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Old 6th August 2006, 05:36 PM   #31
Mare Rosu
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Default Trace element testing

Great information on testing for trace elements. Obvious to me we have some heavy hitters at bat here
I have some knowledge of Neutron Activation Analysis testing from my Georgia Tech days. I wonder if anyone has tried or has any knowledge of it?
For anyone interested, this is a Link to some information about it, I found it using Google search. one side effect is that the item is now radioactive and depending on the isotope half life it may be a while before it decays down.
http://www.missouri.edu/~glascock/naa_over.htm

Gene
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Old 6th August 2006, 07:42 PM   #32
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See what happens when you use the words 'meteorite' and 'dagger' in a thread title, Gene?

It had occured to me that pre-industrial iron would have a different (and more variable) chemical signature; I suspect it would not cause too much noise to obscure the extra-terrestrial signature over all the potential elements...there might be archaeological papers that have previous analyses on old keris, one could check them against modern steel & look for differences.

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Old 6th August 2006, 08:09 PM   #33
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You're certainly right about that, Jeff. To be honest, I only read the thread because I'd just finished reading about the "Arctic Iron Age"--where the Inuit and Dorset peoples before them made tool blades out of meteoric iron for, I don't know, a thousand years or so. Another story.

Anyway, I think it'd be a great subject for a metallurgy/archeology PhD--looking at Indonesian blade making, and determining how much of the steel's chemical composition/isotopic signature depends on the metal source, how much depends on the carbon and fuel sources, and how much depends on the arsenic staining (at least in the keris blades). It would be interesting to know if there is enough information to determine things like blade origin (or origin of materials) or blade age through a test.

Not something I'd want to do, although I'd be happy to help analyze the data for patterns. Oh well, something to dream about.

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Old 7th August 2006, 12:17 AM   #34
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Quote:
Originally Posted by fearn
The obvious problem is that the terrestrial iron isn't pure iron, nor is the carbon to make the steel pure carbon. There's going to be a mix of other trace elements that will have to be factored in.
Fearn, There are a number of Meteorites Labs that receive “large” numbers of unknown samples sent to them. Anything from mining slag to your common variety of earth rocks. The whole point of fingerprinting with trace elements is because the trace elements that are found in cosmic source materials are unique enough for positive identification. You can check against the database and identify what you have. You will know if it is an earth rock… or if it is Lunar (Lunars are a little different than earth rocks)… or Martian, which was a little more work (it was the trapped gassed that ID’ed these). It would be highly improbable that you would get at trace element (ratio/concentration) match by accident. If you have worked with these curves (not much unlike FT-IR), then you know what I mean,

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Originally Posted by fearn
The unobvious problem is that keris blades are occasionally cleaned with an arsenic (As) solution, so the researcher has to factor in the accumulation (if any) from cleaning. Since it's not pure arsenic in the Indonesian cleaning solutions, this would take some experimentation.
Surface contamination is an issue on any sample to be tested. This is the reason the surface is removed (polished), to reveal that actual material that you want to test.
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Old 7th August 2006, 12:53 AM   #35
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I agree BSMStar, so long as we're talking about ID'ing meteorite samples.

When we're trying to ID the meteoric component in a knife made of mixed terrestrial and meteoric materials, it's a bit more complex. The blade is made of:
1) the meteoric material (with a readily identifiable asteroidal fingerprint?)
2) iron from a terrestrial source, with either a known or unknown chemical fingerprint depending on age and source, and
3) carbon (for steel) from a terrestrial source, that probably contains traces of contaminants such as cesium, mercury, or whatever, depending on the source of the carbon (charcoal, coal, etc).

I'll submit that this mixture can be deciphered if 2) and 3) are known--basically, in an industrial setting, especially where the steel is purchased and contains 2 and 3 already. In a non-industrial setting, such as with a century-plus old keris from somewhere in Java, it will be extraordinarily difficult to decipher all three, since we have little idea about the source any of the ingredients.

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Old 7th August 2006, 01:20 PM   #36
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Quote:
Originally Posted by fearn
I agree BSMStar, so long as we're talking about ID'ing meteorite samples.

When we're trying to ID the meteoric component in a knife made of mixed terrestrial and meteoric materials, it's a bit more complex.
Fearn, the distribution for elements in cosmic sources is different than terrestrial sources. It’s that simple and that unique. I do not know how to better explain it. It is a matter of being able to detect that fingerprint in a diluted form. I believe it is possible if the concentration of meteoritic material is high enough. The only issue would be if an exotic alloy was used with the fingerprint traces as ingredients… not likely in a 200 year old Keris.

Also, keep in mind that meteorites are older than earth rocks. We are not looking at Rubidium/Strontium ratios (good age indicators), but are not the trace indicators we are looking for (not looking specifically for isotopes, we are looking at elemental abundance - unless something has changed in the pass thirty some years).

Also, (let me add) in the field of Tektites, LDG (Libyan Desert Glass) has a very small amount of a meteoritic component, that is traceable back to a chondritic impactor. LDG is believed to be earth rock impactites (as are all true Tektites), created during an “impact” event. Talk about an unknown mix and meteoritic dilution… but the fingerprint is still there.

Fearn, you have the last word.

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Old 7th August 2006, 02:38 PM   #37
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I think the amount of Iridium in typical (not the meteorite impact ones)mineralized (ore-bearing) Earth rocks is measured in a couple ppb (part per billion), down to parts per trillion; the two iron meteorite info sheets on the previously posted Metbase link were a couple ppm (parts per million) - it seems like even after taking into account the concentrating effects of smelting and the diluting effects of mixing meteoric metal and earth metal, there's room for a noticeable difference.
But it's all speculation until we get some data to crunch.
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Old 7th August 2006, 04:21 PM   #38
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Quote:
Originally Posted by BSMStar
I believe it is possible if the concentration of meteoritic material is high enough. The only issue would be if an exotic alloy was used with the fingerprint traces as ingredients… not likely in a 200 year old Keris.
But isn't this the rub. I mean, would the concentration of meteoritic really be all that high in a 200 year old keris. Not 50 percent certainly, at least not in the entirety of the blade. Yes, it would probably be concentrated in the pamor areas, but what keris collector that you know is going to alloww someone to polish off ANY amount of the pamor on their keris for testing. Not me, for sure. Frankly i think the obsession with meteorite blades (keris in partictular) is way out of hand anyway. It is not the main determining factor for a good keris. In fact someone has yet to prove to me that it was even used in keris before the Prambanan fall in the mid 18thC, so it is not therefore vital to the art. In many ways this reminds me of the effects of gold fever. I still don't see that the methods discribed are viable in determining tghis question, even if technically it is possible.
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Old 7th August 2006, 05:20 PM   #39
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nechesh, as earlier stated, testing your collection may not be desirable. I would not take a valuable Pusaka and test it (any why would you want to). But I believe I have made the point that testing old blades which are not deemed “valuable,” to see what percentage of the population may contain meteoritic material, may have some worth. My gut feel is that it well be far fewer than people think. It may let us know if there is indeed a look (a pamor affect) and feel (tactile response) to the blades that contain meteorite. Therefore, there will be some benefit for the research effort that could be applied to blades in our collections (or we may find out you can only tell by testing).

I think the rub is talking someone to doing the research… and giving up the samples.
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Old 7th August 2006, 05:42 PM   #40
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Frankly Wayne, i'm not too sure i really like the thought of ANY keris being destroyed for this purpose. I can tell you (though i certainly can't prove it ) that your gut feeling on this matter is most probably entirely correct. I think you would find a relatively few keris actually contain this material. I would also image that when meteorite was used it was not for unimportant blades, so i'm not too sure that looking for meteorite in what some refer to as "junk" blades is going to prove very much since these blades are not likely to contain it. I do believe there is a look and feel that does indicate the likelihood of meteorite and i believe these clues have been discussed in the past, but i think that the only way to really convey this information would be studying these blades in person with someone who is familar with this ID process. It's a bit hard to get that kind of knowledge across on the internet. Ultimitely i think that determining this matters much more to market values and dealers than it does to the real study of keris, but i guess that's just my way of looking at it. It would be nice to know if i had a meteorite keris, but i am not up to destroying any keris to prove it.
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Old 7th August 2006, 06:00 PM   #41
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nechesh, I understand your position. On the Japanese side, knowing they use damaged and broken swords… did not lighten the pain to a collector… that they are in turn cut up... and analyzed. But even if a number of old “not valuable” Keris were tested, they would then be a part of an invaluable/indispensable collection of reference pieces, although further damaged by the testing. But I fully understand not wanting to do this with any (historically valuable) piece (and to me, they all are historically valuable), there will be no replacing them. As I have said, it depends on how bad do you want to know.....

Hey Jeff...

The earlier pic that you posted, is this a "meteorite blade?" It would be interesting to find out as to what affects on layering that you've noticed and at what percent meteorite material.

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Old 8th August 2006, 02:08 PM   #42
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Yes, that blade had 2 patterned pieces of 50% meteorite material sandwitching a piece w/o meteorite. The light layers are pretty much all E.T., and the main thing I noticed while making the blade was how easily Campo Del Cielo forges together, compared to other irons.
I'm not sure what you mean by 'effects on layering,' though, can you be more specific?
If meteoric nickel was all they had to bring out high contrast in the old blades, I bet the ET metal is not very diluted - in the light layers of the pamor.
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Old 8th August 2006, 04:29 PM   #43
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Quote:
Originally Posted by Jeff Pringle
I'm not sure what you mean by 'effects on layering,' though, can you be more specific?
It is my understanding that the cause of pamor is due to the “layers” of nickel and iron (and steel). When stained, the solution of arsenic and lime juice turns the iron black and the nickel remains basically unstained. When creating a mixture of “iron” and meteorite, what happens to the nickel in the process… does it “mix” or does it tend to separate and create “bands” of nickel in the iron (making its own pamor)?
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Old 8th August 2006, 06:09 PM   #44
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Quote:
Originally Posted by BSMStar
It is my understanding that the cause of pamor is due to the “layers” of nickel and iron (and steel). When stained, the solution of arsenic and lime juice turns the iron black and the nickel remains basically unstained. When creating a mixture of “iron” and meteorite, what happens to the nickel in the process… does it “mix” or does it tend to separate and create “bands” of nickel in the iron (making its own pamor)?
While nickel is certainly used as a pamor material and gives quite a better contrast i just wanted to remind everyone once again of the work of Professor Jerzy Piaskowski who determined that many old keris may have used no nickel whatsoever and achieved pamor contrast through the use of different types of iron that i believe may have had different phosphorous levels that create the contrast. I think that perhaps Alan Maisey can address your last question (certainly more accurately than i could ) and perhaps follow up a little on Piaskowski's work with keris materials.
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Old 8th August 2006, 06:28 PM   #45
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You are absolutely correct nechesh... my fault for being focused on the meteorite/nickel iron subject, dealing with the knife that Jeff made. My Pajajaran is nickel "free" and made of contrasting iron alloys. Thanks for keeping me honest.

Quote:
Originally Posted by BSMStar
With the Keris, I have always wondered… how did the method of folding two alloys come into being? The very early Keris did not contain nickel, and relied on two alloys of iron.
A quote from earlier in the thread... to prove I am getting senile.... at least in my focus.
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Old 9th August 2006, 12:36 AM   #46
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Quote:
Originally Posted by BSMStar
A quote from earlier in the thread... to prove I am getting senile.... at least in my focus.
LOL!
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Old 9th August 2006, 07:15 AM   #47
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The most common method of making pamor with nickel is to take a paper thin piece of nickel, sandwich it between two layers of iron and forge weld it. You take four of these little billets and weld them together, then you forge out and double over and weld until you have 128 nominal layers of nickel.
In the finished pamor the nickel layers are quite distinct. The nickel does not melt into the iron, it stays as distinct layers of material. Probably the easiest way to think of the mix of nickel and iron, is that the iron acts as "glue" to hold the layers of nickel together.Accordingly, if you can find a relatively wide band of nickel, you have a pretty large area that could be tested.

I`m sorry, I cannot expand further on Prof Jerzy Piaskowski's work. It is highly technical, and his two largest papers have not yet been published. I am only aware of the content because I have worked with him advising on strictly keris and cultural matters, since about 1988.
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Old 9th August 2006, 01:06 PM   #48
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I understand Alan, and I have not read Prof Piaskowski's work.

My question is regarding the iron-nickel alloys in the meteorite material (my apology for not beening clear).

In Iron Meteorites, there are two major alloys of iron-nickel:

Kamacite: a solid solution of around 7.5% nickel.
Taenite: a solid solution of more than 25 percent nickel.

There are also the possibilities of having Iron Carbides - solid solutions of Fe, Ni & Co with Carbon, such as Cohenite and Haxonite. But let us ignore those for the moment. If I recall, iron and nickel are always alloyed together unless in oxide or silicate form – in meteorites.

My question was, what happens to these concentrations of iron-nickel on forging and folding? Do they leave a pattern that would be pamor like? Or do they simply mix and are indistinguishable (in the iron and meteorite mix- if you were to make a blade from this material alone)?
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Old 9th August 2006, 03:23 PM   #49
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Quote:
When creating a mixture of “iron” and meteorite, what happens to the nickel in the process… does it “mix” or does it tend to separate and create “bands” of nickel in the iron (making its own pamor)?
The acid in the lime juice will etch the layers with nickel less than the ones without, and the arsenic/lime will darken them less; so the nickel-bearing layers will stand out and be lighter and more glossy (although the polish will depend on abrasives and method of their use, too). Phosphorus works the same way, the different alloys are effected by the acid differently. I have never done lime juice and arsenic to a differential phosphorus blade, but with regular etching solutions phosphorus iron etches less deeply and lighter in color, but does not retain its polish like steel with nickel or chrome.

How uniformly the nickel becomes mixed with the other metal depends on how it is worked, how many times the two metals get folded together. At eight folds, the narrowness of the layers and solid-state diffusion are starting to level out the appearance, at least to the naked eye (how uniform it will look also depends on how different the alloys are and how much those elements like to diffuse (Ni does not like to move very fast), and how hot the smith likes to work the metal). It takes ten to twelve folds to really get things smoothed out under magnification. The patterned panels on the knife I posted were folded four times, the base metal was folded eight before going into the mix. The base metal is much more uniform in between the nickel layers, where it got the extra folds. At four folds, the nickel layers are still really obvious, but the meteorite I used welded up so well I didn’t have to fold it many times to get clean metal, so the bright layers are undiluted 6% nickel meteorite.

If a smith were mixing meteorite & plain steel to make the bright layers in the pamor, he would fold it until it was visually uniform (from a foot or two away, at least - otherwise the patterning wouldn't stand out), but there would still be some amount of variation in the metal, quite a lot under the microscope.

Testing the brighter lines in pamor (or the brighter lines within the brighter layers) would get you higher percentage of meteorite material, if it was used.

To get a real big difference in color, I think you need at least 2-3 percent nickel (perhaps less if you’re mixing it with high P metal?), and the Prambanan meteorite has 10% Ni (28.3 ppm Ga, 190 ppm Ge, 4.2 ppm Ir) – I’ll take a wild guess and say the old timers would mix one part meteorite with four or five parts domestic metal, unless the keris was special, when they might bump it up to 33% -50% for the extra contrast that would impart. You’d probably see some degree of contrast all the way down to a one in ten ratio.
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Old 9th August 2006, 11:33 PM   #50
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I can only talk facts about the meteoritic material I myself have handled.

I welded small pieces of Arizona material together, then folded and welded at least seven times, but probably more likely nine or ten times, to make small, solid, clean billets of material that was 100% meteoritic material.

The small solid block of meteoritic material was then forged out to the point where it was starting to separate, which means it was about as thick as a piece of newspaper.

A piece was cut off and put between two pieces of iron about half inch thick.

Four of these pieces were made, then these four pieces welded together, forged out and folded five times to produce 128 nominal layers of the meteoritic material. However, don`t forget that this meteoritic material had---let us say---nine folds in it before it started to be worked as pamor, and there were four layers of it before the first pamor fold was done. That means the meteoritic material itself finished up as 1152 nominal layers.

At this level of layering, the nickelous parts of the original meteoritic material would have lost a lot of the ferric component. It was thin to begin with, and with every weld heat some ferric component would have been lost. If you look at the finished pamor under magnification it is difficult to see if the bright nickelous parts of this pamor have any joints at all.

From an academic point of view I have absolutely no idea what happens with the meteoritic material. From a practical point of view what I can see is an effect that looks very similar to plain, straight nickel.
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Old 11th August 2006, 03:55 PM   #51
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This probably goes without saying, but if anyone goes to the trouble of finding a lab they can work with, and a keris to test, please post the results here so we can have this thread again with some numbers to work with
I'll see if I can switch to a lab that does more trace elements for the tests I do on my steel.
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Old 11th August 2006, 06:30 PM   #52
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For you brave of heart...

Here is an old list...

Maybe, with a little soft shoe and sweet talk, someone could talk one of the following labs into doing some “unknown” testing... for feasibility. Maybe some students need some practice, or may want to do a paper or something on this subject. It would make an interesting thesis.
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