8nW.jpg


i.imgur.com/PMUxFwU.jpg
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+1 #29 Robert Greenyer 2015-09-05 23:37
@Ecco

They are from the same source. However, different paths.

Ed Storms sample was part of the Nickel I got from Parkhomov in Moscow, it was placed in a styrene screw top petri dish and flew with me, then packaged in a polyethylene lock bag and sent via air mail to Bob Higgins, who split it and sent it in a glass sample container with plastic lid from New Mexico to California.

Ubaldo Mastromatteo's sample was received in a glass container with metal lid in Padua from Parkhomov that had travelled by air - apparently from the same batch of 0.5 kg as I took the first sample in Moscow. Ubaldo presented a polyethylene sample container to take the Ni in which when via land to be tested.

University of Missouri's sample that has undergone SEM/EDX came from the Padua lot. I sent it in Clear styrene/polyeth ylene sample containers that had a synthetic rubber seal via Air Mail.

goo.gl/j7gtm4

Slide 15 onwards is the Parkhomov Ni. This is expected to undergo full elemental and Isotopic analysis.
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+3 #28 Ecco 2015-09-05 16:05
Is anybody aware if the Parkhomov Nickel powder analyzed by Ubaldo Mastromatteo and that analyzed by Ed Storms (Kiva Labs) were from the same source? They do look very similar visually, though:


i.imgur.com/J2rujBl.jpg

Mastromatteo's analysis showed (by weight)
7.389% C, 0.759% O, 91.852% Ni
docs.google.com/.../edit

The percentages sum up to 100%, and there's much less oxygen compared to Storm's sample. However the ratio between Ni and C is roughly the same. (this shows his analysis showed percentages by weight too in his case, btw)
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