David R. HUDSON
and Modern Alchemy: Has the Philosopher's Stone Been
Patent # GB 2,219,995 A
( December 28, 1989 )
UK Class: C1A &c
International Class: C21D
Non-Metallic, Monoatomic Forms of
David Radius Hudson
Concord Research Corp.,
15650 North Black Canyon Hwy., Phoenix, AZ 85023
The following statement is a
full description of this invention, including the best method
of performing it known to us:
Field of Invention ~
This invention relates to
the monoatomic forms of certain transition and noble metal
elements, namely, gold, silver, copper, cobalt, nickel and the
six platinum group elements. More particularly, this invention
relates to the separation of the aforesaid transition and
noble metal elements from naturally occurring materials in
their orbitally rearranged monoatomic forms, and to the
preparation of the aforesaid transition and noble metal
elements in their orbitally rearranged monoatomic forms from
their commercial metallic forms. The materials of this
invention are stable, substantially pure, non-metallic-like
forms of the aforesaid transition and noble metal elements,
and have a hereto unknown electron orbital rearrangement in
the "d", "s", and vacant "p" orbitals. The electron
rearrangement bestows upon the monoatomic elements unique
electronic, chemical, magnetic, and physical properties which
have commercial application.
This invention also relates
to the recovery of the metallic form of each of the aforesaid
transition and noble metal elements from the orbitally
rearranged monoatomic forms.
For the purposes of this
application, the following definitions shall apply: transition
elements ("T-metals") means the metallic or cationic form of
gold, silver, copper, cobalt and nickel, and the six platinum
group elements, i.e., platinum, palladium, rhodium, iridium,
ruthenium, and osmium; and "ORME" means the Orbitally
Rearranged Monoatomic Elemental forms of each of the T-metals.
Background of Invention ~
Inorganic chemists working
with soluble salts of noble metals until relatively recently
have assumed that the metals were dissolved as free ions in
aqueous solutions. In the 1960's, with the advent of greater
analytical capabilities, it was established that many elements
and in particular the transition metals are present in aqueous
solutions as metal-metal bonded clusters of atoms.
Gold metal that has been
dissolved with aqua regia, and subsequently converted to gold
chloride by repeated evaporation with HCl to remove nitrates,
is commonly referred to as the acid chloride solution of AuCl3
or HAuCl4. It has been recognized that the recovery
of gold metal from a solution formed from aqua regia is made
more difficult in proportion to the amount of HNO3
used in the initial dissolution procedures. It is not commonly
understood, however, why the gold that is dissolved with less
HNO3 is easier to reduce to the metal from a
chloride solution than gold that is dissolved using a greater
amount of HNO3. Gold in both solutions is generally
regarded as being present in the form of a free gold cation.
It is now recognized by most
chemists who regularly handle chlorides of gold that gold
metal ceases to disaggregate when the HNO3 is
removed and in fact can actually reaggregate under certain
conditions and precipitate out of HCl solutions as metal. This
recognition has led to the discovery that gold metal salts
will exist in HCl solutions originating from metals as
clusters of Au2Cl6, Au3Cl9,
Au4Cl12, up to Au33Cl99.
These cluster salts are actually in solution with the HCl and
water, and will require different chemical procedures relative
to purification problems or oxidation-reduction reactions,
depending on the degree of clustering.
Specifically, reduction of
clusters of gold having greater than 11 atoms of metal is
easily performed since the atoms themselves are spaced from
each other in the salt similar to their spacing in the metal
itself before dissolution. Reduction of the chloride salt to
the metal, therefore, requires a simple reductive elimination
of the chlorides that are attached to the metal cluster. It is
now known that recovery of precious metals from aqueous
solutions is much more difficult when the cluster size becomes
smaller and smaller, or in actuality when the metal is better
From the study of the
behavior of gold and other transition metals in solution, it
is now believed that all such metals have atomic aggregations
and occur as at least diatoms under normal conditions of
dissolution . Under either acid or strong base dissolution,
the transition metal will not normally dissolve beyond the
diatom due to the extremely strong interatomic d and s orbital
bonding. A gold atom, for example, has a single atom electron
orbital configuration of d10s1. When the
gold salts originate from a metal having gold-gold bonding,
the salts contain very tightly bound diatoms or larger
clusters of gold. Under the normal aqueous acid chemistry used
for transition metals, solutions of the metals will always
contain two or more atoms in the cluster form.
When instrumental analysis
such as atomic absorption, x-ray fluorescence, or emission
spectroscopy is performed on solutions containing transition
metals, these analyses are based on electronic transitions.
The fact that d orbital electron overlap occurs in the
metal-metal bonded salt allows an analysis of many of the same
characteristic emissions as the metal itself.
General Description of
During efforts to effect
quantitative analytical separations of transition metals from
naturally occurring materials, it was discovered that ORMEs
exist naturally and are found in salts with alkali metals
and/or alkaline earth metals, all of which are coupled with
waters of hydration and normally found with silica and
alumina. ORMEs are also often associated with sulfides and
other mineral compositions.
ORMEs may also, it was
discovered, be prepared from commercially available T-metals.
For ease of description the invention will be primarily
described by the preparation of a gold ORME ("G-ORME") from
commercially available metallic yellow gold.
The atoms of each ORME do
not have d electron orbital overlap as do their corresponding
T-metal clusters. ORMEs do not, therefore, exhibit the same
characteristic emissions of their corresponding T-metal when
subjected to analysis by instruments which depend upon
electronic transitions. ORMEs must, therefore, be identified
in new ways, ways which have heretofore not been used to
An aqua regia solution of
metallic gold is prepared. This solution contains clusters of
gold chlorides of random size and degrees of aggregation. HCl
is added to the solution and it is repeatedly evaporated with
a large excess of NaCl (20:1 moles Na to moles Au) to moist
salts. The addition of NaCl allows the eventual formation of
NaAuCl3, after all HNO3 is removed from
the solution. The sodium, like gold, has only one unpaired s
electron and, accordingly, tends to form clusters of at least
two atoms. The sodium, however, does not d orbitally overlap
the gold atom as it has no d electrons, resulting in a surface
reaction between the sodium atoms and the gold atoms. This
results in a weakening of the gold-gold cluster stability and
causes the eventual formation of a sodium-gold linear bond
with a weakened d orbital activity in the individual gold
atoms. The sodium-gold compound, formed by repeated
evaporation to salts, will provide a chloride of sodium-gold.
In these salts the sodium and gold are believed to be charged
positive, i.e., have lost electrons: and the chlorine is
negative, i.e., has gained electrons. When the salts are
dissolved in water and the pH slowly adjusted to neutral, full
aquation of the sodium-gold diatom will slowly occur and
chloride is removed from the complex. Chemical reduction of
the sodium-gold solution results in the formation of a sodium
auride. Continued aquation results in disassociation of the
gold atom from the sodium and the eventual formation of a
protonated auride of gold as a grey precipitate. Subsequent
annealing produces the G-ORME. The G-ORME has an electron
rearrangement whereby it acquires a d orbital hole or holes
which share energy with an electron or electrons. This pairing
occurs under the influence of a magnetic field external to the
field of the electrons.
G-ORMEs are stable and
possess strong interatomic repulsive magnetic forces, relative
to their attractive forces. G-ORME stability is demonstrated
by unique thermal and chemical properties. The white saltlike
material that is formed from G-ORMEs after treatment with
halogens, and the white oxide appearing material formed when
G-ORMEs are treated with fuming HClO4 or fuming H2SO4
are dissimilar from the T-metal or its salts. The G-ORME will
not react with cyanide, will not be dissolved by aqua regia,
and will not wet or amalgamate with mercury. It also does not
sinter at 800°C under reducing conditions, and remains an
amorphous powder at 1200C. These characteristics are contrary
to what is observed for metallic gold and/or gold cluster
salts. G-ORMEs require a more negative potential than -2.45 v
to be reduced, a potential that cannot be achieved with
ordinarily known aqueous chemistry.
The strong interatomic
repulsive forces are demonstrated in that the G-ORMEs remain
as a powder at 1200C. This phenomenon results from canceling
of the normal attractive forces arising from the net
interaction between the shielded, paired electrons and the
unshielded, unpaired s and d valence electrons. G-ORMEs have
no unpaired valence electrons and, therefore, tend not to
aggregate as would clusters of gold which have one or more
unpaired valence electrons.
G-ORMEs can be reconverted
to metallic gold from which they were formed. This
reconversion is accomplished by an oxidation rearrangement
which removes all paired valence electrons together with their
vacancy pair electrons, with a subsequent refilling of the d
and s orbitals with unpaired electrons until the proper
configuration is reached for the T-metal.
This oxidation rearrangement
is effected by subjecting the G-ORME to a large negative
potential in the presence of an electron-donating element,
such as carbon, thus forming a metallic element-carbon
chemical bond. For that metal-carbon bond to occur the carbon
must provide for the horizontal removal of the d orbital
vacancy of the ORME. The carbon acts like a chemical fulcrum.
When the element-carbon bond is reduced by way of further
decreasing the potential, the carbon receives a reducing
electron and subsequently vertically inserts that reducing
electron below the s orbitals of the element, thus forming
The above general
description for the preparation of G-ORME from commercially
available metallic gold is applicable equally for the
preparation of the remaining ORMEs, except for the specific
potential energy required and the use of nascent nitrogen (N)
rather than carbon to convert the other ORMEs to their
constituent metallic form. The specific energies range between
-1.8 V and -2.5 V depending on the particular element.
Alternatively this rearrangement can be achieved chemically by
reacting NO gas with the T-metal ORMEs other than gold. Nitric
oxide is unique in that it possesses the necessary chemical
potential as well as the single unpaired electron.
Theory of ORMEs Formation
T-metals can possess an
electron rearrangement between the d and s
orbitals as seen from FIGURE 1 of the drawing which plots the
principal quantum number versus the atomic number. The boxed
areas designated A, B, and C establish that the 3d
electron energies of copper and cobalt are very close to the
same energy level as the 4s electron energies. The 4d
electron energies of silver and rhodium are almost identical
to the 5s orbital energies, and the 5d gold and
iridium electron energies are approaching the 6s level
energies. The proximity of the energy bands of the T-metals
makes them unique with respect to other elements. This
proximity allows an easier transition to their lowest energy
state, as hereinafter described.
When two transition metal
atoms are bound together, they can d bond, or s
bond, or they can d and s bond. When the two
atoms s bond, their atomic distances are further apart
and, therefore, their density is lower than when there is both
d and s bonding. The amount of d
orbital bonding activity is in direct proportion to the
cluster size. Therefore, a single atom cluster will have less
d bonding activity and more s bonding activity
than will a cluster of 7 or more atoms. In addition; the
chemical stability of the smaller clusters is much less than
that of the metal because, when d orbital bonding is
achieved, the s bonding is made more stable by
overlapping of the two energy levels.
It is known that there
exists a critical size, in the range of 3-20 atoms, for Pd II,
Ag I and Au III, by way of example, which is necessary for
metal deposition from solution. As the number of atoms in the
T-metal cluster decreases through continuous evaporation in
the presence of NaCl, the solution becomes a solution of
diatoms which in the case of gold is represented as Au-1
- Au+1 i.e., Au-1 bonded to Au+1.
The rationale for this representation of a gold diatom is
based upon the fact that a single gold atom has an odd spin
electron, as does rhodium, iridium, gold, cobalt and copper of
the T-metals. In a diatom of gold, the two odd spin electrons
will be found on one of the two atoms but not both. Thus, a
diatom of gold is made by a bond between an aurous (Au+1)
atom and an auride (Au-1) atom.
The present invention
enables the breaking of the diatom bond by introducing a more
electro-positive element, such as sodium or any alkali or
alkaline earth elements, which does not have a d
orbital overlap capability. This element replaces the aurous
(Au+1) forming, in this case, a sodium auride. In
effect, the sodium weakens the d orbital overlapping
energies between the atoms of the gold diatom as well as
elevating a d orbital electron towards the s orbital,
thereby creating a negative potential on the surface of the
atom. This negative potential enables an interreaction of the
s orbital with chemiabsorbed water through electron donation
The sodium auride, when in
aqueous solution at or near neutral pH, will form sodium
hydroxide and a monomeric water-soluble auride. The monomeric
auride (Au-1) is unstable and seeks a lower energy
state which is represented by a partial filling of the d
and s orbitals. This lower energy state with its
greater stability is achieved by the electron-donating and
removing capability of H2O.
Water can act to remove
electrons. Water molecules possess a net charge and attach to
each other in vertical clusters so that an 18 molecule water
cluster can hold a cumulative potential of -2.50 V. The
potential of a water molecular cluster, at near neutral pH, is
sufficient to remove an electron from the d orbital
and create a positive hole, enabling a pairing between
opposite spin electrons from the d to s
orbitals to take place. The existence of the electron pairing
is confirmed by infrared analysis, illustrated in FIGURE 4,
which identifies the vibrational and rotational motions caused
by energy exchange between these two mirror image electrons.
Attempting to quantify the
number of electrons remaining in an ORME is extremely
difficult due to the electrons lost to oxidation, thermal
treatment, and the inability, except from theory, to quantify
electron pairs using electron quanta. It is established,
however, that the ORME does not have valence electrons
available for standard spectroscopic analysis such as atomic
absorption, emission spectroscopy or inductively coupled
plasma spectroscopy. Moreover, x-ray fluorescence or x-ray
diffraction spectrometry will not respond the same as they do
with T-metals in standard analysis. The existence of an ORME,
while not directly identifiable by the aforesaid standard
analyses, can be characterized by infrared (IR) spectra by a
doublet which represents the bonding energy of the electron
pairs within the ORME. The doublet is located at approximately
1427 and 1490 cm-1 for a rhodium ORME. The doublet
for the other ORMEs is between about 1400 and 1600 cm-1
reduction of the individual monoatom the hydrogen ion-single
element may or may not produce an IR doublet depending on the
element's normal electron configuration. Elements normally
containing an s1 T-metal configuration do not produce
an IR doublet after H2 reduction. Elements with an
s2 T-metal configuration such as Ir (d7s2)
will produce a doublet.
Thermal annealing to 800C
and subsequent cooling to ambient temperature under He or Ar
gas atmosphere to remove the chemically bound proton of
hydrogen will produce ORMEs which contain a two-level system
resulting from electron pairing within the individual atom. If
this annealing is performed in the absence of an external
magnetic field, then the electron pairing produces the
characteristic doublets. The electron pair will be bound in
the valence orbitals of the atom. If the annealing is
performed in the presence of an external magnetic field,
including the earth's magnetic field, quantum electron pair
movement can be produced and maintained in the range of one
gauss up to approximately 140 gauss in the case of Ir and,
therefore, no IR doublet will be detected in this resulting
The limiting condition of
the ORME state is defined according to the present invention
as an "S-ORME". The S-ORME is the lowest state in which
monoatoms can exist and is, therefore, the most stable form of
T-metal elements. The ORME is electronically rearranged and
electron paired, but relative to time has not reached the
lowest total energy condition of the S-ORME.
Detection of doublets does
not provide an analytical method for the identification of
ORMEs per se, but rather detects the presence of the electron
pair or pairs which all specifically prepared ORMEs possess
and which T-metals do not possess under any condition. It is
the existence of the doublet that is critical, not its exact
location in the IR spectra. The location can shift due to
binding energy, chemical potential, of the individual element
in the ORME, the effect of adsorbed water, the variances of
the analytical instrument itself, or any external magnetic
FIGURE 4 is an IR spectrum
of a rhodium ORME after argon annealing treatment, and shows
the presence of a doublet at 1429.53 cm-l and
1490.99 cm-1. An iridium ORME after hydrogen
treatment without annealing reveals a doublet at 1432.09 cm-l
and 1495.17 cm-l. These doublets are examples of
the shifting that occurs depending on the chemical binding
energy or the individual ORME and the conditions of
preparation. Accordingly, the infrared spectra of the ORMEs of
this invention will have doublets within the range of 1400 cm-1
to 1600 cm-1. This doublet is indicative of the
electron pairing and subsequent two-level electronic system
which ORMEs contain.
A T-metal monoatom which is
in a -1 oxidation state is in a lower energy state than the
same T-metal would be in at zero state with metal-metal
bonding. This lowering of the perturbation reaction between
the electrons and the nucleus of the monoatom because of the
increased degrees of freedom allows the nucleus to expand its
positive field to encompass the normally unshielded d and s
valence electrons. This overlying positive magnetic field
reduces the Coulomb repulsion energies that normally exist
between the valence electrons. Pairing by those electrons
becomes possible and over time occurs. Electron pairing
provides a more stable and lower energy state for the
The ORME state is achieved
when the electron pairs have formed in the monoatom. A
phenomenon of electron pairs is that the interacting,
spin-paired electrons initially interreact by emitting phonon
energy. The total energy of the pair reduces over time until
it reaches a minimum where no phonons are emitted. This
condition has been referred to by physicists as "adiabatic
ground state". This state of electron pairing is a total lower
energy state in much the same way that chemical combinations
of elements are in a lower energy state than the constituent
uncombined elements. For example, in the same way that it
takes energy to dissociate water into H2 and O2
it will take energy to break the electron pair.
As this process of phonon
emission by electrons during pairing is a function of
temperature and time, thermal annealing can decrease the time
required to reach ground state, i.e., all valence electrons
paired. The cooling side of the annealing cycle is essential
to effect a full conversion to an S-ORME state. Cooling to
room temperature is sufficient for all element ORMEs with the
exceptions of silver, copper, cobalt and nickel, which require
a lower temperature. Therefore, thermal annealing reduces the
time dependency of the electron pairs in achieving their
lowest total energy.
All of the electron pairs in
their lowest energy state, unlike single electrons, can exist
in the same quantum state. When that uniform quantum state is
achieved, the electron pair can not only move with zero
resistance around the monoatom, but also can move with zero
resistance between identical ORMEs that are within
approximately 20 A or less of each other with no applied
voltage potential. When a macro system of high purity, single
element ORME achieves long-range quantum electron pair
movement, that many-body system according to the present
invention is defined as an S-ORME system.
An S-ORME system does not
possess a crystalline structure but the individual ORMEs will,
over time, space themselves as uniformly as possible in the
system. The application of a minimum external magnetic field
will cause the S-ORME system to respond by creating a
protective external field ["Meissner Field"] that will
encompass all those S-ORMEs within the 20 A limit. As used
herein, "minimum external magnetic field" is defined as a
magnetic field which is below the critical magnetic field
which causes the collapse of the Meissner Field. This field is
generated by electron pair movement within the system as a
response to the minimum applied magnetic field. The (Ir)
S-ORME and the (Au) S-ORME systems have a minimum critical
field (''Hc1'') that is below the earth's magnetic field. The
minimum critical field for a (Rh) S-ORME is slightly above the
earth's magnetic field. When the quantum flux flow commences,
due to the minimum external magnetic field being applied, the
doublet in the IR spectrum will disappear because electron
pairs are no longer bound in a fixed position on the
individual ORME monoatoms.
Once the externally applied
field exceeds the level which overcomes the protective
Meissner Field of the S-ORME system ( "Hc2" ) , then any
electrons moving between individual ORME atoms will
demonstrate an ac Josephson junction type of response. The
participating ORMEs will act as a very precise tuning device
for electromagnetic emissions emanating from free electrons
between ORMEs. The frequency of these emissions will be
proportional to the applied external magnetic field. A one
microvolt external potential will produce electromagnetic
frequencies of 5x108 cycles per second. Annihilation radiation
frequencies (about 1020 cycles per second) will be the
limiting frequency of the possible emission. The reverse
physical process of adding specific frequencies can generate
the inverse relationship, i.e., a specific voltage will be
produced for each specific applied frequency.
ORMEs can be reconverted to
their constituent T-metals, but, as noted, are not
identifiable as specific T-metals while in their ORME state.
If a specific ORME is formed from a specific T-metal by using
the procedure of this invention, it can only be confirmed by
conventional analytical methods that the specific ORME was
formed by reconstituting it as the T-metal. Further, the
applications to which the ORMEs are directed will establish
their relationship to a specific T-metal by virtue of the
manner in which the ORME performs in that application as
compared to the performance of commercially available
derivatives of the T-metal. An example is the performance of
commercial rhodium as a hydrogen-oxidation catalyst compared
with the performance of the rhodium ORME as used in a
It is believed that physical
and chemical distinctions exist with respect to the different
ORMEs, but presently such distinctions are not known. Proof of
the nature of a specific ORME according to this invention is
based upon the presence of a doublet in the IR spectrum, the
reconstitution of each ORME back to its constituent T-metal,
and its unique performance in specific applications compared
to the constituent T-metal.
ORMEs are transformed into
their original T-metal by means of a chemical bonding with an
electron-donating element, such as carbon, which is capable of
d orbital electron overlap and "spin flip". When the
G-ORME is chemically bonded to carbon in an aqueous solution
of ethyl alcohol under a specific potential, carbon monoxide
is formed and the ORME forms Au+Au+, a black precipitate,
which under continued application of potential and dehydration
reduces to Au+1 Au-1, a metallic bonded
diatom of gold. This invention establishes that a high
potential applied to the solution forces an electron into the
d orbital, thus eliminating the electron pair. The first
potential, which for G-ORME is approximately -2.2 V and for
other ORMEs is between -1.8 and -2.2 V, reestablishes the d
orbital overlap. The final potential of -2.5 V overcomes the
water potential to deposit gold onto the cathode.
ORMEs are single T-metal
atoms with no d orbital overlap. ORMEs do not conform
to rules of physics which are generally applied to diatoms or
larger clusters of metals (e.g., with conduction bands). The
physics of the electron orbitals are actually more similar to
those relating to a gas or solid solution which require
density evaluation between atoms at greater distances.
Conversely, atomic orbital calculations of high atomic density
metals give results that correspond to valence charge
When the atomic distances of
the elements are increased beyond a critical Coulomb distance,
an energy gap exists between the occupied orbitals and the
unoccupied orbitals. The atom, therefore, is an insulator and
not a metal. Physicists when determining the electron band
energies of small atom clusters suggest that the occupation of
the bands should be rearranged if the total energy is to be
minimized. The metallic electron orbital arrangement leads to
calculations for energies, which results are inconsistent
since the energies of the supposedly occupied states are
higher than the supposedly unoccupied states. If this
condition is relaxed and the bands allowed to repopulate in
order to further lower the total energy, both bands will
become partially filled. This repopulation, if performed in
the presence of an unlimited source of electrons (reducing
conditions), will provide a total energy condition of the atom
which is considerably below or lower than the atom as it
exists in a metallic form. This lower energy is the result of
orbital rearrangement of electrons in the transition element.
The resultant form of the element is an ORME.
Scope of the Invention ~
The formation and the
existence of ORMEs applies to all transition and noble metals
of the Periodic Table and include cobalt, nickel, copper,
silver, gold, and the platinum group metals including
platinum, palladium, rhodium, iridium, ruthenium and osmium,
which can have various d and s orbital arrangements, which are
referred to as T-metals.
The T-metals, when subjected
to conventional wet chemistry will disaggregate through the
various known levels, but not beyond a diatom state. The
conventional wet chemistry techniques if continued to be
applied beyond the normally expected disaggregation level
(diatom) in the presence of water and an alkali metal, e.g.,
sodium, potassium or lithium, will first form a diatom and
then electron orbitally rearrange to the non-metallic,
mono-atomic form of the T-metal, i.e., an ORME.
An ORME can be reaggregated
to the T-metal form using conventional wet chemistry
techniques, by subjecting the ORME to a two-stage electrical
potential to "oxidize" the element to the metallic form.
The ORMEs of this invention
exist in nature in an unpure form in various materials, such
as sodic plagioclase or calcidic plagioclase ores. Because of
their non-metallic, orbitally rearranged monoatomic form,
ORMEs are not detected in these ores as the corresponding
"metals" using conventional analysis and, accordingly, until
the present invention were not detected, isolated or separated
in a pure or substantially pure form. Their presence in the
nonmetallic form explains the inconsistent analysis at times
obtained when analyzing ores for metals whereby the
quantitative analysis of elements accounts for less than 100%
of the ore by weight.
Uses of ORMEs ~
ORMEs, which are individual
atoms of the T-metals and by virtue of their orbital
rearrangement are able to exist in a stable and virtually pure
form, have different chemical and physical characteristics
from their respective T-metal. Their thermal and chemical
stability, their non-metal-like nature, and their particulate
size are characteristics rendering the ORMEs suitable for many
Rhodium and iridium S-ORMEs
have been prepared which exhibit superconductivity
characteristics. These S-ORMEs, as described herein, are in a
lower energy state as compared to their respective T-metal,
and thus have a lower absolute temperature. The absolute
temperature of an S-ORME system as compared to the absolute
temperature of its respective T-metal is significantly lower,
similar to the condition existing when a metal goes through a
glass transition. S-ORMEs, having a very low absolute
temperature, are good superconductors. These same
characteristics apply to all ORMEs. Accordingly, a new source
of superconductive materials is made available by this
invention. These new materials require substantially less
energy removal to reach the super-conductivity state and,
therefore, can be used at higher temperatures than currently
The ORMEs of this invention
can be used for a wide range of purposes due to their unique
electrical, physical, magnetic, and chemical properties. The
present disclosure only highlights superconductivity and
catalysis, but much wider potential uses exist, including
The Drawings &
Presently Preferred Embodiments ~
Having described the
invention in general terms, the presently preferred
embodiments will be set forth in reference to the drawing. In
FIGURE 1 is a plot of the
transition elements showing the principle quantum number
versus the atomic number;
FIGURE 2 is a diagrammatic
sketch of an electrodeposition apparatus used in forming the
metallic gold from the G-ORME;
FIGURE 3 is a diagrammatic
drawing of a separation apparatus utilized in separating ORMEs
from ores according to the present invention;
FIGURE 4 is a plot of an
infrared spectrum derived from an analysis of a rhodium ORME;
FIGURE 5 is the cycling
magnetometry evaluation of iridium S-ORME demonstrating the
phenomena of negative magnetization and minimum (Hc1) and
maximum (Hc2) critical fields. In addition, the Josephson
effect is demonstrated by the compensating current flows in
response to the oscillations of the sample in a varying d.c.
FIGURE 6 is a differential
thermal analysis (DTA) of hydrogen reduced iridium being
annealed under helium atmosphere. The exothermic reaction up
to 400 C is due to hydrogen and/or water bond breaking and the
exothermic reaction commencing at 762 C is due to electron
pairing and subsequent phonon emissions leading to S-ORME
system development of the iridium ORME;
FIGURE 7 is a TGA of
hydrogen reduced iridium monoatoms subjected to four (4)
annealing cycles in a He atmosphere. It plots the heating and
cooling time versus temperature. Comparison to Figure 6 shows
an initial weight loss due to hydrogen and possibly water bond
breaking. The significant demonstration is the scale-indicated
weight loss corresponding to the second exothermic reaction
shown in FIGURE 6; and
FIGURES 8-17 are
weight/temperature plots of the alternate heating and cooling
over five cycles of an iridium S-ORME in an He atmosphere.
In the examples, parts are
by weight unless otherwise expressly stated.
Preparation of G-ORME ~
G-ORME was prepared from
metallic gold as follows:
(1) 50 mg gold (99.99% pure)
were dispersed in 200 ml aqua regia to provide clusters of
(2) 60 ml concentrated
hydrochloric acid were added to the dispersion and the mixture
was brought to boil, and continued boiling until the volume
was reduced to approximately 10-15 ml. 60 ml concentrated HCl
were added, and the sample brought to boil and checked for
evolution of NOCl fumes. The process was repeated until no
further fumes evolved, thus indicating that the nitric acid
had been removed and the gold had been converted completely to
the gold chloride.
(3) The volume of the
dispersion was reduced by careful heating until the salt was
just dry. "Just dry" as used herein means that all of the
liquid had been boiled off, but the solid residue had not been
"baked" or scorched.
(4) The just dry salts were
again dispersed in aqua regia and steps (2) and (3) were
repeated. This treatment provides gold chloride clusters of
greater than 11 atoms.
(5) 150 ml 6M hydrochloric
acid were added to the just dry salts and boiled again to
evaporate off the liquid to just dry salts. This step was
repeated four times. This procedure leads to a greater degree
of sub-division to provide smaller clusters of gold chloride.
At the end of this procedure an orangish-red salt of gold
chloride is obtained. The salt will analyze as substantially
(6) Sodium chloride is added
in an amount whereby the sodium is present at a ratio 20 moles
sodium per mole of gold. The solution is then diluted with
deionized water to a volume of 400 ml. The presence of the
aqueous sodium chloride provides the salt Na2Au2Cl8.
The presence of water is essential to break apart the diatoms
(7) The aqueous sodium
chloride solution is very gently boiled to a just dry salt,
and thereafter the salts were taken up alternatively in 200 ml
deionized water and 300 ml 6M hydrochloric acid until no
further change in color is evidenced. The 6M hydrochloric acid
is used in the last treatment.
(8) After the last treatment
with 6M hydrochloric acid, and subsequent boildown, the just
dry salt is diluted with 400 ml deionized water to provide a
monoatomic gold salt solution of NaAuCl2.H2O.
The pH is approximately 1.0.
(9) The pH is adjusted very
slowly with dilute sodium hydroxide solution, while constantly
stirring, until the pH of the solution remains constant at 7.0
for a period of more than twelve hours. This adjustment may
take several days. Care must be taken not to exceed pH 7.0
during the neutralization.
(10) After the pH is
stabilized at pH 7.0, the solution is gently boiled down to 10
ml and 10 ml concentrated nitric acid is added to provide a
sodium-gold nitrate. As is apparent, the nitrate is an
oxidizer and removes the chloride. The product obtained should
be white crystals. If a black or brown precipitate forms, this
is an indication that there is still Na2Au2Cl8
present. If present, it is then necessary to restart the
process at step (1).
(11) If white crystals are
obtained, the solution is boiled to obtain just dry crystals.
It is important not to overheat, i.e., bake.
(12) 5 ml concentrated
nitric acid are added to the crystals and again boiled to
where the solution goes to just dry. Again it is essential not
to overheat or bake. Steps (11) and (12) provide a complete
conversion of the product to a sodium-gold nitrate. No
chlorides are present.
(13) 10 ml deionized water
are added and again boiled to just dry salts. This step is
repeated once. This step eliminates any excess nitric acid
which may be present.
(14) Thereafter, the just
dry material is diluted to 80 ml with deionized water. The
solution will have a pH of approximately 1. This step causes
the nitrate to dissociate to obtain NaAu in water with a small
amount of HNO3 remaining .
(15) The pH is adjusted very
slowly with dilute sodium hydroxide to 7.0 + 0.2. This will
eliminate all free acid, leaving only NaAu in water.
(16) The NaAu hydrolyzes
with the water and dissociates to form HAu. The product will
be a white precipitate in water. The Au atoms have water at
the surface which creates a voluminous cotton-like product.
(17) The white precipitate
is decanted off from any dark grey solids and filtered through
a 0.45 micron cellulose nitrate filter paper. Any dark grey
solids of sodium auride should be redissolved and again
processed starting at step (1).
(18) The filtered white
precipitate on the filter paper is vacuum dried at 120° C for
two hours. The dry solid should be light grey in color which
is HAu.H2O and is easily removed from the filter
(19) The monoatomic gold is
placed in a porcelain ignition boat and annealed at 300° C
under an inert gas to remove hydrogen and to form a very
chemically and thermally stable white gold monomer.
(20) After cooling, the
ignited white gold can be cleaned of remaining traces of
sodium by digesting with dilute nitric acid for approximately
(21) The insoluble white
gold is filtered on 0.45 micron paper and vacuum dried at 120°
C for two hours. The white powder product obtained from the
filtration and drying is pure G-ORME.
The G-ORME made according to
this invention will exhibit the special properties described
in the "General Description" of this application, including
catalytic activity, special magnetic properties, resistance to
sintering at high temperatures, and resistance to aqua regia
and cyanide attack.
Example 2: Recovery of
Metallic Gold from Naturally Occurring Material Containing
(1) 300 gr of dried material
assayed by conventional techniques to show no gold present,
ground to less than 200 mesh, is placed in a one-gallon
vessel, fitted with electrodes, with 120 gr NaCl (Morton rock
salt), 10 gr KBr, and 2 liters of tap water.
(2) The anode consists of a
pair of 3/8" x 12" carbon welding rods wrapped together with
No. 10 copper wire. The cathode consists of 1-5/8" ID x 14"
glass tube with a medium porosity glass frit (ASTM 10-15 M)
with a 1" x 15" x 1/16" stainless steel strip inside in a
solution of 36 gr/l NaCl (approximately 500 ml). Both
electrodes are placed into the sample vessel and supported by
clamps extending about 5" into the sample solution.
(3) The sample is placed on
a roller table at approximately 10 revolutions per minute. The
electrodes are connected to a power supply consisting of a 120
volt variac in conjunction with a 2-3 amp 400-600 PIV
rectifier. A 100 watt light bulb and the electrodes are hooked
in series. The rectifier load is connected to the anode since
the rectifier filters out all negative voltage and only passes
(4) The sample is kept under
load for a period of 6-1/2 hours. The final pH is in the range
of 3 - 6.5. The voltage across the electrode is 5 volts.
(5) After disconnecting the
load, the sample was allowed to settle and the solution over
the settled out material was removed by decantation using a
(6) 800ml of the sample was
placed in a 1000 ml beaker and 20 ml concentrated sulfuric
acid was added to the solution.
(7) With stirring, the
solution was boiled down slowly on a hotplate until the
solution was just dry. "Just dry" is as defined in Example 1.
The just dry salt contains sodium gold chloride.
(8) The just dry salt was
taken up in 400 ml deionized water and again boiled down to
the just dry condition. There should be no discoloration at
this point, i.e., a clear solution is formed.
(9) The just dry salt was
then taken up in 400 ml 6M HCl, and thereafter boiled down to
the just dry condition. The dilution and boiling down step was
repeated four times, alternating with a deionized water and a
6M HCl wash, with the sequence controlled so that the last
washing was with 6M HCl. The purpose of steps (8) and (9) is
to remove all traces of hypochlorite oxidant.
(10) The just dry salts are
taken up in 400 ml anhydrous ethanol and stirred for
approximately ten minutes. This step is to dissolve the gold
chloride salt, to remove the sodium chloride.
(11) After stirring, the
slurry was filtered through #42 paper on a Buchner funnel.
(12) 5ml of concentrated
sulfuric acid was slowly added to the filtrate, mixed, and the
filtrate was then allowed to sit for approximately one hour.
The filtrate was filtered through #42 filter paper on a
Buchner funnel, and then passed through a filter of 0.5 micron
Teflon. The sulfuric acid precipitates out any calcium.
Filtration removes the precipitant and a light yellow filtrate
is recovered, with all traces of calcium sulphate removed.
(13) The light yellow
solution was again boiled down to just dry, taking care to
avoid any charring. At this point there should be no further
evaporation of ethanol and the just dry residue should be free
of color. The residue should have a sweet smell similar to
burnt sugar. The occurrence of the sweet smell indicates the
end point of the boil-down.
(14) The just dry residue is
taken up in 600 ml deionized water to provide a water-soluble
gold form which is the gold auride. If desired, the G-ORME can
be recovered at this stage or converted into metallic gold.
For gold recovery, the solution is put into a 1000 ml beaker
and an electrolysis unit was set up as shown in FIGURE 2 of
As shown in FIGURE 2 of the
drawing, the electrolysis unit comprises a 220 volt, 120 amp
power supply (20) which is connected to the anode (12) and
cathode (14) of the electrolytic cell. The solution is stirred
using a magnetic stirrer (16). The anode (12) is a gold
electrode, 2 cm2 in size, upon which gold in
solution will plate out. The cathode (14) comprises a 6.8 cm2
platinum electrode contained in a Nafion 117 chamber (18).
Nafion 117 is a perfluorocarbon sulfonic acid membrane,
marketed by the duPont Company, and is a proton-conducting
membrane. Inside the Nafion chamber is 200 ml of electrolyte
solution containing 5 ml sulfuric acid per 600 ml of
electrolyte solution. It is important to keep the Nafion
chamber wet at all times. The potential was measured across
the electrodes and then an additional -2.2 volts potential was
applied and maintained for a period of two hours.
(15) After the two hours,
the potential was raised to 3.0 volts and maintained for
approximately 18 hours. Bubbles formed on both the gold and
platinum electrodes. A black material formed on the gold
electrode after three to four hours.
(16) The gold electrode was
removed from solution while voltage was still being applied.
The electrode was dried in a vacuum oven overnight at 115° C.
The electrode was weighed before and after the plating to
determine the amount of gold collected.
The metallic gold is,
therefore, produced from a naturally occurring ore which, when
subjected to conventional assaying, does not test positive for
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
(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 gr of a single
select elemental metal powder is intimately blended with 30 gr
sodium peroxide and 10 gr 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
(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 400 ml 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,
(15) The hydroxide
precipitant is dissolved off the fritted glass filter with 400
ml 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 120° C for approximately
(19) The dried material is
carefully transferred from the filter to a quartz ignition
(20) The ignition boat is
placed in a cold tube furnace and the temperature is slowly
(2° C/min) raised under a hydrogen atmosphere to 600° C and
held at this temperature for one hour and then slowly (2.5°
C/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.
These materials have a number
of applications as previously described, one of which is as
catalysts in an electrochemical cell.
Example 4: Procedure for
Separation of Platinum Group Elements (PEGs) from Ore
Containing ORMEs ~
The class of ores which are
processed to form ORMEs, when analyzed by conventional
instruments normally used for determination of Platinum Group
Metals (PGM), will indicate that essentially no metals of this
PGM group are present.
In the separation of the PGE
from the ore, the pretreatment of the ore sample is crucial.
If the sample is not prepared properly, the pegs in their ORME
state are virtually impossible to separate. The separated
elements are not necessarily in an ORME state.
The purpose of the
pretreatment is primarily for the removal of silica.
Pretreatment comprises crushing and pulverizing the ore to a
fine powder (-200 mesh). A sample of 50 gr of the pulverized
ore and 100 gr ammonium bifluoride, NH4HF2,
are weighed and placed in a 1000 ml Teflon beaker. The ore and
NH4HF2 are moistened with distilled
water and approximately 200 ml HF (hydrofluoric acid) is
added. The sample is baked to dryness on a hotplate. This
procedure is repeated four times each with more HF. The sample
is transferred to a platinum dish and roasted over a hot flame
until the sample turns a dull red-brown color. After this
treatment, most of the silica has been removed as H2SiF6
(white fumes that evolve during roasting).
The sample is now placed in
a zirconium crucible with 200 gr NaNO3 (sodium
nitrate) and 500 gr Na2CO3 (sodium
carbonate). The sample is then fused using a Fisher burner and
a propane torch to a red hot melt. When cool, the fusion
should be an aquamarine color, or a light brown color. The
light brown color means the sample has passed through the
aquamarine stage. This poses no problems in the subsequent
separation and determination of the pegs. If the melt cools to
a light green color, fusion is not complete. It must be fused
again until it reaches the aquamarine end point.
In the zirconium crucible
containing the cooled melt, place an "X" shaped Teflon coated
stirring bar and minimum amount of distilled water. Place the
crucible in a beaker and cover with a watch glass. Place the
beaker on a stir plate to slurry/dissolve the sample from the
crucible. A minimum amount of distilled water should be used
in the removal. The sample is now ready for distillation.
& Separation of Osmium & Ruthenium ~
The first pegs are separated
by a perchloric acid distillation with ruthenium and osmium
being distilled off as RuO4 and OsO4.
Platinum, palladium, rhodium, and iridium are left in the pot
liquor. The distillation apparatus in diagrammatic form is
illustrated in FIGURE 3 of the drawing, as used on a 5 gr
sample of ore.
Referring to FIGURE 3 of the
drawing, Flask #1 has a 500 ml volume and contains 5 gr of ore
in 250 ml of solution/slurry. Flask #2 has a 250 ml volume
with 60 ml 1:1 HCl and 15 ml 30% H2O2.
Flask #3 has a 50 ml volume with 20 ml 1:1 HCl and 15 ml 30% H2O2.
Flask #4 has a 200 ml volume with 100 ml 1:1 HCl saturated
with SO2 (sulfur dioxide). Flasks #5 and #6 have a
100 ml volume with 60 ml 1:1 HCl saturated with SO2.
The flasks are all interconnected with glass conduits and
ground glass ball and socket joints. The distillation proceeds
as follows: A closed system is used with N2
(nitrogen) as a carrier gas for RuO4 and OsO4.
To Flask #1 60 ml of 70 % HClO4 (perchloric acid)
is added slowly from the separatory funnel 10. Once all of the
HClO4 is added, the flask is heated. At a
temperature of 105-112° C, a white cloud is seen flowing into
Flask #2. The heat is continued until fumes of HClO4
begin to come off at approximately 175 C. The heating is
continued to 210° C when the temperature stops rising. The
system is then cooled to 100 C. At this point 20 ml of 70%
HClO4 and 20 ml distilled water are added to Flask
#1, again through the separatory funnel; and the system is
heated to 210° C again, then cooled again to 100° C. 10 ml of
70% HClO4 and 10 ml distilled water are added to
Flask #1 and the sample is
heated again to 210° C. The distillation is repeated once more
After the fourth
distillation, the heat on Flask #1 is turned off and heat is
applied to Flask #2, bringing it to a boil slowly to drive any
OsO4 out of the RuO4 fraction. Nitrogen
purge gas is still flowing and must be controlled to prevent
back flow. Boiling is continued until Flask #3 is almost full
or the H2O2 has been almost driven out
of Flask #3. The presence of H2O2 is
indicated by tiny bubbles forming all over the glass surface.
The entire system is then cooled to room temperature, with the
nitrogen gas flowing continuously through the cool down.
The distillation receiving
flasks are then dismantled. Flask #4, #5, and #6 contain the
osmium fraction as OsO4. These are combined in a
600 ml beaker. Flask #2 and #3 contain the ruthenium fraction
as RuO4 and are combined in a 600 ml beaker. The
contents of Flask #1 which contains platinum, palladium,
rhodium, and iridium are retained in the distillation flask to
remove HClO4 by heating to dryness as described in
Section 4. These fractions are now ready for further analysis
and separation. The osmium and ruthenium fractions must sit in
solution at room temperature for 16-24 hours before continuing
with the steps (2) and (3).
(2) Separation of Osmium
The osmium distillate after
sitting for 16-24 hours at room temperature is processed as
follows: The osmium fraction from the distillation is slowly
evaporated to approximately 10 ml of solution. Then 25 ml of
concentrated HCl (hydrochloric acid) are added and the sample
is again evaporated to approximately 10 ml. This is repeated
five times. On the last digestion, the sample is carefully
taken to moist salts at which point it is diluted to 200 ml
with distilled water and brought to a boil. The hot solution
is filtered through #42 Whatman paper, washing with a minimum
amount of 0.1 N HCl.
After cooling to
approximately 40° C, the pH of the sample is then slowly
adjusted on a calibrated pH meter using a saturated solution
of NaHCO3 (sodium bicarbonate), to a pH of 4 while
stirring vigorously. The solution then is gently boiled for
5-10 minutes, removed from the heat, and let stand for a
period of at least twelve hours. The osmium precipitates are a
reddish-brown hydrated dioxide.
The solution is filtered
through a dry, tared porcelain filter crucible using the
Walters crucible holder. Most of the solution is decanted
through the filter crucible, being careful not to disturb or
float the precipitate. The filter should not pull dry. Pour
the last 100-200 ml of solution containing precipitate in the
filter. Be prepared to immediately rinse the precipitate with
hot 1% w/v NH4Cl solution (filtered through 0.45
micron pad during preparation). A wetted rubber policeman is
used to thoroughly scrub the beaker and rinse after each scrub
with hot 1% NH4Cl.
The crucible is dried
overnight at 105° C in a vacuum oven. The cooled, dry crucible
is weighed and the approximate osmium value is calculated from
this OsO2 weight.
With the crucible on vacuum
again, the precipitate is rinsed with two aliquots of 20 ml
each saturated NH4Cl solution. Leave 100-200 mg of
the solid NH4Cl on the precipitate. Dry gently in a
vacuum oven for 1-2 hours at 100° C.
The sample is now ready for
tube furnace hydrogen reduction. Place the filter crucible on
its side in a quartz tube, and insert the tube into the
furnace center. Start argon and hydrogen gas flow through the
furnace. Allow the temperature to increase slowly to dehydrate
the precipitate without igniting it. Decrease the argon flow
until only hydrogen flows. Then heat at 360-375° C until all
NH4Cl is sublimed.
Continue heating the
precipitate in hydrogen only at 500° C for 20 minutes to
complete reduction to osmium metal. Cool the crucible in
hydrogen to ambient temperature. Replace hydrogen with carbon
dioxide for 20 minutes to prevent any oxidation when the
reduced metal is first exposed to air. Weigh as elemental
(3) Separation of
The ruthenium distillate
after sitting 16-24 hours at room temperature is processed as
follows: The ruthenium fraction from the distillation is
slowly evaporated to approximately 10 ml of solution. Then 25
ml of concentrated HCl are added and the sample is digested
again to approximately 10 ml. This procedure is repeated five
times. On the last digestion, the sample is carefully taken to
moist salts on a steam bath. The sample must not be hot enough
for HClO4 traces to reoxidize the ruthenium. Add
200 ml of distilled water, and bring the solution to a boil.
Filter the hot solution through No. 42 Whatman paper, washing
with a minimum amount of 0.1 N HCl.
After cooling to
approximately 40° C, the pH of the sample is slowly adjusted
on a calibrated pH meter with a saturated solution of NaHCO3
to pH 6 while stirring vigorously. The solution is brought to
a gentle boil for 5-10 minutes before removing it from the
heat. The sample is permitted to stand for a period of at
least twelve hours. The ruthenium precipitates as a
yellowish-brown hydrated dioxide.
The solution is filtered
through a #42 Whatman ashless filter paper wetted with 1% w/v
(NH4)2SO4 (filtered through a
0.45 micron pad during preparation). Decant most of the
solution through the filter paper, being careful not to
disturb or float the precipitate. Pour the last 100-200 ml of
solution containing most of the hydrated oxide in the paper
all at once. A wetted rubber policeman is used to thoroughly
scrub the beaker. A piece of #42 ashless filter paper wetted
with 1% w/v (NH4)2SO4 is used
to complete the transfer. The precipitate is washed twice with
hot 1% w/v (NH4)2SO4 and once
with hot 2.5% w/v (NH4)2SO4.
The filter is allowed to drain as dry as possible.
The paper is transferred to
a tared quartz boat, and dried gently in an oven at 110° C.
The boat is placed in a
quartz tube for final firing and reduction in the tube
furnace. From a cold start (below 100° C), pass enough air
over the sample to ignite the paper without mechanical loss of
precipitate. Increase the furnace temperature slowly to 500° C
and maintain this temperature until the paper ignition is
complete. Pull the boat out of the heated section and allow it
to cool to 150° C or less. Purge the tube with argon, then
hydrogen. Complete the hydrogen reduction with sample in the
heated section at 500° C, then to 600° C for 20-30 minutes.
Pull the sample out of the
heated section to cool to less than 100 C with hydrogen being
passed over the sample. Complete the cooling with carbon
dioxide to ambient temperature (approximately 10-15 minutes).
The cooled ruthenium is
washed twice with 1% w/v (NH4)2SO4
to dissolve the last traces of soluble salts. Ignite again in
air and hydrogen as described above. Weigh as elemental
(4) Separation of
The platinum, palladium,
rhodium, and iridium fraction in HClO4 from the
distillation is evaporated to dryness in a beaker. The
procedure takes considerable time and care since HClO4
is being fumed off. When the sample reaches a dry salt state
and is cooled, distilled water and concentrated HCl are added,
and the sample is evaporated again. The water, HCl treatment
is repeated twice more. After the sample has been evaporated
for the last time, it is diluted with distilled water to 300
ml. The sample is now ready to separate platinum from rhodium,
palladium, and iridium. At this stage either an ion-exchange
process, which is designed for production of larger quantities
of separated ORMEs, or a non-precise quantitative separation
may be used. The following procedure details the quantitative
The sample is brought to a
boil and 200 ml of 10% w/v NaBrO3 (sodium bromate)
solution are added and the sample is boiled again. When the
sample has reached boiling, it is removed from the heat,
cooled to 40° C, and the pH is adjusted with a calibrated pH
meter to pH 6 with a saturated NaCHO3 solution. 100
ml of 10% NaBrO3 are added and the solution is
brought to a gentle boil for 15 minutes. The sample is then
cooled and the precipitate is allowed to coagulate for 20-30
The sample is then filtered
on a medium porosity fritted glass filter and washed with 1%
NaCl solution pH 6.5-7.5 (filtered during preparation through
a 0.45 micron pad). The filtrate contains the platinum and the
precipitate contains palladium, rhodium, and iridium as PdO2,
RhO2 and IrO2 in hydrated form. The
precipitate is redissolved with 6N HCl, boiled and
reprecipitated as above two or more times to ensure complete
separation of platinum from palladium, rhodium, and iridium.
The filtrates from the three
precipitations are combined in a 1000 ml beaker and 50 ml of
concentrated HCl are added. The sample is boiled to dryness to
remove bromine and any traces of HClO4 that still
might be present. Add 50 ml of water and 50 ml concentrated
HCl. Boil to dryness again and repeat two more times, with the
last time being to provide moist crystals rather than boiling
to dryness. The sample is diluted to 200 ml with distilled
water and 40 ml of HCl are added.
The sample is heated to a
gentle boil and a stream of H2 (hydrogen) gas is
passed through the sample for ten minutes, followed by passing
a stream of H2S (hydrogen sulfide) gas through the
solution while continuing with a flow of H2. The
solution is allowed to cool while H2S is passing
though it. The platinum precipitates as brown black PtS2.
The solids are filtered
through #42 Whatman ashless filter paper and the precipitate
washed with 1% v/v HCl. The filter and precipitate are
transferred to a tared porcelain crucible. The filter is dried
gently, then the residue ignited in air to red heat using a
Meeker burner. The metal residue is leached with 1% v/v HCl
and washed onto a second #42 ashless filter paper. The residue
is washed thoroughly with hot distilled water. The filter is
transferred to the same porcelain crucible, dried, and heated
to red heat using a Meeker burner. The residue is weighed as
platinum metal. The PtS2 precipitate can also be
reduced under H2 in the tube furnace.
(5) Separation of
The precipitate of hydrated
dioxides of palladium, rhodium, and iridium remaining from
step (4) are dissolved in 1000 ml of 6 N HCl and diluted to
4000 ml with distilled water. The sample is then filtered on a
0.45 micron filter. To the solution is added a sufficient
volume of 1% w/v dimethylglyoxime in 95% ethanol (250 ml) to
precipitate all the palladium with gentle boiling. The sample
is set aside for a minimum of one hour, then filtered into a
tared porcelain filter crucible. Wash with 0.1 N HCl and then
with water. The filtrate is retained for rhodium and iridium
separation. The precipitate is dried at 1100° C and the yellow
precipitate is weighed as palladium dimethylglyoxime, with
palladium being 31.67% w/w of the total precipitate.
(6) Separation of Rhodium
The filtrate from the first
palladium precipitation is diluted to 500 ml and 10 ml of
concentrated H2SO4 and 10 ml of
concentrated HNO3 are added. The filtrate is
evaporated with heat until heavy fumes of H2SO4
are evolved. After cooling, 10 ml concentrated HNO3
are added and again heated until fumes are evolved. This
treatment is repeated until no more charring results and all
organic material has been destroyed. The solution remaining is
cooled and 20 ml water are added. Evaporation with heating to
heavy fumes is again repeated. The water wash is repeated two
times to destroy any nitroso compounds that might interfere in
the rhodium determination.
The solution is diluted to
200 ml and heated to boiling. A solution of 20% TiCl3
(titanous chloride) is added dropwise until the solution
retains a slight pink color. Boil the solution for two
minutes, cool, and filter the solution through Whatman #42
ashless filter paper. If any rhodium has precipitated out,
wash the paper with 0.9 N H2SO4. Then
char the filter paper in a 5 ml concentrated H2SO4.
Add 5 ml HNO3 to heat and destroy organic matter as
previously described. Dilute the solution with 50 ml water and
combine with the filtrate from the TiCl3
The rhodium is separated
from the iridium by removal of the excess titanium in a
cupferron extraction with chloroform. The solution is chilled
in an ice bath and placed in a 500 ml separatory funnel. To
this 5 ml aliquots of chilled 6% aqueous cupferron are added,
giving a milky yellow solution. If the cupferron solution is
darkened, it should be treated with activated charcoal and
filtered through a 0.45 micron pad. The titanium is extracted
in 25 ml aliquots of cold chloroform. The extract is a clear
yellow solution which is poured into a waste container. When
no more yellow color is extracted, another 5 ml aliquot of
cupferron solution is added. After many aliquots to remove the
yellow titanium cupferrate, the extract turns a red brown.
This fraction is collected in a separate beaker as the rhodium
fraction. All extractions following this are added to the
rhodium fraction in a 600 ml beaker. The extraction is
complete when an aliquot of cupferron turns the solution milky
white and the chloroform extract is clear to very light green.
Retain the solution for iridium separation.
The extract is evaporated to
dryness separating the chloroform from the rhodium fraction.
50 ml of aqua regia are added and the sample is evaporated to
dryness to destroy organic material. Add 10 ml concentrated H2SO4
and 10 ml HNO3 and heat to fumes. Repeat HNO3
treatment until no more charring results and all organic
material has been destroyed. The solution is cooled and 20 ml
water is added, followed by evaporation to heavy fumes again.
Repeat the water wash two times to destroy any nitroso
The sample solution is
diluted to 200 ml with water. Then 10 ml of 10% NaBrO3
is added and the sample is heated to boiling. The sample is
then cooled to 40° C and the pH adjusted to pH 6.0 with NaHCO3.
10 ml of NaBrO3 are added and the sample heated to
a boil. The sample is cooled and filtered on a weighed
porcelain crucible. The sample is dried in a vacuum oven and
the precipitate is weighed as RhO2.
The material is then
purified by dissolving the RhO2 precipitate from
the weighing crucible with 6 N HCl and evaporate to moist
salts and proceed as above.
The rhodium oxide is removed
from the weighing crucible by using a 20% v/v H2SO4
solution. Then dilute the solution to 200 ml with water, and
heat to boiling. Add dropwise a solution of 20% TiCl3
until the solution retains a slight pink color while boiling.
A precipitate of rhodium will form. Allow the solution to cool
to 40° C. If it loses color, boil and add more TiCl3.
If color remains, filter through Whatman #42 ashless filter
paper. The precipitate is washed with hot 10% v/v H2SO4
until the filtrate ceases to show the orange titanium complex
with H2O2, then wash twice more.
Redissolve the rhodium as
before to destroy the organic material. Add 10 ml concentrated
H2SO4 and 10 ml of HNO3 to
char the paper. Repeat the HNO3 treatment until no
more charring results and all organic material has been
destroyed. Cool the solution, add 200 ml water, and evaporate
to heavy fumes again. Repeat the water treatment two times to
destroy any nitroso compounds.
Add 20 ml of water and 10 ml
of concentrated HCl. Gently boil the solution 15 minutes to
get the rhodium into the state from which it can be
precipitated as a sulfide. During treatment the color of the
solution will change from yellow to rose. Filter the solution
#42 Whatman filter paper and wash with 1% v/v HCl. Dilute the
solution to 400 ml with water.
Precipitate the rhodium as
sulfide from the solution kept at the boiling point by passing
a rapid stream of H2S (hydrogen sulfide) gas
through it. Allow the solution to cool with H2S
passing through it. Allow the brown-black rhodium sulfide to
Filter the produce sulfide
through #42 Whatman ashless filter paper. Wash with 2.5% v/v H2SO4
and finally with 1% v/v HCl. Finally, dry the filter paper
gently in a tared quartz boat.
Place the boat in the quartz
tube for final firing and reduction in the tube furnace. From
a cold start (below 100° C), pass enough air over the sample
to ignite the paper without mechanical loss of precipitate.
Increase the furnace temperature slowly to 500° C and maintain
this temperature until paper ignition is complete. Then
complete the air firing at 900° C for 20 minutes. Pull the
crucible out of the heated section and allow it to cool to 200
C or less. Purge the tube with argon, then hydrogen. Complete
the hydrogen reduction with sample in the heated section at
900° C for 20-30 minutes.
Pull the sample out of the
heated section to cool to less than 100° C, with hydrogen
being passed over the sample. Complete the cooling with carbon
dioxide to ambient temperature for 10-15 minutes.
Wash the cooled rhodium
twice by decantation with cool 1% w/v (NH4)2SO2
to dissolve the last traces of soluble salts. Dry gently,
ignite again in air and hydrogen as described above. Weigh as
(7) Separation of Iridium
The solution left in the
separatory funnel from the cupferron extraction contains the
iridium. Transfer it quantitatively with a 1% v/v H2SO4
wash to a 600 ml beaker. Add 10 ml of concentrated HNO3.
Evaporate to heavy fumes of H2SO4. Cool,
add 10 ml more HNO3 and again heat to fumes. Repeat
this treatment until no more charring results and all organic
material has been destroyed. Cool the solution, add 20 ml
water and evaporate to heavy fumes again. Repeat with the
water treatment two times to destroy any nitroso compounds.
Dilute with water to 300 ml.
Bring the sample to a boil
and add 20 ml of 10% w/v NaBrO3 solution and boil
again. When the sample has reached boiling, it is removed from
the heat, cooled to 40° C, and the pH is adjusted with a
calibrated pH meter to 7 with saturated NaHCO3
solution. Add 10 ml of 10% NaBrO3 and bring to a
gentle boil for 15 minutes. The sample is then cooled slowly
and the precipitate is allowed to coagulate for 20-30 minutes.
The precipitate is filtered
into a tared porcelain crucible in a Walters crucible holder.
Decant most of the solution through the filter crucible, being
careful not to disturb or float the precipitate. Do not let
the filter pull dry. Pour the last 10-20 ml of solution
containing the precipitate into the filter. Be prepared to
immediately rinse and police and beaker with 10% w/v NaCl
solution. Dry the filter at 110C under vacuum for 1-2 hours.
Dissolve the precipitate with 6N HCl and evaporate to moist
salts and proceed as before, for a cleaner iridium fraction.
Wet the precipitate with
saturated NH4Cl solution and approximately 100 mg
of solid NH4Cl.
Dry gently in a vacuum oven again at 110° C for 1-2 hours.
The sample at this point,
which is the hydrated iridium ORME can be treated by alternate
procedures. In the first procedure the sample will be treated
to provide an iridium S-ORME and then utilized to establish
the existence of a Meissner field, a property unique to
superconducting materials. In the second procedure, the sample
will be treated so as to form elemental iridium.
Procedure A ~
The iridium fraction is
placed in a quartz ignition boat and the boat inserted into a
tube furnace for slow reduction under hydrogen gas. The
hydrogen gas is flowed slowly over the sample maintaining a
slight positive pressure in the tube at all times. The
temperature of the tube furnace is raised very slowly and
uniformly up to 850° C, taking care not to allow the heating
rate to exceed 2° C per minute. The 850° C temperature is
maintained for one hour, then the sample is slowly cooled
under hydrogen gas, being careful not to exceed a 2.5° C
reduction in temperature per minute until room temperature has
been achieved. Nitrogen gas is then introduced into the tube
and the hydrogen gas is shut off. The tube is then purged for
eight hours with nitrogen gas. The sample at this point will
be a grey-black amorphous powder. The powder is removed from
the tube and then placed in a protected area so that it can
react with air for at least two days (48 hours).
Approximately 10 mg of the
resultant powder is transferred to a controlled atmosphere
bifilar-wound heating element Thermo Gravimetric Analysis
(TGA) instrument (Perkin-Elmer Thermal Analysis (PE/TGS-2),
Temperature Programmer (PE/System 4), Thermal Data Station
(PE/TADS). And Graphics Plotter (PE/THERM PLTTR). The sample
is heated in the instrument at the rate of 1.2° C per minute
under an atmosphere of helium gas to 850° C, and then
immediately cooled at 2° C per minute to room temperature. The
heating and cooling cycles are repeated four times.
The bifilar winding of the
heating element possesses an extremely small magnetic field in
that the weighed sample can never be exactly equal distance
from both wires due to the winding configuration. The
depolarized field will not react with ordinary metal samples
or normal magnetic (N-S polarized) materials. However, a
superconductor will react with an external magnetic field,
even one of small magnitude.
FIGURES 8-17, which are
weight/temperature plots of alternate heating and cooling of
the iridium S-ORME sample material over five cycles, depict
the Meissner field generation and the frequent collapsing and
regeneration of the field. Specifically, FIGURE 8, Plot IR1H1,
demonstrates the first heating cycle which establishes
approximately a 26% weight loss. This weight loss is primarily
due to loss of water. FIGURE 9, Plot IR1C1, read from the
right to the left with 100% being the 75% of Plot IR1H1
(FIGURE 8), demonstrates weight gain and flux jumping upon
cooling. The apparent weight gain and flux jumping establishes
that the material is superconductive. A material such as iron
which is not superconductive would show a plot which is
essentially a flat line. The remaining plots, i.e., FIGURES
10-17, showing the effect of alternate heating and cooling,
establish that each treatment extends the Meissner field
generation in the direction of room temperature. FIGURE 17,
Plot IR1C5, shows the flux jumping very close to room
The sample, after the above
annealing treatment has been completed, will be white in
color. The white powder is chemically inert to normal
oxidation-reduction chemistries. It does not gain weight
readily on exposure to air. However, gases such as nitrogen,
oxygen, carbon monoxide, and carbon dioxide do apparently
absorb to the surface resulting in "flux pinning" as the term
is used in describing behaviour of superconducting materials
of the S-ORME.
Procedure B ~
The sample is subjected to
furnace ignition and hydrogen reduction. Place the filter
crucible on its side in the quartz tube and insert into the
tube furnace center. Start the air flowing gently. Allow the
temperature to increase slowly to dehydrate the precipitate
completely. Heat until all NH4Cl is sublimed at
360-375° C. Continue heating in air to 800° C.
Remove the crucible from the
heated section of the furnace and cool to 200° C or less.
Purge the tube with argon, then hydrogen. Complete the
hydrogen reduction of the sample in the heated section at 800°
C for 20-30 minutes.
Pull the sample out of the
heated section to cool to less than 100° C while hydrogen is
being passed over the sample. Complete the cooling by
treatment with carbon dioxide for 10-15 minutes to ambient
Wash the cooled iridium with
1% w/v (NH4)2SO4 twice
to dissolve the last traces of soluble salts. Dry gently,
ignite again in air and hydrogen as described above. Weigh as
elemental iridium, or the Ir-ORME. If the sample is partially
dissolved in aqua regia in preparation for an Inductively
Coupled Plasma Mass Spectroscopy (ICP-MS) testing, then the
instrument will indicate the presence of metallic iridium. In
other words, prior to treatment of the ore, conventional assay
techniques indicated that no iridium was present. After
treatment and separation of the ORMEs, a slow reduction under
hydrogen gas, followed by aqua regia treatment, will convert
part of the Ir-ORMEs into their constituent T-metal.
As will be apparent to one
skilled in the art, various modifications can be made within
the scope of the aforesaid description. Such modifications
being within the ability of one skilled in the art form a part
of the present invention and are embraced by the appended
The Claims Defining the
Invention are as follows:
1. In a separated and
substantially pure, stable form, a non-metallic, orbitally
rearranged monoatomic transition or noble metal element
selected from the group consisting of cobalt, nickel, copper,
silver, gold, palladium, platinum, ruthenium, rhodium,
iridium, and osmium having a d orbital hole sharing energy
with an electron or electrons, said shared energy identified
as a doublet in an infrared spectrum of from between about
1400 and 1600-1 cm.
2. The orbitally rearranged
monoatomic element of claim 1 wherein said element is gold.
3. The orbitally rearranged
monoatomic element of claim 1 wherein said element is silver.
4. The orbitally rearranged
monoatomic element of claim 1 wherein said element is copper.
5. The orbitally rearranged
monoatomic element of claim 1 wherein said element is
6. The orbitally rearranged
monoatomic element of claim 1 wherein said element is
7. The orbitally rearranged
monoatomic element of claim 1 wherein said element is
8. The orbitally rearranged
monoatomic element of claim 1 wherein said element is rhodium.
9. The orbitally rearranged
monoatomic element of claim 1 wherein said element is iridium.
10. The orbitally rearranged
monoatomic element of claim 1 wherein said element is osmium.
11. The orbitally rearranged
monoatomic element of claim 1 wherein said element is cobalt.
12. The orbitally rearranged
monoatomic element of claim 1 wherein said element is nickel.
13. Process of forming a
non-metallic, orbitally rearranged monoatomic form of an
element selected from the
group consisting of cobalt,
nickel, copper, silver, gold, palladium, platinum, ruthenium,
rhodium, iridium, and osmium from the corresponding element in
metal form comprising treating said metal form by forming a
salt thereof, exhaustively solubilizing and evaporating said
salt in an aqueous medium until a diatom of said metal form is
obtained; and thereafter treating said diatom with an alkali
metal in the presence of water to form said orbitally
rearranged, stable monoatomic form of said element.
14. Process of forming a
metal selected from the group consisting of cobalt, nickel,
copper, silver, gold, palladium, platinum, ruthenium, rhodium,
iridium, and osmium from a material having the corresponding
element present in a non-metallic, orbitally rearranged
monoatomic stable form of said element, comprising separating
said element in said orbitally rearranged monoatomic form from
said material, and then subjecting said separated,
non-metallic, orbitally rearranged monoatomic stable form to a
two-step negative potential of at least 1.8 to 2.2 V
initially, and then to at least 2.5 V until the said element
is formed by electroplating techniques.
15. Process of forming a
metal selected from the group consisting of cobalt, nickel,
silver, palladium, platinum, ruthenium, rhodium, iridium, and
osmium from a material having the corresponding element
present in a non-metallic, orbitally rearranged monoatomic
stable form of said element, comprising subjecting said
element in said orbitally rearranged monoatomic stable form to
a treatment with nitric oxide at elevated temperatures.
16. Process of treating the
stable non-metallic, orbitally rearranged monoatomic
transition or noble metal element of claim 1 by subjecting
said element to alternate heating and cooling cycles under an
inert gas and supplying an external magnetic field to said
element until said element no longer exhibits a doublet in the
infrared spectrum and exhibits magnetic flux exclusion at
temperatures above 200° K.
17. The product formed by
the process of claim 16.
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