StevieH Member
  • Member since Jul 21st 2019
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Posts by StevieH

    I've just been reading about a failure to reproduce a series of positive experiments due to running out of Pd. New Pd was bought from the same supplier, JM, and the same experiment ceased to produce excess heat. This prompted analysis of the Pd wire. It was then found that although it was commercially pure Pd, from the same source, the original contained a small fraction of Rh which differed from the Rh content of the new one.


    Would it be possible to get a proper analysis of TM's Pd rod while it still is around. This could prove vital information, as there is no doubt that he has found something major. We don't know the mechanisms, so the devil is going to be in the detail.


    Does anyone here, like AlanG for example (certainly not trying to put you on the spot, just using your excellent CaCO3 analysis as an example), have access to the necessary kit to save expense for TM and get the results to us all?

    I definitely plan on attempting a Mizuno replication, and already have most of the equipment from previous experiments. Here is a brief overview.

    Jeff

    I was just wondering what your plan is re the r.g.a / mass spec / leak tracing situation. This seems to be the one where it is difficult to avoid big expense, and the only alternative is to run blind. There are rga s available on ebay, but even if they are ok technically, they are usually useless without OEM software, which is proprietary and expensive.

    This is another picture from the same source- and this definitely looks like a different rod. And it also shows the supplier Alfa Aesar, which is the most useful thing.




    Yes, so he's tried a few then.


    Mind you, one campany's 999 Pd should be the same as another's. It would really have to boil down to a very fine tuned mechanism if one of the p.p.t contaminants were to be the critical component. Also, although they might have different company names on them, there's very limited range of places on the planet that the Pd comes from, and also, you will find that there are very few original refiners.


    Most of these companies will be buying from a refiner and selling it on at a profit. That's why it's easy to wind up paying well above spot for precious metals. It really does pay to shop around.

    Is the Pd in the chuck a recommendation to take the mesh and rub it against a turning piece of Pd?

    No, quite the opposite, I think.9205-pasted-from-clipboard-png9162-mizunopladdium001-jpg

    On the left is in Alan Smith's post on p23. I have posted previously regarding the Pd rod, and the markings on it not matching the rubbing process we are emulating, but after a couple of sherbets and a night or two sleep, with the brain still churning over, it's feels like it is starting to make sense now. Alan, you said this was a different rod. Well I don't reckon it is , I think it's the same one. The barrel like markings to the right of the nodule are not consistent with linear rubbing, but they certainly are explained by the rod in the drill chuck. Rapid rotation on the abrasive surface of the mesh leaving circumfrencial marks makes sense to me.


    The next thing is the marks on the left end of the rod. These could be chuck scores. I think this is a previous system which did not work well. The mesh would need to be on a raised surface or the edge of a bench. I could be wrong but I think I read somewhere that TM works alone. So if you are holding a drill and trying to rub the mesh, you would need a very effective clamping system for the mesh, or, when the rotation of the rod was pushing towards the centre of the mesh, it would grip and get tangled. That would be consistent with the marks on the left being chuck scores if he hasn't tightened the chuck enough, or if it is tight, and the mesh has tangled like hell.


    Another thing that was concerning me was the nodule area, and the fact that the right of the rod is not co-axial with the left. Well, if you look at the chuck, there is not apparently enough length of it to contain the whole rod as it appears in the image "with nodule", but if he has realised the need for a handle, it would be consistent with him having cut the deeply scored part of the rod off, and homogeneously welded it to a different Pd rod, or even spliced a bit in. You would only need an oxy torch. That would also explain the "hanging drop" appearance of the nodule., and the thicker shoulder aroung that area which is bigger than the diameter of the rod. In a manual rub, the right hand bit would not be used due to lack of contact pressure, but it would make a good handle part, as it would not impart pollution if it came into contact with the mesh.


    I know this is a bit of an essay, but the evidence all seems to be there. Good detective work finding those pictures Alan. What do you think guys?

    None taken Nick. I am totally on board with everything you said. My work requires the utmost dilligence and determination through adversity. Giving up is not the order of the day. Persistence is omnipotent.


    I was not trying to say that high stakes mean no action, quite the opposite. I was just trying to make the point that with the stakes so high, it is more vital than with a normal replication, to get the best information possible about what was done. We have already seen from the Pd rod and AlanG's ESM image that there may well be variables that we are totally unaware of, and a slight deviation, even unknowingly, may result in failure.


    If I might just refine what I meant using your basketball analogy: your philosophy is excellent, but if you apply it to shooting at a basket that you can "see", but unbeknown to you there is a trick of the light, and it is actually 3 feet further along the wall, then you aren't going to get many in.


    Of course, that does not mean that we should not take the best shot that we think we have, and go for it.

    The Mizuno mesh is 'twill weave' I'm pretty sure that makes little difference. The critical thing is always 'process knowledge. When you have done a lot of lab work you learn to 'fill in the gaps' in descriptions of a method. But, you can never be sure you filled them in in the right way when attempting a close replication.

    Precisely, sir. Which is, of course, why I was making the point regarding as much detailed information as possible. Close replication of some experiment is one thing, but when the stakes are this high, it is vital to put the utmost dillingence into attaining a positive result, n'est ce pas? As the bloke with the little grey cells would say.


    Incidentally, I have modelled the new twill pattern in CAD, and the difference is that for the same depth of cut, (and the size of the sites matches AlanG's SEM image well), the double twill has 1/2 of the reactive area. Of course as it matches the mesh that TM used, it will at least give a similar result. However, there do seem to be inconsistencies with the sites produced by abrasive paper. There should be a herring bone pattern, and one the SEM, some of the sites are missing. But I suppose the is just part of the randomness of a manual rather than machine treatment.

    I am getting conflicting messages. Some say they can not proceed unless more info is made available. Others appear to have enough (info) to proceed on with their attempted replication.


    So which is it?

    I don't think it's either Shane, it's just the spectrum of differing levels of knowledge, experience, approach, aspiration and all the other human qualities that you get when a bunch of individuals come into contact with the aim of doing something.


    Yesterday, I was surprised to learn from AlanG that the mesh he received from the "Mizuno source" was a double weave. I'm stuffed if I can find where, in the papers I have, that it states it is made this way. I had done some CAD drawings to get an appreciation for the physical nature of the application and the reaction sites. I did it as normal single weave. Now you could say that isn't going to make a quantum difference. However, the point seems to have been made by Jed and others that we need to replicate in as much detail as possibe, the Mizuno experiment. It looks like yet another dichotomy to me, so make of it what you will. I've got 30 years experience in freelance technical development, and, motivated believer though I am, I'm not happy to proceed until much more attention gets paid to detailed information. There are too many unanswered questions. Proceed and hope isn't an approach I apply to projects.


    But then, of course, you could apply Cydonia's perfectly valid approach of "get inspired, and trust your engineering skills". That is though, of course, if you have confidence in them to get past the details and hope that none of them is the one that you miss and which turns out to be crucial. Another of these was again pointed out by AlanG's discovery of the presence of CaCO3 crystals due to washing with tap water. This could be purely incidental, or a vital catalyst.


    At this point I would like to make it clear that my issue is not with lack of explanations of mechanisms- we know we are in the dark on that front- it's the possible missing of detail of exactly what TM has done that could cause the missing of something unknown, but vital. This may well lead to failure, and loss of faith in the results of TM. Then there is the potential charge of deliberate failure, and all the rest of it. It's a tricky one to call.

    My initial report on the Ni mesh preparation:

    https://bit.ly/2Mv13HY

    Excellent Alan. You obviously have access to some hot kit.

    I did a CAD drawing a few days ago to get my head around the situation with preparation. Perhaps someone could help me. I have read the papers published, but can't for the life of me find where it says the mesh is a double spaced weave. I did it single both ways and then a few calcs., for numbers of sites and likely thickness of Pd.


    Also, re the CaCO3 crystals, I wonder if these are more likely to be swept away by the physical application galling technique, rather than included in the bonding. I say this because I reckoned that one reason for the better performance of the rub method is that it physically wipes away any oxide that will have formed over the Ni mesh after cleaning. Ni gains its anti-oxidation properties from its formation of an instant cover of oxide, even if it looks clean and has just been "cleaned". This gives it a passivation layer which soon gets thick enough to prevent further oxidation. It could be removed by the low pH of an electroless plating solution, but these are all difficult mechanisms to quantify. Any oxide on the uncovered surface of the mesh would likely be reduced and evolved as water in the bake out with D2 present.

    Hi All,

    I've just joined but have been thinking about this situation for a while now.


    1st off, as has been said, but no updates yet, that Pd bar looks like it has some fairly idiosyncratic history :- not exactly off-the-shelf, is it.

    We need a run down on exactly what it is and where it has been. These experiments are notoriously tricky to replicate, and that bar, focussing on the fact that it is so crucial, isn't helping.


    Jed Rothwell reckons that the notching is from the rubbing. Well I don't reckon that. The spacing is way off. What I see, judging by the 5mm diam. is 3 notches on the left with 2 different gaps of around 7mm. On the right are about 7 sections which are rounded, or barrel shaped, like the profile that is rolled onto heat exchanger tubes, but without the spiral. We are dealing with 180 mesh here, and any effect from the limited amount of rubbing it has done would surely be far finer than that, probably noticable only as a bit of polishing or wear on the edge opposite to that strange nodule, which looks suspiciously like a cleverly formed handle. I did wonder how he was gripping a 5 mm rod without using tools that would introduce the likelihood of wiped contamination.


    Still on the subject of the totally vital Pd on Ni mesh : I might get a bit of grief from Jed here, ( if I haven't already from the first comment :) ), and this is only a thought. It probably would take him a fair bit of preparatory work, but as this is all about rubbing a bit of Ni mesh with about 2k currency units worth of Pd rod, would it not be possible for a couple of us to produce rubbed mesh, and for him to test it in his set up first. It would be much more efficient than everyone investing in turbo molecular kit and mass spec or rga. Then, if he gets similar results, we can get our meshes back and invest in the kit, knowing that all we need to do is get the details right and we are sorted. If he doesn't, we need a full on forensic examination of that rod ! Whereas, if people fail now, it will be called a case of bad replication or a one-off that can't, or likely will never, be replicated. If we take this suggested route, it surely offers cover both ways.


    Finally, nice find and share by Alan Smith, it's in my SSD, thanks for that!