Unconventional electrolysis

  • BTW, I suspect your ferromagnetic particles are actually magnetite. Martin and I were running a multi-plate electrolyser a while back using mild steel plates ( we were trying to bind the oxygen and just make hydrogen. We cartainly made a lot of black iron oxide, Fe3O4.

  • Alan Smith

    My assumption is that when the electrodes reach operating conditions where they can easily short-circuit, most of the black particles in the gap would be composed of elemental iron; it's certainly plausible though that a good portion would still be composed of various iron oxides (which would be electrically insulating), possibly mainly magnetite.


    EDIT:

    magicsound

    Thinking about after you'll manage to reproduce the observations (it looks like it's just a matter of time at this point) and/or set up a closer "Woodpecker" replication, without purchasing anything do you have the materials needed for arranging something along these lines? I haven't had the chance to personally attempt this yet.




    Rationale: if any sort of penetrating "strange radiation" -like neutral emission is being produced by these experiments, it might be able to get moderated and captured by a relatively thick "shielding" or "insulation" composed of both light and heavier elements, in a way similarly to how neutrons are usually dealt with in nuclear reactors. In absence of it, this emission would otherwise not interact significantly with nearby materials.


    On this regard I posted a possibly relevant excerpt from a recently published paper in another thread. For the record, I contacted the author, made an observation similar to the above on the effects that such shielding would have on the emission described, and he seemed to agree with it.


    EDIT2: charged particle emission and to some extent neutral emission may also leave the outer metal container in the diagram above electrically charged and produce a current. This could be measured with the oscilloscope.

  • Alan Smith

    Magnetite is certainly a possible constituent of the sludge. Can you suggest an unambiguous chemical test for its presence in such mixed ferrous/ferric amalgams?


    can  

    Yes I can put the glass jar in a surround like your suggestion. That will result in thermal insulation of the cell and lead to more rapid heating of the contents. A natural progression from this scheme would be to provide water flow through the solid filler material. This would enable both controlling the temperature of the electrolyte and a crude form of mass flow calorimetry.

  • magicsound

    That sounds like a good plan, but loose, granular, or water-soluble materials like those I suggested might not be very practical to use in that case. Perhaps something like stainless steel (or other material) wool or fine mesh could work better with a water flow through it, but it wouldn't be zero- or near-zero cost.


    Under the theoretical scenario described, emissions might vary depending on the heavy material/elements used in the shielding/absorbing material.

  • Magnetite is certainly a possible constituent of the sludge. Can you suggest an unambiguous chemical test for its presence in such mixed ferrous/ferric amalgams?


    That's a tricky one, since as you have implied there would be some particulate iron present, plus all three oxides, FeO, Fe2O3 and Fe3O4 at some level. The simplest thing to try would (probably) be agitate your sludge in DI water and use a magnet to separate magnetite and any iron particles from the heamatite etc which is only weakly magnetic. Do that a couple of times - marinating the resulting magnetic fraction in 0.5M HCl overnight in a warm place would probably be enough to transform any free particulate iron to yellow-green dissolved ferric chloride. HCl will also attack magnetite and the other oxides but much more slowly. If your SEM is up and running, the washed, magnetically separated (again) and dried remaining sludge (if any) should exhibit the crystalline features of magnetite, - examples of which can be found in many publications.

  • magicsound

    That sounds like a good plan, but loose, granular, or water-soluble materials like those I suggested might not be very practical to use in that case. Perhaps something like stainless steel (or other material) wool or fine mesh could work better with a water flow through it, but it wouldn't be zero- or near-zero cost.


    Under the theoretical scenario described, emissions might vary depending on the heavy material/elements used in the shielding/absorbing material.

    Two materials that are readily available are fine gravel (2-6 mm) and cellulose sponge. The gravel would work dry or wet and would block most gammas as well as less energetic photons. Cellulose sponge is mostly lighter elements: (C6H10O5)n and would pass energetic gammas and moderate any neutrons. Potential effect of these materials on EVOs needs discussion.

  • magicsound

    It depends on what you would define as EVO. I'm referring to the decay products of the initially formed entities, which have been suggested to be initially neutral for the most part. If they are neutral particles eventually decaying to charged particles, then a shielding composed of both light and heavy elements, the former primarily acting on the neutral component and the latter on the charged component, should work better.


    Depending on what the final charged decay products actually are, shielding materials could then be selected to produce recognizable emissions from, say, their beta decay.


    All of this of course assumes that there is something actually going on in the first place. Excessive shielding might possibly also work against detection efficiency, but the reaction energy could at least be seen as excess heat. Without shielding there would be neither, or only a very limited amount depending on surrounding materials and the environment.


    The materials I previously listed were intended to work as an alternative (easily available and able to be uniformly arranged around the reactor core) to materials like refractory bricks (generally composed of mostly O, Al/Si, then metallic elements, often also H) and the like, which on several occasions throughout the past years seemed to be instrumental in making people from different groups observe anomalous gamma radiation or excess heat from otherwise normally lifeless experiments. These would not necessarily be the optimal choice, but that's what I would have attempted using eventually in my own tests.

  • Today, from a comment made by Robert Bryant elsewhere, I accidentally came to learn about the work of late John Dash (1933-2016). He was a metallurgist who performed electrolytic cold fusion experiments with acidic electrolytes (generally <<1M H2SO4, occasionally HNO3). His last work as a coauthor was a paper with other known researchers in the LENR field, on co-deposition experiments.


    There might possibly be some correlation with the tests I've made with HCl in the past couple months, although I used no heavy water nor Pd/Pt.


    I went on LENR-CANR.org and tried retrieving all papers where he was an author or coauthor. Here is a list for reference and quick access.


    * * * * *


    In other news, I must admit that recently, because of the frustratingly short continuous duration caused by my testing conditions, difficulties in OCR'ing the instrumentation reliably (and long OCR times) and winter temperatures+bad weather preventing me keeping the window open in the testing room during the experiment, I haven't performed more tests as I initially thought I would do. Only last Saturday I tried cleaning the materials and electrodes from the last experiment I made on mid January (using first KOH, then progressively adding HCl until the usual reaction started occurring.


    The electrodes, stored in air, were pretty badly corroded. All residues, including mica sheet fragments, ended up being ferromagnetic and easily attracted to a magnet due to the iron thin film deposition layer formed in the process.



    Soon after extensive scraping, cleaning in HCl and thorough washing in warm water the electordes got corroded again, developing a light brown oxide layer.



    I'm not sure how much more I can add to the observations on my part with the limited equipment I already have. The main issue is that power measurement with the current probe might not be accurate, and easily performed water evaporation calorimetry has large error margins.


    I planned to run at some point a few more tests with the Geiger counter in a different location (between a 40-cm thick solid brick wall and 2 liter water-filled bottles placed in front of the experiment, which would partially and effortlessly reproduce the suggestion I made a few days ago), or also actively placing the most powerful magnet directly on one of the electrodes and/or using only slight amounts of K2CO3 (initially) and HCl with a shorter gap so that the deposition process would develop slower to check out how it affects the resonant noise.


    Just performing narrow-gap electrolysis without significant deposition processes going on also makes significant broadband AM radio noise occur (not resonant), but I'm not sure if it's just an ordinary effect (e.g. rotation of excited nascent water molecules from the recombination of oxygen and hydrogen. Similar radio emission is sometimes used for certain spectroscopy techniques https://en.wikipedia.org/wiki/Rotational_spectroscopy).

  • Alan Smith

    That is just one factor. Ideally these tests would be performed under a proper fume hood or wide open area with a large fan pulling the evolved gases away. Another factor is that they tend to be messy to clean up and kind of hazardous, although at the concentrations I have been using, HCl is still relatively safe.

  • Dash, J., C. Lee, and S. Pedersen, The Quest for Excess. 2003, Portland State University.


    This one with the High School kids, was one of my favorites when first getting interested. Clean, simple, and lots of explanations as they go along. I always wondered what happened to the young students involved. Hard to see XH, and transmutations, and then just walk away.

  • Shane D.

    You might be overestimating the willingness of high students to pursue their teachers' pet projects beyond what is required to get good grades, especially if they involve controversial topics that some might consider a waste of taxpayer money.


    * * * * *


    In other news, since today the weather was good :) I tried coming up with something extremely simple that could possibly improve the reliability and the performance of the last experiments. I haven't tried it yet, but the gap should be easier to tune up and clear if required. Furthermore it should allow a higher current density through the active area.




    I have also changed the location of the Geiger counter so that it's now essentially measuring the radioactivity of a 40 cm thick wall about 50 cm away from the testing location. It's sitting on a large computer case and any directly emitted particle from the jar would go through it before reaching the detector. Why this unusual arrangement that would likely not be able to measure gamma radiation directly coming from the jar, if any? The reason is that I argue (or better, others do) that such emission would not normally be visible at a close distance unless it's properly moderated and absorbed. Now I need a few days of background data to check out how it behaves ordinarily.


    According to Leif Holmlid from his latest paper (open access) as of writing it sounds like different detection arrangements than what one would normally employ might be worth checking out:


    Quote

    [...] The radiation in our laboratory has been checked by hand-held G-M counters (mainly Mirion RDS-80) close to the muon source, and no dangerous radiation levels have been observed. Of course, the G-M device response is limited to one count per laser shot so the real intensity may be higher. The sensitivity of this type of device is otherwise high enough to easily observe random radioactive decay in antireflective coatings on optical parts like lenses and windows. Instead of charged kaons, mainly neutral kaons seem to pass out into the laboratory, and the interaction of such particles with matter is believed to give considerably lower radiation levels, maybe mainly due to their longer decay times which allow them to move further before decay, thus depositing much of their energy in the building walls and in the laboratory equipment.


    I might perform some testing within a few days, but I'd like to first go through John Dash's papers on electrolytic LENR experiments with an acidic electrolyte; perhaps something useful that could be related with or applicable to my testing conditions might be found.

  • So far the Geiger counter in the new location isn't giving large swings in measurements, although the level is relatively high compared to what the lead brick cave in magicsound's location is giving. Below is the data for the previous 30 hours or so. The red lines denote when I opened/closed the window in the room.




    * * * * *


    In other news, I quickly read through all the papers by John Dash that I previously linked from LENR-CANR.org and I tried to make a summary of the main findings that could be relevant to the tests I've performed so far.


    • In a paper the rationale for using an acidic electrolyte was as follows:
      • "[Fleischmann and Pons] used a basic electrolyte and we used an acidic electrolyte which had a lower pH, thus enhancing the discharge of hydrogen isotopes at the cathode due to the much higher concentration of these species in the acidic electrolyte; [...]"
    • Most experiments used D2O electrolyte with 0.06M H2SO4 (sulfuric acid).
    • The experiments performed in the early '90s were often only a few hours long in duration.
      • In some experiments electrolysis was applied for just a few minutes, still giving anomalous results later on.
    • On one occasion where the Pd cathode accidentally became the anode for a short while, the electrolyte solution turned black, depositing Pd on Pt.
    • When the original electrode polarity was restored, this caused deposition of Pd on the Pd cathode.
      • This method is also known as co-deposition in the LENR field, notably used by Szpak and Mosier-Boss. This method causes Pd to be deposited together with hydrogen atoms.
      • Later on this was also intentionally performed.
    • This electrode polarity reversal could cause a temporary prolonged enhancement in measured excess heat.
    • The cathode was most of the time Pd, sometimes Ti.
      • It was formed by cold-rolling thicker foils into the desired (lower) thickness.
        • A lower thickness was initially found to yield better and more reproducible excess heat than as-received foils.
        • Later on it was determined that rather than volume, excess heat seemed to be more dependent on the surface, or changes induced into it.
    • At least up to a certain level (the maximum generally allowed by the cell) it was found that excess heat was proportional to current density.
    • A higher electrolyte and cell wall temperature was found to improve excess heat and reproducibility, together with the presence of temperature gradients.
      • Conversely, the lack of results by other groups was attributed to the often too low temperatures.
      • It is thought that triggering methods such as laser, higher input power, etc, could mitigate the effects of low temperatures, but ultimately in many electrolytic experiments by other groups it's generally too low.
    • Titanium cathodes, used since early on, were found to yield generally higher excess heat results and in less time.
      • Excess heat with Ti foil would often appear right away, whereas with Pd this would require a kind of induction time depending on the thickness of the sample.
        • From what it is suggested later on, more than the thickness it is probably the stresses caused by the cold-rolling process.
    • Unexpectedly it was later found that reusing the electrolyte employed for Ti foil experiments would enhance results with Pd cathode.
      • This was attributed to the Ti dissolved in the electrolyte having a chemical-catalytic effect on the processes involved with the cell under operating conditions.
    • Generally the tests that produced anomalous effects were those employing D2O (heavy water) instead of H2O (light water).
      • However, in a test performed much later on, a control cell was found to produce excess heat and other changes typical of active cells using heavy water.
        • It used tap water and commercially available battery fluid instead of analytical-grade H2SO4 and deionized water.
        • It is suggested that highly purified chemicals are not necessary for LENR
    • Samples showing excess heat, isotopic changes in the Pd composition and nuclear transmutation were found to change/evolve over time many months after storing at ambient temperature and pressure.
      • "Fibers" and other visual changes often appeared on the surface of such samples. Such spots also showed evolving nuclear changes over time.
  • Bob Ellefson

    Most of the longer, more structured comments I write on the forum are from my personal notes or eventually end up being part of them, so with the above summary I didn't put much more time than I would have by keeping it to myself.


    By the way, here is a paper from Dash's group reportedly showing that excess heat with a Ti cathode was achieved right away, with steady state operation within 45 minutes: https://www.lenr-canr.org/acrobat/DashJexcessheat.pdf



  • Dash appears to have workhardened the titanium uniformly using a big roller..

    (more uniform than hitting it with a hammer.)


    Perhaps one could twist Celani knots on a titanium wire... and soak it in iron solution like he did

    The purity of the titanium was high.. with some vanadium... but what else was present in the foils?

    For example very low amounts of rhodium103,... less than 0.1 % ... in palladium enhanced LENR greatly


    Other researchers used lathe turnings of TI 662 -which of course contain metastable tin isomers.


    Vanadium??


    V50 has a lowlying gamma state at 226.25 kEV... may be relevant?




    CHARACTERIZATION OF CHARGED PARTICLE BURSTS FROM DEUTERIUM LOADED THIN TITANIUM FOILSlenr-forum.com/attachment/7563/

    D.H. Beddingfield et al Colorado School of Mines,

    Following our recently reportedobservation of intense bursts of charged particles

    from deuterium gas load thin Titanium foils,

    Our samples consisted of Ti662 (6%V, 6%Al, 2%SN)2lathe turnings of nominal thickness

    about 100 µm and of surface dimension about 1 cm. by 2 cm.

    The D2 gas was introduced by first annealing the samples at 700° C for three hours under vacuum

    and then introducing 1 Atm of D2 and allowing the samples cool slowly



    From my armchair

    It was formed by cold-rolling thicker foils into the desired (lower) thickness.

  • .

    It's odd that back in the day of Egyptians they would bother refining this stuff to make paint


    The oldest pharmacy was Egyptian

    There were plenty of nasty pathogen vectors in the Nile Delta

    So eye paint was not just cosmetic


    Black antimony, however, showed considerable antibacterial activity even against P. aeruginosa

    https://www.ajol.info/index.php/ijs/article/view/131594


    If they refined it too much to get rid of the Pb and Cd it probably wouldn't have worked


  • RobertBryant

    He also observed excess heat with "as received" foils. Although in other papers it looked as if cold rolling had a measurable impact especially on Pd, in the study below on Ti foils it didn't seem to bring very large changes. Furthermore excessive thickness reduction worked against excess heat observation:


    https://www.lenr-canr.org/acrobat/DashJinteractio.pdf




    But it might also be that too pure chemicals don't work well: https://www.lenr-canr.org/acro…teVproceeding.pdf#page=82



    (most of the time up to that point light water was used as a control)

  • But it might also be that too pure chemicals don't work well


    Which is one of the tenets of atom-ecology


    ...to keep the gamma fires simmering and not exploding..as in magma broth that stays simmering for thousands of years


    Impure battery acid is supposed to have small Fe and Cd (ppm)... Cd has a few metastable isomers with lowlying gamma


    https://www.researchgate.net/p…-acid_batteryelectrolytes

    from my armchair



  • RobertBryant

    To be honest I'd suspect the significantly more abundant Ca (plus Mg) in tap water to have a greater effect, in case introduced additional impurities/elements in this test had a positive influence on the reaction. Didn't Iwamura used CaO layers alternated with Pd after all?


    https://lenr-canr.org/acrobat/IwamuraYobservatiob.pdf


    I also understand that one of the Atom-ecology tenets (...) is that the reaction spontaneously occurs in nature, and in that case more common elements should work too.


    Magma broth? Then so-called rock-forming elements (plus hydrogen/water) should be fine and perhaps even desirable.


    https://en.wikipedia.org/wiki/…_of_the_chemical_elements

    https://opentextbc.ca/geology/…agma-and-magma-formation/

    https://en.wikipedia.org/wiki/…ements_in_Earth%27s_crust



  • Observing high excess heat production on reversing electrode polarity suggests a protocol for continuous heat production by applying a slow sinusoidal AC voltage. This would cause co-deposition of Pd/Ti/Ni/Fe or V each from an electrolyte containing such an atom-ecology mix of transition metals and light, fusable elements (H, D, Li, Be, B, C etc) on BOTH electrodes periodically Using low pH boosts the proton concentration so is clearly advantageous. Mosier-Boise's papers mainly document radiation release from the cathodes due to LENR during the CO-DEPOSITION process ie on electroplating rather than on electrolysis per se, so selecting a low voltage/high current density might produce the best excess heat results. I was thinking of experimenting with plasmas to study LENR but maybe unconventional electrolysis needs further work.

  • Dr Richard

    A slow sinusoidal AC voltage could be good if the electrodes are composed of the same material and therefore expected to erode at about the same rate in the process, but this might not necessarily be the case. John Dash typically used Pt for at least one of the electrodes, which wouldn't get significantly affected by the electrolysis in the acidic H2SO4 electrolyte solution (although some Pt did deposit on the Pd cathode).


    This would also require a somewhat more advanced and potentially expensive power supply. I think it might be easier with a square DC wave which wouldn't require particularly expensive equipment, but in my latest tests I typically deliberately arrange the electrodes so that eventually they short-circuit and produce arc discharges, which might not be so great for the reliability of integrated components used for the polarity reversal (a good while back in the thread several options were considered and H-bridges or other high current DC motor controllers could have worked in their absence).


    The arc discharges might or might not be necessary, but they can provide an intense impulsive trigger (typically absent in light water electrolysis experiments) and very high localized temperatures, in addition of themselves causing electrode material sputtering and ablation. Furthermore Parkhomov et al suggested that setups employing them (e.g. as in his "Woodpecker" shown some time ago) might be able to emit "strange radiation" which would be interesting to observe.


    * * * * *


    EDIT: on a different note, in reference to elements in tap water potentially improving results in some of John Dash's experiments as I previously suggested and as John Dash also did for one experiment he reported in 2009, I tried looking online at the latest chemical analyses for tap water from various locations in my general area of residence.


    Ca is generally the most abundant ion, but not always. Values in the table below in mg/L.


    #
    Ca Mg Cl2 NH4 NO3 NO2 Cl K Na SO4
    (1)
    87.7 26.20 0.19 <0.10 10.60 <0.05 36.8 12.20 25.6 52.90
    (2)
    77.8 17.95 0.11 <0.10 20.97 <0.05 26.2 31.20 26.1 18.43
    (3)
    14.3 3.65 0.10 <0.05 6.30 <0.05 7.4 16.93 12.3 8.13
    (4)
    92.4 21.88 0.16 <0.03 2.00 <0.01 4.9 0.68 3.0 4.10
    (5)
    107.2 19.53 0.14 <0.03 3.59 <0.01 9.1 2.29 6.9 23.34


    * * * * *


    EDIT: again changing subject, I have now background Geiger counter data from the new testing location for the past 52 hours or so. The red dashed line denote opening-closing the window. It seems that slight changes occur following that, but they might be coincidental. This afternoon I tried opening the window at a different time and no short-term reduction in counts was observed.



    In general anyway it looks like readings are relatively stable. The weather has also been stable, on the other hand.

  • Shane D.

    He's trying to solve some electromagnetic interference issues with his instrumentation. Meanwhile I'm doing a slowly progressing test with the new electrode arrangement, and I haven't added relatively large amounts of HCl yet.



    EDIT: In the end I could kind of reproduce a similar noise, but not to the same extent as before. However I made a lot of changes. The condition where after a while numerous small discharges occur in the gap could still be reproduced, so it's not critically dependent on electrode geometry/arrangement.


    In one occasion a persistent short-circuit bringing current up to 38A occurred, but I could easily fix it this time, so at least on this regard this new arrangement is less frustrating.


    I made a couple videos with my old cell phone but I haven't checked if they're usable/show anything interesting yet.


    No significant change in Geiger counter readings observed (red dashed lines: beginning-end of test):



    Longer term measurement about an hour later (here it looks almost as if there is a kind of decrease from the average of the past few days):





    EDIT2: here are a couple videos, unfortunately of poor quality:



    It's not very visible or audible, but small yellow-red discharges occur in the electrode gap portion not immersed in the electrolyte, making a faint resonant noise reminiscent of what I previously reported. At some point temperature unexpectedly increased and caused the dark-looking metal particle-filled electrolyte to partially overflow by boiling.



    Here I tried pulling the electrodes in and out of the electrolyte solution while they were operating, which was made easy by the thick plastic support. A few presumably high-current density areas where would often briefly become incandescent in the process. Several weeks ago I started looking more into electrolysis in HCl after making similar observations, by the way.