Examination of Novel Powdered Materials Prepared from Platinum Group Metals by Variants of the Hudson Method

By

N. Reiter and Dr. S. P. Faile

25 August 2004

Background:

From January to June of 2004, we continued our examination of claims related to the so- called "ORME" form of transition metals, as promoted since the 1980s by D. Hudson et al. Previously published work performed by us in 2003 related primarily to the attempted replication of anomalous forms of gold, with particular attention to the examples disclosed in Australian patent #AU3662489 (04-01-1990) awarded to David Radius Hudson.

While the unusual properties attributed to the ORME form of gold remain minimally documented and replicated, they are accompanied in lore and anecdote by claims of even more peculiar or dramatic behavior exhibited by the analagous forms of some platinum group metals. Most popular among speculative claims is iridium, which as disclosed by Hudson, exhibited the most dramatic anomalous physical effects, such as room temperature superconductivity (as ascertained by flux exclusion) and extreme apparent fluctuations in weight.

Evaluation Method and Procedures:

As we discovered in our investigation into ORME gold claims, it becomes after a point quite difficult to isolate empirical knowledge from second hand accounts and speculation. One particular personality long active in the genre has claimed that the ORME form of iridium was found to produce a strange antigravitational effect when rotated in a specific manner. Others active in the field have been cautious enough to state that no known positive replications of those particular claims exist.

For our evaluation, we turn once again to the Hudson Australian patent, which seems to provide the clearest or at least the most precise set of examples for replication. Of particular interest to us has been Example #3. We transcribe the example text herewith:

"EXAMPLE 3

The Preparation of Platinum Group Elements In Monoatomic State (ORMEs) From Pure Metals

The non-metallic, monoatomic transition elements of the platinum group are prepared as follows:

(1) A selected sample of pure metal or metal salts from the group platinum, palladium, ruthenium, osmium, rhodium, or iridium are pulverized to a finely divided powder.

(2) 5.0 g of a single select elemental metal powder is intimately blended with 30 g sodium peroxide and 10 g sodium hydroxide (silica free) in an agate mortar and pestle.

(3) The blended sample is placed in a zirconium crucible and fused over a Meeker burner at maximum heat for 30 minutes.

(4) After cooling the melt, the crucible is placed into a 600 ml beaker containing 300 ml of 6M HCl.

(5) The melt should completely dissolve into the HCl. The crucible is removed from the solution and rinsed with water, and the HCl solution is carefully inspected for any insoluble metals or metal oxides which, if present, must be filtered out and fused again as in step (2) above.

(6) The HCl solution is gently boiled down to just dry salts. "Just dry" is as defined in Example 1.

(7) The just dry salts are taken up in 300 ml of pH 1 HCl solution and then gently boiled down to salts again. The salts at this point, depending on the selected metal sample, are alkali chlorides together with alkali-cluster-noble metals-metal chlorides.

(8) The procedure of steps (6) and (7) is repeated four times, being careful not to bake the salts.

(9) The salts are diluted with 400 ml of deionized water.

(10) 30 ml of concentrated perchloric acid is added to the solution and then slowly boiled to fumes of perchloric acid.

(11) Steps (9) and (10) are repeated three additional times. If the solution salts out before fuming is achieved, it is necessary to add an additional 5 ml of perchloric acid to replace acid lost in fuming. If ruthenium or osmium is the select metal, steps (10), (11) and (12) must be carried out under reflux and washed back with water since ruthenium and osmium will volatilize. The salts at this point, depending on the selected metal sample, are alkali monoatomic noble metal oxides.

(12) The salts are diluted to 400ml with deionized water.

(13) The pH is adjusted very slowly with sodium hydroxide solution until the solution maintains the pH of 7.0 + 0.2 for more than 12 hours.

(14) Boil the solution for several hours, adding deionized water to maintain 400 ml during the entire boiling until a reddish-brown hydroxide precipitant is formed which is filtered on a fine fritted, glass filter.

(15) The hydroxide precipitant is dissolved off the fritted glass filter with 400ml of pH 1 HCl and then boiled for approximately ten minutes. If the sample contains rhodium or iridium, sodium bromate should be added as an oxidant prior to boiling.

(16) The solution is neutralized slowly with sodium bicarbonate to pH 7, and the solution is boiled again and allowed to cool.

(17) The precipitant which is formed is filtered again through a fine fritted glass filter. The material at this point, depending on the selected metal sample, is a monoatomic noble element hydroxide.

(18) The hydroxide together with the filter are vacuum dried at 120C for approximately 12 hours.

(19) The dried material is carefully transferred from the filter to a quartz ignition boat.

(20) The ignition boat is placed in a cold tube furnace and the temperature is slowly (2C/min) raised under a hydrogen atmosphere to 600C and held at this temperature for one hour and then slowly (2.5C/min) cooled down to room temperature under hydrogen and then the sample is purged with argon for approximately one hour to remove occluded hydrogen. The material, an ORME, will be a greyish-black powder and will be completely amorphous to x-ray analysis. In other words, a certified pure noble metal powder has been converted to a "non-analyzable" form.

At this point the ORMEs, depending upon the selected element sample, will be orbitally rearranged due to the d orbital hole or holes, i.e., positive hole(s). The ORMEs are identified as having an infrared doublet between 1400 and 1600 cm-1. The doublet indicates the presence of an electron pair moving between the d and s orbitals. "

In our initial evaluation of this generic "recipe", it became apparent that certain aspects were going to prove extremely problematic, and that we would not be able to perform a true replication of the art. The overwhelming problem was the procurement and useage of perchloric acid - a highly regulated and extraordinarily expensive oxidizer. After review of prices, safety requirements, availability, and permits, we decided that it was beyond our capacity as independent experimentalists to buy and accommodate perchloric acid. This being agreed upon, we decided nevertheless that it would be worth our while to attempt to use a modified version of the Hudson recipe to attempt to produce materials with unusual properties anyway - as sheer exploration!

It had become apparent to us in our examination of gold processing that a number of diverse recipes had been cited by experimenters - all producing precipitated powders with varying degrees of interesting anecdote attached. What could we discover from processing some platinum group metals with a simplified protocol based on Hudson's patent example as framework?

We settled on a basic processing recipe:

A small quantity of the platinum group metal in the form of a powder or shavings was fused with NaOH and sodium peroxide (both ACS grade - Alfa Aesar) in a zirconium foil (99.99%) boat over a propane flame for five minutes. Fusing was done in air. The ratio of the PG metal selected to sodium hydroxide and sodium peroxide was taken from the Hudson patent text: 5 to 10 to 30 respectively.

Following the fusing, the Zr boat was allowed to cool for five minutes before immersing it whole in a 1000 ml pyrex beaker filled typically with 300 to 500 ml of 6M HCl:H2O. Following the dissolution of the residues inside the Zr boat, the boat was removed, leaving a beaker of typically pristine solution, of distinctive color.

Concentrated NaOH solution was added slowly to the PGM solution to adjust pH until precipitation occurred. We then allowed the solution to rest overnight or until the precipitants had fully settled.

Precipitants were then separated, and washed with distilled water a minimum of three times. Final precipitants were then dried over a 200C hotplate, and initial properties of the resulting powders were examined and recorded. We then would typically anneal portions of the powders acquired in a tube oven under controlled atmospheres at temperatures between 200C and 500C.

In addition to establishing a baseline process recipe, we needed to derive an adequate set of criteria for evaluating any materials produced. In our previous discussions of anomalous forms of gold, we disclosed an interesting but yet undefined phenomenon that we referred to as grain hopping. With gold derived powders and some powders derived from natural pricipitatates, we observed a minor Meisner Effect - like repelling of select individual grains in the aggregate. Would iridium or other PGM orme powders exhibit this same property? Anecdote would suggest so, since iridium orme was said to be more dramatic in its physical anomalies than gold. Could we directly measure the resistivity of bulk powders as an indicator of actual room temperature superconductivity?

These two criteria would augment the overall qualitative evaluation of properties. We now disclose basic appearances and properties of the materials we worked with. A simple test for comparative electrical conductivities, and results, will follow.

Iridium:

Three batches of iridium based material were prepared. In all three cases, the iridium powdered metal (-325 mesh 99.99% from Alfa Aesar) fused rapidly with the sodium compounds. Upon immersion in the dilute HCl, the fused material dissolved completely into a brilliant and beautiful deep blue-violet solution. With pH adjustment using NaOH, we observe the beginning of precipitation at about pH 6. Precipitates were extremely fine grained and of a deep cobalt blue color. Speed with which precipitation occurred may depend on relative ratio of water to HCl. In all cases, the dried precipitate was of a deep nearly irridescent indigo-black, with some hues of blue and green seen.

We observed that the iridium precipitate did seem to be quite vigorous in its propensity for grain hopping; at least matching that of gold based powders. Some smaller number of individual grains appeared to be ferromagnetic, attracted and dragged by a small rare earth magnet held under a plastic weighing dish in which a quantity of the powder is placed.

The anecdotal source mentioned previously who claimed dramatic properties for iridium orme disclosed an embodiment that supposedly resulted in the levitation of a rotating ceramic disk. It was claimed that iridium orme powder had been blended into a green clay slurry, then fired to form a ceramic disc that when spun on its axis, would levitate. In May, 2004, we took a small quantity of our own powder (about 50 mg) and dispersed it into a zirconia silicate cement which was cast into a small 2 inch diameter hexagonal "chip". After firing at 200C, we looked for transient weight changes after spinning or accerating the disc laterally. None were observed to the resolution of our balances.

Attempts to quantify the overall magnetic properties of the powder were inconclusive, as diamagnetic properties of plastic or glass weighing dishes seemed to swamp any foces resulting from the small quantity of powder at our disposal. We also suspected that any aggregats of the grain hopping force may have been counterbalanced somewhat by the stronger attraction of selected grains.

In early spring of 2004, we observed that the Ir precipitate, while retaining most of its grain hopping potential, appeared to be adversely affected by long exposure to atmospheric moisture. A short annealing (15min. typ.) in air at 300C would restore the vigor of the grain hopping. This was also noted with the material derived from rhodium, described next.

PHOTO of Ir Orme

PHOTO of magnet and disc

Rhodium:

325 mesh rhodium powder (99.99% pure Alfa Aesar) fused into a dark glassy mass with our sodium components with nearly the same appearance as iridium. However, upon dissolution in HCl:H2O, a dark olive green solution resulted. Precipitate was brownish green and finely flaked. When washed and dried, the powder resulting was approximately the color of coffee or cocoa powder. Before and after annealing, we observed some amount of grain hopping, though comparatively less than with iridium derived material. Only one batch of Rh material was prepared.

PHOTO of Rh Orme

Platinum:

Perhaps 100mg of very tiny niblets of platinum thermocouple wire (26 ga) were fused with the sodium compounds. Yet again, the glassy material formed from fusing closely resembled that of the previous materials, however with Pt, the color of the fused mass was lighter and slightly yellowish. In HCl:H2O, it dissolved without color. Precipitate was whitish, and when washed and dried, assumed a cream color. This color remained consistent after annealing. Very little grain hopping was observed - the powder appeared to be primarily inert and without any special property. Only one batch of Pt material was prepared.

PHOTO of Pt orme

Gold:

Although not included in example #3 of the Hudson patent, we felt that it might be rewarding to try the dual sodium compound recipe with gold. About 100 mg of minute shavings of 99.99% gold were used. Fusing in the Zr boat seemed problematic, with the gold not easily wetting. After about three extra minutes of fusing time, the mass appeared to be fairly homogeneous, and thus was cooled and added to the HCl:H2O. The resulting solution was a light yellow green in color - resembling the dissolved Au from the middle steps of Hudson's patent example #1. With pH correction, we acquired only a slight amount of precipitate, of a faint cream color. When carefully washed three times and dried, we recover a sparse heterogeneous mix of white flakes, white waxy looking salts, and purple colloidal gold dispersed in said waxy salts. Before and after annealing, we observe a slight amount of grain hopping - more than platinum but less than rhodium powders. The grain hopping property diminished within 48 hours - an effect seen previously in our early experiments with gold ORME.

PHOTO of Au Orme

Rhenium:

While technically not one of the PGM, rhenium is mentioned by Hudson et al as having an ORME form. During our experiments with Th and U doped fungi, Re was found on multiple occasions to be present in the final EDS analysis of cultures in which unusual alterations of radioactive decay were observed. We procured a small quantity of -325 mesh 99.99% Re from Alfa Aesar, and applied it to our generic recipe. A clear solution results when the fused mass in the Zr boat dissolves in HCl:H2O. Adjustment to about pH 10 caused a very delicate hazy white precipitate to form. After settling, washing, and drying, we recover a slight amount of slightly waxy pearl white powder. When tested for grain hopping, the Re precipitate was found to be very poor - almost completely inert.

PHOTO of Re Orme

Electrical Conductivity Tests:

Early in our investigations, it was suggested that simple direct measurements of the resistance of a powder aggregate might provide clues as to whether room temperature superconductivity had been achieved. As far as can be ascertained from literature, simple oxides of platinum group elements should be quite high in resistivity, well above values for metal or metalloid powder. It has been frequently observed that when finely divided powders of even highly conductive metals are measured in a bulk column or aggregate, the total electrical resistance of said column is quite high. A useful example is nickel powder. Could a bulk resistance measurement of our precipitated powders be compared to known metal powders?

Approximately equal amounts by volume of our assorted powder products were tapped and packed into the edge of a weighing dish, and contacted at 3mm spacing with meter probes from our Keithley 175 multimeter. A similar quantity of one micron 99.99% nickel powder was examined as a control. What we observe is interesting, although our technique is admittedly quite crude. The following figures represent the average of five readings each in different spots:

Ni powder: >200M-ohms

Ir precipitate: 47M-ohms

Rh precipitate: 175M-ohms

Pt precipitate: >200M-ohms

Au precipitate: 188M-ohms

Re precipitate: >200M-ohms

Admittedly, many sources of error could enter into these figures. Grain size, packing, purity, residual oxide and chloride species, all could play a role. Yet in the most outward way, it does appear as though the Ir precipitate has an appreciable conductivity. It is followed in series by the Rh and Au materials. The Au precipitate over time has continued to change color toward a purple hue, indicating the presence of colloidal metallic gold. We suggest that the ordering of conductivity among Ir, Rh, and Au material does seem to correspond with the degree and robustness of the grain hopping effect.

Several metal powders (Al, Zn, and Cu) were examined in plastic weighing dishes for signs of grain hopping. No signature effect was noted. Were grain hopping an electrostatic or electret artifact, it should be quite apparent with any high dielectric powder, and absent with metallic powders. This poses an interesting puzzle with respect to the Ir precipitate, as it does display an apparent electrically conductive nature, yet exhibits the most robust grain hopping effect of any of our produced materials.

The Chemistry of the PGM Precipitates:

What would conventional chemistry predict as to the compositions of our materials? Given our technique, we probably should be ending up conventionally with platinum group oxides, hydroxides, or oxychlorides. Currently, our analytical resources as far as EDS, XRD, and IR Spectroscopy have become quite limited, thus forcing our detective work along old fashioned routes. In the case of our Ir and Rh materials, the CRC Handbook of Chemistry and Physics gives its ever practical clues. IrO2 is listed as a black or blue crystal, in the di-hydrate form it is an indigo color. Rh in the form of RhO2 is said to be brown, and in the di-hydrate form is olive green. Thus for both of these elements, we find that the colors of our precipitates do indeed match the traditional published properties of the hydrated dioxide.

In the Australian patent by Hudson, this is discussed. Hudson’s claim appears to be that the precipitates formed from his processing of PGM elements are in the form of oxides and hydrides containing unusual or surprising properties due to their orbitally re-arranged "orme" character.

General Conclusions and Discussion:

Our experiments with platinum group elements, plus a novel ORME recipe for gold and for Re have provided some interesting results, despite the ultimate failure to replicate certain specific dramatic claims. We summarize and disclose the following:

1. A simplified variant of the D.R. Hudson Australian patent example #3 for PGM elements was found to produce precipitates for Ir, Rh, and Pt starting metals. When applied to Au and Re, the process also produced precipitated material.
2. In the case of at least two of the PGMs (Ir and Rh) the resulting precipitates resemble the classical descriptions of the dioxide or hydrated oxide forms of said elements.
3. Dramatic weight alteration claims made for Ir derived powders encapsulated in ceramic discs and rotated were not successfully replicated.
4. A still ill-defined phenomenon resembling Meisner Effect flux exclusion referred to by us as grain hopping was observed to a robust degree in Ir material, and to a lesser extent in Rh and Au derived materials.
5. A crude measurement of electrical resistivity in the powders from our process showed a surprisingly conductive nature for the Ir material.
6. This above measurement may relate to the vigor of the grain hopping effect observed in the same material (Ir derived powder).
7. In a general sense, we have apparently found some corroboration with the claims of Hudson et al that Ir ORME is the most dramatic of elements for physical anomalies. Among our experiments, Ir did indeed produce the most interesting results.

Presently, we are limited in our further directions for investigating claims of unusual matter or ormes. Procurement of a small quantity of perchloric acid would allow us to perform a true replication of the example #3 steps. If such can be obtained, our plan is to focus on iridium. Apart from this effort, we will continue to characterize and understand the grain hopping effect. As in our past ventures, we eagerly invite dialogue with other researchers interested in replication, or clarification of our procedures.

As is well known among those familiar with the lore of ORMEs, unusual biological and psycho-interactive effects are frequently claimed for human ingestion of small quantities of materials. We have explored this to a very limited degree with respect to Ir and Rh precipitates. Results were extremely subjective, and out of the scope of this report.

During the experimental phase of this project, we did not neglect looking into historical accounts of "strange matter" or matter exhibiting implausible behavior. Perhaps the closest corollary surround some of the lesser known claims of Dr. Wilhelm Reich, with respect to materials he referred to as Orene, Orite, Brownite, and Melanor. While lacking any known critical replication since their disclosure during the 1950s, Reich was quite specific in his accounts of these materials, said to be "pre-atomic." In particular, the white powder called Orene, found near vessels containing alkaline aqueous solutions, bears an interesting resemblance to the "g-orme" of Hudson. Both materials have been said to produce strong bio-interactive effects. Nevertheless, until such a time as we can better verify such material's existence, as well as come up with a coherent model same, there is little more we can do except note the resemblance and speculate.

Our overall investigation into the matter of David Hudson's claims and ORME matter has carried us along for over a year. While we have not successfully verified the more dramatic claims made for both gold and PGMs, we have seen evidence to suggest that the claims are not entirely without basis in empirical fact. Whether some non-intuitive but otherwise mundane explanation for grain hopping will arise or not, we cannot yet say.

In closing, we would like to thank the following parties for their help and participation: Mr. Art Ziegler, Mr. Barry Carter, and the members of the Vortex on-line science discussion group, chaired and operated by Mr. Bill Beaty.