MERCURIC PYRO-ANTIMONATE 1. 2. 3. 4. 5. 1. The completion of the production process, vapourised nitric acid being added to the compound to oxidize any free mercury remaining. 2. The production of pyro-antimonic acid. 3. An attempt to produce stable mercuric pyro-antimonate by combining antimony pentachloride with mercuric oxide. 4. An attempt to produce stable mercuric pyro-antimonate by combining mercuric chloride with antimonic acid. 5. The stabilisation of mercuric pyro-antimonate with recovery of nitric acid. These illustrations and images of many other paintings are also located at: http://id.sito.org/sms. Want to find out more or contact me? Then email: - [email protected] See also 'Red Mercury' by Mark Fabi, published 2004-09-30. ISBN-13: 9780553378757 ISBN-10: 0553378759 CONTENTS A synopsis of the book. PART I 1. Note on the contents of this part concerning its limitations. 2. RM 20-20. 3. A brief description of the compound and related compounds. Basic crystal forms. 4. Mercuric and antimonic sulphides and oxides as minerals. 5. The distinctions between ortho-, meta- and pyro- compounds. Mercuric meta-antimonate, lead pyro-antimonate and mercuric pyro-phosphate. 6. A conclusion about the structure of mercuric pyro-antimonate drawn from comparative studies of the other, analogous crystalline compounds. 7. An overview of those episodes in alchemical history that involve mercury and antimony and the scientific judgement on alchemy. 8. An experiment to determine the propensity of mercury and antimony to form mixed oxides. 9. Note on silicates that may have entered into the composition of 'philosopher's stones' during their production. 10. X-ray diffraction. 11. Neutron diffraction. Page 1 2 4 6 8 10 11 20 24 25 27 PART II 1. Introduction, containing a relation of the new influences that were brought to bear on my researches after April '96. 28 2. Dr.Sleight's report to the Journal of Inorganic Chemistry of April '68. 29 3. The production of pyro-antimonic acid and mercuric oxide. 30 4. The masses involved in the course of an experiment designed to produce mercuric pyroantimonate. 31 5. The interpretation of X-ray scans of my oxide samples, the adjustments in my experimental approach and the final results of the experiments. 33 6. Conclusions drawn from comparison of my samples to those described in Dr.Sleight's report. 36 7. Note on Dr.Sleight's work after '68, his contribution to the development of superconductors and collaboration with Arne Magnéli. 37 8. The use of neutron reflectors in nuclear reactors; mercury as a neutron mirror. 39 9. The muon as an agent for atomic fission. An explanation for Dr. Price's results. 42 10. Observations of transmutations in ancient China; the 'out of China' theory of alchemy's origin. 48 APPENDICES Page A. Atoms and fundamental particles. 54 B. The conventional representation of chemical reactions. 57 C. The periodic table and the proximity of alchemy's 'metallic elements'. 60 D. Basic crystallography. 63 E. Scans of samples taken using the PW1720 X-ray analyser. Numbered diagrams. F. Atomic decay sequences. 66 G. Cosmic rays, the pion and the muon. 68 H. An analysis of Ripley’s ‘Bosome-Booke’ from a modern chemistry perspective. 69 I. Circumstantial evidence for the existence of red mercury referred to in 'The Mini-Nuke Conspiracy'. 74 J. Useful Internet addresses for further information on red mercury. 77 BIBLIOGRAPY INDEX Any enquiries about this book should be addressed to: - [email protected] A synopsis of the book. My account of the subject is intended to be an informative rather than fictionalised one, cutting to the scientific bone of the matter. Red Mercury (RM) has become a by-word for nuclear smuggling swindles but, according to one of its modern progenitors, Oleg Sadykov, could be a means to faster semiconductors and of dealing with nuclear waste. If it exists at all it is a dangerous substance though, apparently, non-explosive. According to the most consistent accounts it is a viscous amalgam of mercuric pyro-antimonate containing a small (~4%) amount of an actinide. This is used as a neutron provider and mirror whilst acting to compress the deuterium-tritium content of a 'pure fusion bomb' above its critical mass under the influence of trigger charges, producing a blast with a destruction radius of about 600 metres for a 500 cc bomb, flooding the area with fast neutrons, the fallout lasting for only about 2 days. Essentially, it would represent a strategic advance over the neutron bomb. Although the principal compound is almost completely undocumented, the metallic elements involved loom large in the history of alchemy and the descriptions of it bear an uncanny resemblance to those of the Philosopher's Stone (PS), right down to its being a form of 'fixed', i.e. thermally stable, mercury which can then be 'projected upon', i.e. amalgamated with, liquid mercury. The product in both cases is supposed to be remarkable for its high density, 20.20 g/cc in the case of RM 20:20. However, I should state at this point that I now consider the claims made for its density, as well as those for the densities of its related amalgams to be pure rubbish. According to the only book on the subject that I know of the packing requirements for RM 20:20 (or 'RM 20/20') state that 12 litres of it has a mass of 90.89 kg, allowing for a little ambiguity in the description of the volume. RM 20:20 therefore has a density of 7.57 g/cc, a perfectly plausible density for a gel with the apparent viscosity of black treacle (at room temperature). The expression describes only what it appears to describe, a simple quantitative ratio. I am currently satisfied that it is the molar ratio of the mercury to the mercuric compound (the latter having a density of 9.02 g/cc according to Dr. Sleight). The references to this ratio in 'The MiniNuke Conspiracy'(Hounam & McQuillan) are ambiguous or even unscientific (cf. footnote on p.127). It is as if a garbled rendition of the information translated from the original Russian sources had been made worse rather than corrected during editing, at certain vital points in the text. Analyses of my own versions of the compound, based on Dr. Sleight's synthesis of '68, broadly confirm that chemist's findings but with an odd twist concerning the purity of its most thermally stable allotrope. Certainly, I can confirm that both the meta- and (impure) pyro-antimonates are stable at ~1,0000C, but pure pyro-antimonate always begins to decompose at ~7000C. The supposition that this substance might be useful as an agent for cold fission relies on two mechanisms. One is muon induced atomic fission (initiated by cosmic radiation) and the other is a neutron cascade due to the neutron mirror effect of mercuric ions trapped between antimony and lead atoms at temperatures in excess of mercury's normal boiling point. The analogy between the densification of tinted lead in the (so-called) alchemical gold and that of mercury, amalgamated in a 5 MW reactor with the pyro-antimonate, also represents an important condition for and strong constraint upon this hypothesis. It is the point at which RM and PS become crucially co-dependant on each other's existence. If the one never existed then, in all likelihood, the other never can. Fortunately, at least one sulphide exists in the form of a mineral that combines mercury and antimony whilst the proximity of deposits of those metals in certain areas of China, the great antiquity of Chinese alchemy and the tendency of sulphides to form oxides as alteration products provide an, admittedly circumstantial, origin for the legend of the PS. According to my hypothesis it never required to be invented (always a dubious proposition given the universally acknowledged difficulties surrounding its production) but was originally found with, and mistaken for, Cinnabar. Its mysterious properties then came to light but poor qualitative analysis of the substance led to rumours, rather than hard facts, circulating concerning its composition. Current analytical facilities should therefore be devoted to this purpose before the opportunity of identifying PS/RM is again lost, likewise to the more general question of what happens to volatile metals once their atoms become bonded into pyroxenes. 1 PART I 1. Note on the contents of this part concerning its limitations. The following represents the extent of my researches and speculations up to March 1996, concerning a largely unacknowledged compound with a number of allotropic forms, one of which is credited with the capacity to 'pigment' mercury, rendering it viscous. Although it may be considered that my findings after that date obviate most of the difficulties previously encountered and make the associations I have suggested superfluous and irrelevant, the plain fact is that there are too many aspects to this compound for a researcher to confidently dismiss a finding as otherwise accounted for. Even the professionally produced report introduced in Part II describes two structurally different compounds for mercuric pyro-antimonate whilst only providing data for one. That is not to say that definite conclusions are not reached in Part II, merely that they are insufficient to preclude the hypotheses of Part I at this stage. The background information is so incomplete and disagreements on the significance or otherwise of this compound are so common that the whole project for producing and identifying it is essentially a tentative exercise. 2 2. RM 20-20 In April 1994 there appeared a TV documentary, "The Pocket Neutron", in which an interviewee stated that tons of a substance called Red Mercury were being smuggled through Italy to developing countries each year and that this was a matter of grave concern to the authorities as it could be used in the manufacture of neutron bombs. Elsewhere in the programme it was referred to as mercury antimony oxide and, more helpfully, as a mercury salt of antimony acid, which, given the formula, would seem to indicate pyro- as opposed to meta-antimonic acid. Consistent with a previous programme on this subject it also gave the code-name for this double oxide as RM 20-20, and attributed its production to Russian scientific progress whilst repeating the Ministry of Defence's assertion that it was non-existent. Apparently the mode of operation of RM 20-20 within neutron bombs is that it reflects neutron radiation, a quality exploited by using it as the packing material for plutonium or tritium, 1 kg. of it supposedly being present in each warhead of the SS-20 missiles. Its effect when used in conjunction with tritium gas, for instance, was to generate thermonuclear fusion by producing great concentrations of nuclear energy. An estimate in the previous programme, "The Hunt for Red Mercury", was that it would only take a teacup of fissile material in RM 20-20 to destroy Manhattan. The process was described, by Russian witnesses, as being both slow and difficult. One military specialist, interviewed by the American physicist Dr. Frank Barnaby, displayed a sample of "liquid Red Mercury", but declined to give details of its manufacture. A Russian scientist previously employed by the military establishment was more forthcoming and during the interview Dr. Barnaby drew a chemical structure: - 3 However, the programme makers of 'Dispatches' felt unable to broadcast the dialogue of this interview. Back in the USA one Dr. Sam Cohen, largely responsible for the development of the neutron bomb in the 1950's, gave his assessment of Russian progress towards a pocket-sized nuclear fusion bomb. He was more concerned about this at that time than at almost any previous time, he said, and the root of his concern was the existence of RM 20-20. In attempting to discover a structure for the compound and thereby assess the probability of its existence and the requirements for its production two courses naturally spring to mind. The first is to examine compounds with similar features and/or similar component elements and seek out documentary evidence for its having been synthesised. Dr. Arthur Sleight produced a report describing its synthesis and structure, carried out in the USA in 1968, whilst Dr. Oleg Sadykov is reported as having discovered it in that same year, in the former USSR. The idea that these two events were unconnected is, of course, laughable. The second course is to refer to and investigate the efforts of those who sought to promote nuclear change in lead and mercury through the application of a powder remarkably similar to that used in the production of RM 20-20, namely, the alchemists. The association of mercury and antimony with each other and the alchemists' target element, gold, is far from being the only reason for believing they chose them for the creation of their transmuting powder, the so-called Philosophers' Stone. The references in their literature to 'Our Lead' (antimony) and assertions that their injunctions not to use common mercury were mere double-talk are too prominent to be disregarded. Note here that the powder and RM 20-20 are not one and the same, for the makers of the two 'Dispatches' programmes were misled. The powder must be 'projected upon' (amalgamated with) mercury in order to achieve its 'multiplication', in alchemical terminology, followed by the addition of just a soupçon of an actinide and compression at the heart of a 4MW reactor till the viscous packing agent, 'Red Mercury' is produced. This instance illustrates how the one area of study can serve to illuminate another. Experiments aimed at producing the powder need to start with the most common reactants and progress to the less stable variety used by Dr. Sleight until success is achieved. For my own part, these involved testing a combination of antimony sulphides and antimony and mercury oxides to find out if these would react in such a way as to displace the sulphide ions, forming the double oxide, replacement of sulphides by oxides being a common feature of mineral production underground; the results are called alteration products. I then took the stable compound remaining, added mercuric oxide (HgO) again and marinaded the result in a solution of sodium peroxide. Next I added mercuric chloride (HgCl2) to it, heating it at each stage of the process and noting any changes. Finally I heated it to about 4000C in order to find out what part of it would continue stable. 4 3. A brief description of the compound and related compounds, with their basic crystal forms. Hg2Sb2O7 Mercuric Pyro-antimonate M.P. 356.60C Colour: Cherry Red Density: 9.02 g/cc or 9.6 g/cc Structure: By analogy with K2Cr2O7, monoclinic/ triclinic, or, using HgSb2O6 and IF7 as the basic ionic structures, a development of the pentagonal bipyramidal or octahedral type. Production: Hypothetically, by displacing the H+ ion in H4Sb2O7, pyro-antimonic acid, but the essential reaction would be: 2HgO + Sb2O5 → Hg2Sb2O7 At 2000C pyro-antimonic acid converts to meta-antimonic acid and, at 3000C, to antimony pentoxide, which process might facilitate the reaction : 2HgO + H4Sb2O7 → Hg2Sb2O7 + H2O It may also be worthwhile to take account of the fact that most antimonates contain the [Sb(OH)6 ]- ion, which derives from the pentoxide. The compound closest in valency terms to the pyro-antimonate is that which contains the key Group 5 element, phosphorous, namely, mercury pyro-phosphate, Hg2P2O7, which forms an aqueous Hg22+ - P2O74- system but there is much less documentation for it than for the orthophosphate Hg3 (PO4)2. The meta-antimonate, HgSb2O6, by way of contrast, is among the few solid mixed mercury oxides to have been investigated structurally. It forms hexagonal crystals, isomorphous with PbSb2O6, in which layers of linked SbO6 octahedra are separated by layers of Hg. Suggesting as it does that the pyro-antimonate should have the structural formula Hg2O.Sb2O6 there is plainly another analogy for it involving the configuration of the mercurous oxide ionic units, this being Hg6Cl4O. This is structured with slightly deformed Hg2Cl2 molecules connected via the Cl- anions to infinite chains of Hg2O. 5 Compounds possibly analogous to mercuric pyro-antimonate in ionic structure and crystalline form: Mg2P2O7, K2Cr2O7, Mn2P2O7, Ca3(PO4)2, Hg2CrO4 ,HgCrO4, HgSb2O6, K4P2O7, K2H2Sb2O7, M2+Sb2O6, (M = Mg, Fe, Co, Ni, Zn), MnSb2O6, Ca2P2O7. Mg2P2O7 :- tablets, monoclinic. K2Cr2O7 :- red, mono/triclinic. Mn2P2O7 :- monoclinic. Ca3(PO4)2 :- fusible slag. Hg2CrO4 :- red needles/powder. +HgCrO4 :- red, rhombic/orthorhombic. HgSb2O6 :- trirutile. M2+Sb2O6 :- trirutile. MnSb2O6 :- Columbite, octahedral. Ca2P2O7 :- monoclinic (alpha), tetragonal/uniaxial, positive crystals (beta). As a mineral, manganese meta-antimonate and the M-meta-antimonates are analogous to a large group of silicates, the pyroxenes, M2+Si2O6. THE RELEVANT CRYSTAL SYSTEMS 1. Hypothetical disposition of ions in a crystal lattice of antimony pentoxide, based on the octahedral form of bismuth pentoxide 2. Pyro-antimonic acid Potassium Dichromate 3. Hypothetical disposition of ions and bonds in a crystal lattice of antimony hexoxide octahedra with shared edges based on the hypothetical disposition of antimony pentoxide ions and the arrangement of the hexoxide ions in mercury meta-antimonate 4. 5. HEXAGONAL HgO - Hexagonal HgO has the same crystal structure as red hexagonal HgS. It is orange, being derived by slow precipitation from Hg(NO3)2, as opposed to the red , orthorhombic form and, in contrast to either yellow or red particulate forms, its infinite chains of -O-Hg-O- are helical in structure: - 6 4. Mercuric and antimonic sulphides and oxides as minerals Mercury and antimony occur in various locations about the world, notably those in Spain, Mexico, Russia and China, in the form of their mineral sulphides, Cinnabar and Stibnite. Cinnabar is mercuric sulphide, Stibnite is antimony sulphide. On rare occasions these two can unite to form a single mineral, as in the case of Livingstonite, HgSb4S8. Although steel-grey in colour this leaves a red streak when rubbed against the touchstone, and thin slices of the rock exhibit a reddish translucence when it is held up to the light. Its crystal form is monoclinic, it has a density of 4.9 gm/cc and it is found in association with Cinnabar, Stibnite and Valentinite. Locations of its occurrence are reported to include Chaidarkan in the former USSR and Mexico. The mineral oxides of mercury and antimony exist as alteration products of their sulphides. Alteration products are formed due to exposure of the source minerals to steam and gas issuing from vents in the surrounding rock formations in a process that may last for millennia. As a result, they are much rarer than their sulphides. Valentinite is one form of antimony trioxide (Sb2O3), having a rhombic crystal form, Senarmonite, which has a cubic form, is another. Antimony trioxide is therefore said to be dimorphous. Mercuric oxide, HgO, exists in nature in its mineral form Montroydite. This is dark-red to brown in colour, with a glassy translucence, but can be transparent in thin enough sections. However, it leaves a yellowish-brown streak on the touchstone. It has an orthorhombic crystal system and a density of 11.2 gm/cc. Unsurprisingly, it is found associating with mercury, Cinnabar and/or calomel (mercuric chloride), at five locations in California and one in Texas. Sometimes exposure to both oxygen and steam will produce a double compound comprising both oxide and hydroxide, as in the case of Stibiconite, or hydrous antimony oxide, Sb3O6 (OH). In its pure form this is chalky white, but it has a range of other colours, pale yellow or darker in tone, associated with different impurities. In thin slices it is translucent to transparent. It has a cubic crystal system and a density varying from 3.3 to 5.5 gm/cc. Occasionally it can be found in large crystal aggregates replacing the Stibnite with which it is normally associated, but more commonly with the pure oxide, Valentinite. It is found in many more locations than Montroydite, occurring extensively in the western USA and Mexico, also in Bolivia, Peru, England, Spain, Italy, Rumania, Algeria, Borneo, Australia and China. Incomplete oxidation of the Stibnite can produce Kermesite, the mineralised form of antimony oxysulphide, 8[Sb2S2O]. Its red, needle-shaped crystals contain both monoclinic and orthorhombic crystal forms and it occurs in association with Valentinite and Senarmonite. Note the much greater density of mercuric oxide relative to Livingstonite. This runs counter to expectations based on the high densities of antimony (6.69 gm/cc) and sulphur (2.07 gm/cc) relative to the density of oxygen (1.33 gm/cc) but is due to the extra electron bonds associated with the presence of the ions of a third element. These take up space that would otherwise be occupied by the ions of the twoelement single compound and possess negligible mass. Double or ternary compounds thus have a lower density than single compounds comprising similar elements. This represents an important consideration in relation to the maximum possible density of an amalgam containing mercuric pyroantimonate, the latter having a measured density of 9.02 gm/cc (see Part II). Note also the prevalence of cubic and rhombic crystal forms among the oxides, a useful clue to the crystal form of that ternary oxide. 7 Red Mercury powder, assuming it to have been originally discovered in the ground rather than synthesized, an assumption supported by the difficulties surrounding its production, would therefore appear to be one of these alteration products and to have been generated only where both Cinnabar and Stibnite were undergoing oxidation in close proximity to one another. Due to the high prevalence of Cinnabar deposits that occur in conjunction with Stibnite all the way across central China, it seems likely that the myth/account of the Philosopher's Stone owes its origin to that country, provided that it shares a common identity with mercuric pyro-antimonate or some closely related variant of this ternary oxide. Meanwhile, for a specific case of a mineral association between Red Mercury's constituents and Russia, reference may be made to the Chemical Abstract Services' entry in volume 125 (1996) 'Mercury-antimony content in ores of the Nikitovka Hg-Sb deposit', Russia 280881n. CONCERNING IONIC STRUCTURES OR MINERALS THAT MAY BEAR UPON THE NATURE OF RED MERCURY'S BASE COMPOUND. Potassium dichromate, being a common, stable compound with a structure similar to that of the supposedly unstable compound, pyro-antimonic acid, would seem to be a good starting point for determining the stereochemistry of mercuric pyro-antimonate, particularly when deciding where to place the mercury ions. Like the antimony hydroxide ion, pyro-antimonic acid is associated with the acid oxide, antimony pentoxide, being ditetrahedral in structure (see diagrams 1 and 2). The position of the potassium ions in the dichromate provides an initial concept of how the mercury ions might bond to the dehydrogenated acid (see diagram 2). Meanwhile, given that the Stone was regarded as the product of natural components, such as the "quintessence", the "moist vapour" that, passing through geological strata, caused metals to breed underground, it would seem fitting that minerals which were probably used in the Work should be examined. Stibiconite, or hydrous antimony oxide (Sb2O6 (OH)), is a yellow mineral, white when pure, with a prismatic crystalline form. Kermesite (2Sb2O6.Sb2O3 or 8[Sb2S2O]) is a course dark red powder, turning black when heated but reverting to red when cool again, which forms light feathery aggregates of crystals if a little water of crystallization is present. Cinnabar (HgS) is likewise red, forming hexagonal crystals, the same formation as that adopted by orange HgO (see photos of crystal aggregates). If these mineral structures were in close proximity it would not be surprising if, once the sulphur had vapourised, they gave rise to an alteration product, a double oxide that was symmetrical despite the odd number of ions it possessed in each formula unit (11). 8 5. The distinction between ortho-, meta-, and pyro- compounds. These prefixes are used to indicate the relative levels of oxidation in double oxides, those containing two metals or one metal and hydrogen. Ortho- compounds are just ordinary compounds, as suggested by the prefix, which is associated with the description of something as 'proper', 'normal' or 'right', e.g. orthodoxy, meaning 'the standard doctrine'. Therefore ortho-phosphates, for example, are simply referred to as phosphates. Pyro-compounds, as the prefix suggests, involve oxidation through the action of heat. Pyrophosphoric acid is rapidly formed, as white granular crystals, when orthophosphoric acid is heated above 240oC: 1) 2H3PO4→ H4P2O7 + H2O The meta- compounds represent an intermediate level of oxidation between the ortho- and pyrooxides. Metaphosphoric acid is formed from orthophosphoric acid when it is heated at 316oC: 2) 2H3PO4→ HPO3 + H2O Note that doubling the number of interacting molecules involved to compare with those in the previous case and balancing the equation gives an empirical formula for meta- phosphoric acid of 2(HPO3) or H2P2O6. The oxide ion sequence O3, O6, and O7 corresponding to ortho, meta and pyro oxidation levels is found to be quite standard for different compounds. Ortho-antimonic acid is H3SbO4, meta-antimonic acid HSbO3 (empirically equivalent to H2Sb2O6) and pyro-antimonic acid H4Sb2O7. Regardless of arguments developed over the last 50 years to the effect that these may 'really' be hydroxides, experience of their nature shows them to be strongly acidic. Substituting mercury for hydrogen in equation 1) and adjusting for the difference in valency gives: 3) 2Hg3(PO4) 2 → 2Hg2P2O7 + O2 and this is the reaction observed. However, whilst it might be supposed that antimonite equivalents for these phosphates would be practically achievable, this would not appear to be the case. The tetroxide Sb2O4 is known to exist, being obtained from the heating of the trioxide Sb2O3, and potassium antimonite, K3SbO4, together with acid potassium pyro-antimonate, K2H2Sb2O7, 6H2O, have been obtained in a similar fashion (Textbook of Inorganic Chemistry: J.R. Partington (1931)), the substitution of mercury for potassium in these compounds does not represent any reaction that I have been able to come at, either in my research into reported experiments or on my own account. 9 Lead pyro-antimonate is described in the following terms in 'Introduction to Advanced Inorganic Chemistry' by Durrant & Durrant: 'The pyro-antimonate is a dark yellow powder with a density of 6.72 (gm/cc). It is insoluble in hot or cold water, and very slightly soluble in hydrochloric acid. The compound occurs in nature as the mineral Bindheimite. It has a cubic structure. The crystals have a pyrochlorite framework with cell edge, a = 10.47 Å. In pyrochlorite structures the octahedral SbO6 groups share each oxygen ion with another group, so that the lattice composition is SbO3 (see diagram 4). Although the seventh oxygen ion is not essential for lattice stability, there is room for it.' This consideration has a particular resonance when considering the stability of Hg2Sb2O7. Odd numbers of atoms of any element are difficult to accommodate within symmetric structures, these structures having the highest stability, most notably cubic ones, with their 4-fold symmetry. If the loss of the seventh ion would produce a more stable compound then decomposition from pyro-antimonate to meta-antimonate should soon take place. 'Preparation. Lead pyro-antimonate can be prepared by heating mixtures of lead nitrate or lead acetate with antimonic acid, H3SbO4, to red heat. During slow cooling in a lead refining furnace an idiomorphic (i.e. of a form peculiar to that compound) Pb-Sb oxide, very similar to cubic bindheimite, Pb2Sb2O7, is formed. Applications. Naples yellow is a mixture of lead antimonites and antimonates used as a pigment in ceramics and in oil paints (therefore being of particular interest to myself). The addition of lead antimonate to lead titanate changes its ferroelectric properties.' Mercuric pyrophosphate, Hg2P2O7 has also gained a practical application, in the manufacture of Hg-vapour-containing electric lamps and electron tubes. From a report by the Compagnie Generale de Telegraphie sans Fil, 1964-65: 'The use of Hg pyrophosphate as the Hg generating substance, instead of elemental Hg, to fill Hg vapour tubes exactly with the desired amount of Hg necessary for the perfect function of such tubes is described. The applicability of Hg2P2O7 for this purpose is based on its high thermal stability up to 6000C, and its quantitative decomposition between 600 and 8000C; these properties insure that no Hg is lost during the degassing step, and that exactly the theoretical amount of Hg is charged into the tubes during the filling step of the manufacturing process....' 10 6. A conclusion about the structure of Mercuric Pyro-antimonate Hg2Sb2O7 has an OCTAHEDRAL crystal structure. (Ref. Wells: Structural Inorganic Chemistry.): 'The oxygen chemistry of pentavalent antimony was formerly very perplexing, and many compounds were described as ortho-, meta-, and pyro-antimonates and were assigned formulae analogous to those of phosphates. As a result of the study of the structures of many of these crystalline compounds it is found that their structural chemistry is very simple and quite different from that of phosphates, arsenates and vanadates, being based not on tetrahedral but on octahedral co-ordination of Sb(V) by oxygen ... either as Sb(OH)6- ions in compounds which were once described as hydrated meta- or pyroantimonates, or as SbO6 groups in compounds of the following types - SbO3, M(III)SbO4, M(II)Sb2O6, M2(II)Sb2O7' (my underlining). Also, the meta-antimonate of mercury has the same crystal structure as trirutile Pb(ll)Sb2O6. Pb2Sb2O7 has a pyrochlorite structure. In such structures the octahedral SbO6 groups share each oxygen with another group, so that the lattice composition is SbO3. This generates octahedra with oxide ions at each shared corner. 11 7. An overview of those episodes in alchemical history that involve mercury and antimony and the scientific judgement on alchemy One major psychological barrier to the proper examination of these is the supposed degeneration of alchemy after the beginning of the history of iatrochemistry and the reputation it acquired following the reviews of it given by such as Robert Boyle. However, Boyle himself admitted, in his 'Sceptical Chymist' (1667) that, inasmuch as he had 'ventured long ago to write of matters philosophical' he was 'made to believe that 'tis not inexpedient they should be known to come from a person altogether a stranger to chymical affairs'. This situation evidently altered as he and Isaac Newton spent many years studying the metals of alchemy. The publication of ‘Principia Mathematica’ was supposedly delayed by Newton's laboratory experiments and he wrote about 650,000 words on the subject of alchemy, though he and Boyle do not, by their own account, appear to have got much further in investigating gold than the production of gold sols. These are colloids, or suspensions, of various colours. Certainly, Newton spent much of his later life trying to find the Philosophers' Stone and may have gone mad from mercury poisoning caused during his experiments. Details of the experiments recorded in Newton's 'Chemistry Notebook' were first published by Boas and Hall in 1958. They include some on the action of distilled liquor of antimony on salts of lead, iron and copper and on the preparation of regulus of antimony (a pure, crystalline form of the element) and chlorides of mercury. According to the publishers they read like those of a rational experimental scientist. Much of Boyle's purpose in writing 'The Sceptical Chymist' was to propagate the Aristotelian alternative to the Arabic ‘Tria Prima’ or the ‘Three Chymical Principles of Mixt bodies’, namely, the theory that there are four rather than three basic elements. He writes about a meeting of ‘persons of several opinions, in a place that need not here be named’, principally ‘the inquisitive Eleutherius’, a pseudonym for Boyle himself, and one Carneades, the sceptical chymist of the title. He tells them that (from experiment) he ‘was quickly induced to think that the number of elements has been contended about by philosophers with more earnestness than success’. However, in disputing with them on the subject he had ‘but a negative to defend’, the same position as that adopted by the British and US ministries of defence nowadays, with regards to Red Mercury. Nevertheless, he seems to have realised the importance alchemists placed upon the purification of antimony but not their reason for using ‘muriatic acid’ (HCl) for the purpose. He states that 'Some years ago I sublimed out of antimony a sulphur and that in greater plenty that ever I saw obtained from that mineral, by a method which I shall therefore acquaint you with, because chymists seem not to have taken notice of what importance such experiments may be in the indagation of the nature, and especially of the number, of the elements. Having then purposely digested eight ounces of good and well powdered antimony with twelve ounces of oil of vitriol in a well stopt glass vessel for about six or seven weeks (followed by distillation in a 12 retort)..our antimony afforded us…about an ounce of sulphur, yellow and brittle like common brimstone, and of so sulphureous a smell, that upon the unluting the vessels it infected the room with a scarce supportable stink’, something which also occurs when HCl is used instead, or a similar method used to decompose Cinnabar. However, he plainly did not realise that oil of vitriol (H2SO4) contributed sulphur to the process anyway. Now, antimony had become almost as much a focus of alchemical attention as mercury by the dawn of the C17. Basil Valentine, the pseudonym of Johan Tholde, who wished to publish his own findings as those of a C15 monk, wrote ‘Triumphwagen des antimonii’ in 1604 and it was considered the most important work on metallurgy since Agricola's ‘De re metallica’ of 1556. Paracelsus himself, who mentioned compounds of mercury and antimony as medicinal compounds in his ‘Paragranum’ of 1530, gave the name ‘Al kohol’ to ‘the quintessence’ a hypothetical substance supposed capable of ‘opening the pores’ of intractable metals like mercury so that they could unite to form the Stone, which was thought to be a single metallic element (see also chhi in Part II, section 10). Al kohol was the arabic name for finely divided stibnite (Sb2S3) and, as the quintessence was reckoned a very penetrating vapour, the name came to be applied, by association, to spirits of wine. The author of ‘Alchemy, the Ancient Science’ appears to take alchemical recipes too literally, in the manner of Boyle (who thought the alchemists merely wished to produce a lot of Sulphur from their antimony), as appears in his translator's parenthetical comments on ‘the alchemical process called the ‘Red Lion’’. The original description of it is due to Solomon Trismosin (a pseudonym), a well respected author writing c. 1475 to 1500. The first half of this reads: '1. Take 4 ounces calcined alum, 4 ounces calcined saltpetre (KNO3), and 2 ounces calcined sublimate (HgCl2), and sublimate [refine] in a proper subliming vessel. 2. Carefully take out the sublimate, and resublimate it with 10 ounces fresh salts. During this operation it will be wholesome, on account of the poisonous fumes, to eat bread thickly spread with butter. 3. Put the sublimate in a glass retort, and cover it with alcohol, and distill it over in a water bath until half the fluid remains as an oil behind. 4. The alcohol distilled over is poured back [cohobated] on the residue in the retort, until it is covered about a finger's breadth. 5. This distillation repeat three times, and the whole of the sublimate will pass over into the recipient. This is the Mercury of the Philosophers, the Mercurial Water, as it were the Hellish fire in water (aqua regia?). This Mercurial Water fumes always, and it must be kept in a closed phial, or glass-stoppered bottle. 6. Take fine gold, in leaf or thin beaten, put it in a glass retort, just cover it with the Mercurial Water, and put the retort on gentle heat, when the Water will begin to act upon the gold, and dissolve it, but it will not be reduced to a liquid entirely, and only remain at the bottom like a greasy substance, then pour off the Mercurial Water, which can be used again. 13 7. The gold sediment divide into two parts. Take one half and pour thereon alcohol, and let the mixture putrefy on a gentle heat fifteen days, and it will become blood red; this is the Lion's Blood. 8. This Lion's Blood pour into another glass retort, or phial, which seal hermetically, and give it the heat of the Dog Days, and it will at first turn black, then variegated, then light gray; when heat is increased it will turn yellow and at last deep red. This is the first Tincture. [Provided it does not explode!] 9. The Red Tincture triturate [How will a fulminate triturate?] in a glass mortar. Take one grain thereof, wrap it in paper and project it on 1000 grains of gold in fusion. When it has remained in fusion for 1 hour, the gold will turn to the second Tincture. 10. Take one part of this Tincture, project it on one thousand parts of pure quicksilver, which has been heated until the fumes arise, and the quicksilver will be changed into the third Tincture.’ Unfortunately, the subsequent stages in the process merely involve implausible transmutations of copper and iron into gold rather than cold fissioning lead into gold and are effectively invitations to commit fraud. The salient issue here is that naively presuming the alcohol mentioned to be ethanol pre-supposes the production of mercury fulminate (Hg(ONC)2), whilst Paracelsus’ definition suggests the possibility of developing a mercury salt of an oxy-acid of antimony. In his book ‘Auream Vellus’, dealing with the period 1473-5, Trismosin claims he performed a transmutation upon Cinnabar, ‘and on testing the ingot of the fixed Mercury, the whole weighed nine loth, the test gave three loth of fine Gold.’ Fixed Mercury, Mercurius Fixatus, and the alternatives ‘Mercurius praecipitatus per se’ (or ‘Calcinatus per se’) were all equally HgO, the only distinction being in the method of production which was always thought to lead to a different outcome depending on the method chosen. Trismosin's achievement was far from unique. In 1602, one Alexander Seton performed transmutations at a goldsmith's in Strasbourg and supervised one in Frankfurt, where he took care to avoid the accusation of having used the type of frauds then current, by causing his witness, a merchant named Koch, to perform it himself; the latter wrote: ‘He did not put a hand to the work himself, but allowed me to do everything. He gave me a reddish-gray powder, weighing about three grains. I dropped it into two half-ounces of quicksilver in a crucible. Then I filled the crucible about halfway up with potash (K2CO3, to avoid oxidation), and we put it over a gentle heat. After this I filled the furnace with charcoal, so that the crucible was entirely embedded in a very hot fire; I left it there for about half an hour. When the crucible was red hot, he told me to throw a little piece of yellow wax into it. A few minutes later, I cooled the crucible and broke it open. At the bottom I found a small piece of gold that weighed 54 ounces three grains. It was melted in my presence and submitted to an assay; 23 carats 15 grains of gold resulted, together with six of silver - both of an exceptionally brilliant color….' Note the point about it being a small piece of gold. All accredited examples of anomalous or paranormal transmutations that have come down to us from alchemy involved small pieces of gold. Nobody ever generated a ton of it in a single demonstration. 14 Seton certainly convinced at least one important individual of his abilities. After his servant had demonstrated a transmutation at the court of Christian II of Saxony, the latter had him tortured so badly, in the attempt to extract his secret means of making the Stone, that he afterwards died, but not before passing on his red powder to a Pole, Michael Sendivogius. Sendivogius demonstrated a transmutation to the Emperor of Bohemia, Rudolf, himself an enthusiastic laboratory worker. The Emperor had a marble plaque made, bearing the inscription 'Faciat hoc quispiam alius quod fecit Sendivogius Polonus?'; 'Whoever else could do what Sendivogius the Pole has done? Quite a few, apparently. Tales of visits by wandering strangers with the power to turn mercury and lead into gold became part of European folklore and on occasion the visits were to professional men of established integrity. One such, Dr. Johan Schweitzer, called Helvetius, was visited in Holland, in 1666, by a stranger who gave him a sample ‘about as big as a rape or turnip seed' from a stone 'about the bigness of a small walnut, transparent, of a pale brimstone color.’ Wrapped in wax and put into half an ounce of molten lead it 'made such a hissing and bubbling in its perfect operation, that within a quarter of an hour all the mass of lead was totally transmuted into the best and finest gold...' The Assay Master of the province, a Mr. Porelius, tested the metal and pronounced it genuine. Another instance in which the stone or powder appeared yellow as opposed to the more conventional red colour was a transmutation performed by Boyle's preferred authority on chemical matters, the Fleming J.B. van Helmont, in 1618. Once again it resulted from a visit by a stranger and the gift of a minute quantity of the Philosopher’s Stone, which van Helmont described as 'of color such as saffron in its powder, yet weighty and shining like unto powdered glass.' Heating about eight ounces of mercury in a crucible and adding the powder he noted 'Straightaway all the Quicksilver...stood still from flowing and being congealed settled like unto a yellow lump’ but after pouring it out 'there were found eight ounces and a little less than eleven grains of gold.' The small quantities involved and the transmuting power of the powder relative to the mass of base metal, its textural qualities and high density are all consistent with similar reports of transmutations and typical of the descriptions of the Stone given in 'theoretical' alchemical literature. A document supposedly derived from a manuscript in the possession of the Rosicrucians in 1777 describes it as 'a ponderous mass, thoroughly of a scarlet colour, which is easily reducible to powder, by scraping, or otherwise, and in being heated in the fire flows like wax, without smoking, flaming, or loss of substance, (another account reads 'flows like wax upon hot iron') returning when cold to its former fixity, heavier than gold, bulk for bulk, yet easy to be dissolved in any liquid…' 15 Relations between alchemists and the treasuries of the countries they inhabited, with their goldbased currencies, were bound to remain fraught, although Boyle managed to persuade William III's government of the efficacy of legalising the production of gold from base metal under licence. Meanwhile, the pretensions of the new scientific societies would not permit of their researching anything that had been associated with low-class charlatanism. However, in 1782, a recently elected member of the Royal Society, James Price (born Higginbotham) demonstrated the transmutation of mercury into its equivalent weight of silver using a white powder (a product of an alchemical process called the Higher Circulation, though in this case, as in similar accounts, the transmutation seems highly suspect, given the relative positions of those elements in the Periodic Table) and that of mercury into gold, using a red powder. The metals were tested and found to be genuine, causing an enormous sensation. The Royal Society felt bound to investigate the powders officially, but Price had already let it be known that they were exhausted so he was given six weeks to prepare some more. He evidently failed, a sure sign that, like all alchemists before him who thought they had cracked the Stone's chemical composition, he was really working blind. However, whatever his shortcomings as a chemist in this respect he was well apprised of the fatal effects of prussic acid. On the appointed day the Society's representatives were shown into his laboratory, Price disappeared, drank a concoction of the stuff, returned, and died before their eyes. It was the last occasion on which a learned scientific association was prepared to officially investigate the claims of alchemy. In order to illustrate the relationship between Aristotle's four elements, or states of existence, and the processes alchemists associated with them I attach a copy of a figure produced by George Ripley, termed Ripley's Wheel and dated early C15 to 1490, for which I provide the following interpretation. The Lesser Circulation Earth. Beginning 'Heere the red man to his white wife ' Iron (Mars) is added to impure antimony trioxide (Venus inverted) and the mixture put into solution after roasting since the antimony precipitates out, leaving dissolved ferric sulphide (FeS). This is then removed by washing and filtration. The presence of black sulphides corresponds with the 'nigredo' or black stage. Water. The addition of hydrochloric acid (HCl) to the antimony, followed by heating, produces a range of colours due to chlorides of impurities going into solution, particularly those of iron and copper. Air. Reflux distillation gradually separates out the compounds in accordance with their different levels of solubility (i.e. their relative ionisations) and some hydrogen sulphide (H2S) is emitted. The 'albedo', or silvery-white stage, is reached, suggesting the metal is pure, but this is misleading. Fire. Continual heating, in the alembic, or closed flask, produces a red compound, Kermesite (8[Sb2S2O]), the synthetic form of Kermes mineral. GEORGE RIPLEY'S WHEEL – Please refer to: - http://www.yudu.com/item/details/106144/ 16 The Higher Circulation Air. The 'white wife' is again antimony trioxide (Sb2O3) but this time the 'red man' is Mercury, in the guise of Cinnabar. The Kermesite from the Lesser Circulation is added, in solution, and the slow heating process recommences. Water. The 'nigredo' or black stage is reached again followed by a lighter tone as water is added and the Stibnite (Sb2S3) derived from the Kermesite hydrolises, producing sulphate (SO3-) ions. Earth. This time a stronger oxidising agent is added, probably nitric acid (HNO3) in the impure form of green vitriol, and pale nitrates form. The colour variations in these nitrates and the hydroxides and oxides that subsequently displace them, particularly those due to the presence of copper, contrasting strongly with those of antimony and mercury, may have given rise to the description 'The Peacock's Tail', a stage expected between the black and white stages. The nitrate and remaining sulphide ions are removed with steam as distillations since this stage is traditionally carried out in a retort. Fire. Oxidation by heating the precipitate left in the retort in a crucible gives rise first to a mixture characteristic of Sb2O3 and yellow mercuric oxide (HgO). Further heating then produces a crystalline red compound that melts at the boiling point of mercury. The symbol for mercury commonly appears in illustrations of the final process but is most likely intended to represent 'sophic' mercury as opposed to the metallic element. Confusion about the sequence of these stages as depicted on the wheel may be avoided by referring to the 'Sphaera colorum principalium' or 'Sphere of principal colours'. The timing of the stages of the process may be determined by referring to an interpretation of Ripley's poem 'Vision' made by one Eiranaeus Philalethes in the C17, Thought to be reliable because Philalethes himself was considered an adept, or one who had himself produced the Philosopher's Stone. They are defined in terms of the alchemist's only guide to progress, that is to say, colour change. 'In six and forty or fifty days expect the beginning of intire Blackness; and after six and fifty days more, or sixty, expect the Peacock's Tayl, and Colors of the Rainbow; and after two and twenty days more, or four and twenty, expect Luna perfect, the Whitest White, which will grow more and more glorious for the space of twenty days, or two and twenty at the most: After which, in a little more increased Fire, expect the Rule of Venus for the space of forty days more; and after him the Rule of Sol flavus forty days, or two and forty: And then in a moment comes the Tyrian Color, the sparkling Red, the fiery Vermilion, and Red Poppy of the Rock..' etc. The total time required adds up to about nine months, a typical requirement of the process. Two further points seem worth mentioning in this context. In the celebrated document 'Collectanea Chemica' (author anonymous) the usual injunction not to overheat the work during the white stage takes the following form: - '…if the dry, fixing quality of the sulphur exceeds so as not to suffer an alternate resolution of its substance into vapors, there is danger of the whole vitrifying; and thus you shall have only glass instead of the noble tincture.' The author recommends trituration 'and then its actuated mercury must be added, incorporating both 17 together till the earth will imbibe no more', a clear reference to metallic mercury and one seldom provided for the production of the Stone, plus a reference to antimony glass, a plasticised form of stibnite. The other point is that this stage is supposed, depending on the text referred to, to be carried out in a 'strong glass', earthen or iron vessel, 'well luted', even though the alternatives to a glass container would naturally deprive the researchers of their only means of identifying changes. Their more fragile glass vessels were presumed to be destroyed by the heat employed at this stage, since the pressures exerted by gases was not a recognised factor up until Von Guericke's vacuum experiments in the mid C17. Pressures above 1 atmosphere improve the quality of mercuric pyro-antimonate produced so this may be a prime instance of the alchemists recognising a requirement without understanding the reason for it. In his conclusion to 'The Sceptical Chymist' Boyle criticises, understandably, the deliberately obscure writings of Paracelsus, expressing himself in a less reserved manner than elsewhere: '...methinks the chymists, in their searches after truth, are not unlike the navigators of Solomon's Tarshish fleet, who brought home from their long and tedious voyages, not only gold, and silver, and ivory, but apes and peacocks too; for so the writings of several [I say not, all] of your hermetick philosophers present us, together with divers substantial and noble experiments, theories, which, either like peacocks' feathers make a great shew, but are neither solid nor useful; or else like apes, if they have some appearance of being rational, are blemished with some absurdity or other, that when they are attentively considered, makes them appear ridiculous.' The didactic purpose of his book was that chymists should 'learn by particular experiments, what differing parts particular bodies do consist of' and how to isolate them 'without fruitlessly contending to force them into more elements than nature made them up of, or strip the severed principles (elements) so naked, as by making them exquisitely elementary to make them almost useless.' Nevertheless, the sceptical chymist rejects the notion of settling for one or other theory if either would conflict with 'undoubted truths'. 'And, (concludes Carneades, smiling) it were no disparagement for a sceptick to confesse to you ... I can yet so little discover what to acquiesce in, that perchance the enquiries of others have scarce been more unsatisfactory to me, than my own have been to myself.' An unwholesome certainty has crept into these kinds of discussions since 1667. The 1780's brought a revolution in the concept of 'calxes' due to their identification as oxides and the development of a structured approach to chemicals in general. The scientists principally involved in it were, significantly, no more inclined to credit the original researcher responsible for the isolation of oxygen or the person whose discoveries gave rise to their own regarding this element than Michael Sendivogius was to acknowledge Alexander Seton's achievement or any other 'adept by proxy' to acknowledge the true alchemist's contribution to their borrowed status. Lavoisier, taxed with making scant reference to Cavendish in his report to the Paris Academy of Science concerning inflammable air, commented cruelly that 'those who start the hare 18 do not necessarily catch it', yet even this acknowledgement oversimplified the case inasmuch as it was Scheele who metaphorically started the hare (by identifying 'fire air'), Priestley caught it, then Cavendish, but it was Lavoisier who took it and ran with it (and named it). In order to incorporate radioactive isotopes into the established, rigid order then associated with elements previously thought to be eternal and immutable, Rutherford and Soddy put forward, in 1903, the idea of the spontaneous disintegration of atoms still current today: 'In radioactive changes the transmutation of the elements, so long but so vainly sought by the alchemists, is proceeding of its own accord. No human effort can in the minutest detail change any phase of the process; the rate at which the atoms of radio-elements break down is unchanged by temperature, by chemical reagents, or by any other means.' Rutherford's own discovery of secondary emission due to the impact of alpha rays in 1919* does not contradict the spirit of this statement so much as emphasise the difficulty of minting durable generalisations about atomic activity. All the same, isotopes are categorised as either stable and immutable or radioactive but, in either case, they are considered to be immune to the influence of subatomic particles other than those generated by particle accelerators or nuclear fallout, due to consideration of the energy barriers involved. Therefore, neither 'cold' fusion nor fission, i.e. roomtemperature transmutation, can occur. If there is any truth in the reports concerning the effects of Red Mercury Rutherford and Soddy's statement is nonetheless disproved in detail and those energy barriers no longer exist. *by 147N + 42He2+ → 168O + 11H + 10n An anecdote concerning the Philosopher's Stone* Thomas Charnock, 1524/6 -1581, related the tale of the last Prior of Bath, William Holway (or Gibbs) who, so he told Charnock several years later, possessed the 'Red Elixir' but had hidden it at the time of the dissolution of the Abbey. When, sometime afterwards, he went to look for it in the wall where he had secreted it, he could not find it, and was so overcome by grief that he temporarily lost his reason. Charnock met him as a blind old man, probably shortly after the catastrophe that had destroyed his (Charnock's) first 'Work' (another source describes Holway as "having lost his reason and gone blind and had to be led about by a boy"). According to Elias Ashmole, when workmen had pulled down some stone-work of the Abbey "there was a Glasse found in a Wall full of Red Tincture, which being flung away to a dunghill (or Rubish), forthwith coloured it, exceeding red. This dunghill was afterwards fetched away by Boate by Bathwicke men, and layd in Bathwicke field, and in the places where it was spread, for a long tyme after, the Corne grew wonderfully ranke, thick and high: insomuch as it was there look'd upon as a wonder." Witnesses to this event, or reports of its having occurred, are then mentioned. *From 'Alchemy': E.J. Holmyard. 19 Philosophers on alchemy Avicenna (Abu Ali ibn Sina), 11th. century: - Regarded transmutation as impossible "since there is no way of splitting up one metallic combination into another." He considered that the essential distinctions between one metallic element and another was unknown "And if a thing is unknown, how is it possible for anyone to endeavour to produce it or to destroy it?" Vincent of Beauvais, 13th. century: - Thought that alchemy bore the same relation to mineralogy that agriculture bore to botany and believed that metals are generated and grow in the bowels of the earth. Petrus Bonus, in "The New Pearl of Great Price", c. 1330: - "In Nature, the generation of metals takes thousands of years, and occurs in the bowels of the Earth..... Transmutation is merely the work of Nature aided by the Art and directed by the divine will." 20 8. An experiment to determine the propensity of mercury and antimony for forming mixed oxides TEST 1. After roasting stibnite, melting the impure antimony (Sb) derived from it and combining a little of the cooled crystalline compound with HgO the Hg was seen to vapourise out of the mixture; a typical reaction. However, a dark red compound was left, which withstood heating to 4000C, turning black and slightly liquid , the red colour returning as it cooled. A little water was added and feathery, needle-like shapes crystallized out on its surface. On adding a pinch of this to a little HgO plus water an exothermic reaction developed once the mixture was heated moderately, cautious repetition of the process leading, once more, to separation of the Hg from the other constituents and further separation into compounds of antimony. Observations and interpretation. Initially, a little of the pinkish-grey mixture produced after the second operation proved to be soluble. When heated it turned brown, but on cooling this separated into a grey precipitate below an orange-brown solution. This turned a russet colour on reheating, but eventually cooled to give a thin red layer precipitated on top of a light grey one. The effects of this process are practically the same as when the constituent compounds are heated separately, illustrating the perennial difficulty of persuading these stubborn metals to unite. The reaction equations obtaining here would appear to be: 2HgO → 2Hg + O2 and Sb2S3.Sb2O3 (aq) → Sb2S3 (s) + Sb2O3 (Kermesite?)heated The situation is somewhat strange as, apparently, the presence of antimony in cinnabar is not uncommon and renders the refining of the mercury difficult, suggesting amalgamation of the metals; but HgSb amalgams do not appear to be listed. TEST 2. This is designed to test the similarity in behaviour of Hg and Sb in the presence of an alkali metal to that of Mg and P combined with NH3. Should a single compound form it might later decompose in accordance with the reaction equation: 2 Mg(NH4)PO4 → Mg2P2O7 + 2NH3 + H2O By analogy, 2 HgNaSbO4→ Hg2Sb2O7 + Na2O 21 Antimony, its trioxide, its pentoxide and its trisulphide were added to HgO so that about 2 gm of the mixture was present and heated in a 150 ml flat-bottomed flask with a bent exhaust tube until an exothermic reaction developed. Allowed to cool, it was removed to an evaporating dish and warmed until it resembled a single compound, by reason of its uniform appearance. Sodium peroxide solution was added to a sample of it, together with a little of the Kermesite (?) from Test 1 and it was left to soak overnight, then heated until another thermally stable compound was seen to form. Observations and interpretation. Initially dark brown, the mixture turned black on heating. The exothermic reaction proceeded vigorously, a splint test confirming the emission of oxygen gas, with light grey and white vapour condensing on the inside of the flask. The mixture itself turned light grey, then a reddish-lilac colour when allowed to cool, a mirror effect forming on the inside of the flask the while. As crystallization occurred a pale, powdery crust appeared above the light red crystals. Adding water restored the brown colour but a russet colour, accompanied by the development of a texture like that of clay, appeared when the product was reheated. Meanwhile, the appearance of tiny beads of Hg upon its surface indicated that progress to a stable compound had not yet been achieved. On adding sodium peroxide and Kermesite (?) an opaque amber solution was seen to form which then cleared leaving a pinkish precipitate. Upon heating, Hg gradually re-appeared as tiny beads upon the precipitate. It may be surmised that, in the first instance, the reaction: Sb + Sb2O3 + Sb2S3 + 2HgO → Sb + 2Sb2O3(v) + Sb2S3(v) + 2Hg(v) + 2O2↑ occurred, and subsequently: 2Sb2S3 + Sb2O3 + Sb2S3.Sb2O3(aq) + Na2O2(aq) + 3HgO(s)→ Sb2S5 + Na2S + Sb2S3 + O2 + 3Hg All of the elements, save oxygen, formed a single unidentifiable, thermally unstable complex. TEST 3. Mercuric chloride was added to some of the Kermesite(?) in a boiling tube and heat applied until the sequence of colour changes appeared to be complete. After allowing it to cool until its appearance changed it was reheated to drive off any remaining water and heated in a 0.5L roundbottomed flask with thermometer, testing for thermal stability. Trituration of the resultant product then served to confirm its consistency and fixedness. Observations and interpretation. A creamy-pink transparent solution formed, turning deep brown on heating, then grey. Allowed to cool, it turned light greyish yellow with a grey precipitate. On dehydration a grey concretion with a powdery white surface appeared, but almost all of this vapourised, leaving a creamy white 22 coating on the entire inner surface of the flask, only a few small crystalline lumps remaining in the bottom. Trituration yielded a uniform grey-brown powder. The creamy white powder suggests the presence of mercury (finely divided), antimony trioxide and mercuric oxide, as its readiness to vapourise would seem to confirm. The remaining lumps probably contain a complex of sulphides and the appearance of the triturated product supports this as well as the supposition that the chloride ions had all been emitted as chlorine gas by this stage. However, stable sulphides are readily obtainable from combining cinnabar or mercuric oxide with antimony oxides or sulphides. They do not produce stable mixed oxides when heated, unless, perhaps, they are heated under oxygen or for much longer than would be usual given the time constraints in a modern laboratory. TEST 4. A layer of moistened antimony pentoxide (<1gm) was applied to a supporting mesh of iron wire and covered with ~1gm of mercuric oxide (yellow particulate form). This was heated, gently at first, then more strongly, in a length of combustion tubing, until the cycle of changes appeared to be complete. The resultant product was then scraped off the wire and the inside of the tube, triturated with sodium hydroxide crystals and replaced, unsupported, in the tube. This was heated strongly until an exothermic reaction developed and then again, to observe the dehydrated product. Observations and interpretation. The layered mixture turned orange, then dark red when heated strongly, vapourisation occurring but ceasing rapidly when it was allowed to cool. It appeared to solidify as an orange-brown product but the red colour returned on reheating it. However, with the sodium chloride added it first turned black and moist and then bubbled like potassium carbonate when heated. Finally, a light-grey, blue, green and yellow variegated product resulted, vitrification appearing where it touched the glass tube. Essentially, the reactions indicate the production of Schlippe's salt (dehydrated) or sodium thioantimonate, which forms yellow, tetrahedral crystals. These would appear green or blue when intimately mixed with the grey mercury and antimony. The initial reaction would be: 2HgO → 2Hg + O2 (incomplete reaction) (heated in presence of antimony) followed by: 6NaOH + Sb2S3 → 3Na2S + Sb2O3 + 3H2O(v) Then, on reheating: Sb2S3 + 3Na2S + HgO + Sb2O3 → 2Na3SbS4 + Hg + 3O2 23 CONCLUSION The limited oxidising effect of the halides, on Hg at least, is well illustrated by the failure of the chloride ions to replace the sulphide ions in Test 3. Iodine, though it forms HgI readily enough with HgO, disguises the development of the red mixed oxide of Hg and Sb and the iodide is difficult to eliminate afterwards so it was not introduced into the process. The alkali metals seem better candidates when it comes to producing complex catalytic compounds aimed at assisting oxidation. Potassium introduces the sort of dangers associated with the nitrates and ethanol but sodium is less problematical and is equally easy to separate by filtration from the less soluble mercury and antimony ions. Combination of mercury with a Group 5 element more reactive than antimony, in a mixed oxide, might appear to be a suitable intermediate strategy but nitrogen excludes itself because it forms dangerous nitrates. Not having a bismuth compound to hand I tried using orthophosphoric acid. A fine, crystalline, white powder is produced when mercuric oxide is slowly heated in an excess of this acid. As tiny droplets of mercury were seen to form on the surface of the powder after it had been left standing for a few days, it might be thought that this compound was unstable at room temperature, but this symptom is characteristic of the standard reaction for the production of mercuric phosphate. Consequently, phosphorus may yet prove to be the most suitable Group 5 element for the purpose of producing a mixed oxide of antimony and mercury by a displacement reaction. The problem highlighted by these tests is the mutual reduction of mercury and antimony compounds to their metallic elements, or, at any rate, the reduction to mercury and an antimony compound. It is difficult to create antimony amalgam but there is sufficient tendency for it to form to cause gaseous ions like oxides and chlorides to be expelled from mixtures of their compounds due to their displacement by the metal atoms. Heating the metals together does not appear to reverse this process. It simply prevents their oxides from forming. In observing the diagrams of infinite chains of mercuric and oxide ions and antimony hexoxide octahedra the adjective polymeric comes to mind. It is not surprising that early chemists associated them with organic substances. The emphasis laid on complete purification of the metals, in alchemical literature, becomes understandable in the current context since any impurity could form a buffer compound, preventing a slow reaction that was difficult to maintain from taking place at all. The vitreous character attributed to the Stone links it, by association, to the pyroxenes. Nonetheless, it would have been easy for the fragile soda glass vessels used by the alchemists to contribute to the final product due to long term thermal stress gradually breaking down the surface of the glass, a process that could easily go undetected. The production of pure mercuric pyro-antimonate seems to require an unusually close packed arrangement of metal ions in the crystal structure in order that its high thermal stability should not be compromised by the natural volatility of the metals. However, on the basis of these test results, the only response to the question "What tendency have antimony and mercury to form a stable mixed oxide?" must be "Hardly any". 24 9. Note on silicates that may have entered into the composition of 'philosopher's stones' during their production. Medieval alchemists' glass vessels were notoriously friable, their tendency to shatter under the stresses generated by pressure and heat being due not only to early chemists' misunderstanding of energy transfer mechanisms between their reactants, which led to unexpected exothermic reactions, but also to a failure to fortify the soda glass with metals during the production process. In short, they had no 'Pyrex' brand containers. Coloured glass was made in ancient Sumeria, by the addition of powdered metals to the molten glass and this may have more than a circumstantial association with some of the descriptions of the (supposed) transmuting powder. The inclusion of thinly veiled references to sand was not unusual in the context of alchemical recipes. However, it is more likely that the alchemists sometimes rediscovered the ancient colouring technique by default, if only because they placed their reactants in 'hermetically sealed' vessels for months on end. This circumstance would have provided ideal conditions for the incorporation of glass shards into the emerging 'stone'. Therefore the sample of 'transmuting powder' given to Van Helmont in 1618, which he described as being 'of colour such as saffron,.... , yet weighty and shining like unto powdered glass' , may well have been just that, i.e. glass. 25 10. X-ray diffraction This is used to distinguish the crystal planes comprising atoms of one element from those of another. The X-rays are uncharged, being electromagnetic waves, but interact with the electrons surrounding the nuclei of the atoms. The number and distribution of the electrons being different for the atoms of different elements, they reflect the X-rays differently. The result is that a series of planes of reflection for each element involved, when presented in turn to incident X-rays, reflect the rays at different angles, termed scattering angles. This produces a complete set of peaks in the intensity of the reflected rays which is related to those scattering angles, for each of the elements in a compound. The X-rays themselves are generated by interactions between electrons. In 1913 Henry Moseley investigated the production of X-rays, bombarding samples of different elements with electrons and then measuring the energy of the emitted rays by recording their scattering from a single potassium ferrocyanide crystal. Einstein had already worked out the relationship between a wave's energy and its frequency, which is given by his equation E = hf, where h is Planck's constant. So Moseley could calculate the frequency, f, of his X-rays from their energy, E. He found the frequency to be related to the atomic number, Z, of the bombarded element by: f = a(Z - b)2 where a and b are constants. Now, as the frequency of a wave is related to its wavelength, lambda, by: - c = f lambda, c being the speed of light, Moseley could check the spacing between the atomic planes of his scattering crystal by using the Bragg equation: n lambda = 2d sin thetaB (see Appendix D). Of course, he had to use this equation to derive the wavelength and hence the energy of the rays, but adjustment of the crystal position provided intensity peaks related to the different scattering angles (2 thetaB) so he could check the consistency of the relationship of his values for d and E over the intensity range. Maximising the number of crystal planes available at a given angle with respect to the incident Xrays maximises the intensity of the reflected rays for angles at which they are in phase, one with another. Grinding the crystalline test sample to a fine powder maximises the number of crystal planes lying at all angles. Slowly rotating a finely powdered sample of the element/compound in a beam of X-rays emerging from one fixed direction then presents a large number of crystal planes to those rays. This is the principle behind the Debye-Scherrer X-ray powder camera, which produces a set of lines on a negative, representing the reflected ray intensity peaks. The process was later computerised to generate a graph of the X-ray counts comprising the peaks against the scattering angles. 26 A set of intensity peaks presents a pattern characteristic of a particular crystal structure but it does not follow that the structure itself is readily identifiable. This is because the positions of atoms in a crystal are represented far more accurately by the positions of their tiny nuclei than their spread out electron shells. It is those atomic positions that identify the crystal structure (see 11. Neutron diffraction). Whilst the intensity with which the rays are reflected from the atoms comprising unit cells of the crystal structure is crucial to determining their composition the calculation of the intensity appropriate to a given structure is a much more complex process than that involved in the calculation of the plane spacing. It is given by: I0 = K2 C S02 S0 is called the observed structure amplitude, a measure of the amplitude of the waves reflected per unit cell. I0 is the observed intensity per unit cell of reflected X-rays. K is a scaling factor related to S0. C is a factor dependent on the cell characteristics and experimental conditions. Unsurprisingly, it is far easier to compare the intensity of reflected X-rays for a known unit cell, using data derived from a previous experiment, involving a reliably pure samples repeatedly tested to provide a standard reference, than to start from scratch and build up a picture of the structure just by analysing a test sample and trying to estimate K and C. However, it is worth while approaching the problem as if the ambient conditions, and hence C, were constant over a reasonable period of X-ray exposure, say, 2 hours, so that the relationship between intensity and structure amplitude may be regarded as constant for a given experiment. Then at least, meaningful comparisons may be made between the intensity peaks for the test sample and those for the standard. This is because once the peaks have been associated with specific planes of reflection the ratios of the peak intensities in relation to one another are a constant for any particular structure, i.e. there is no need to calculate their individual absolute values as per the formula. The relative intensities of identified peaks for a test sample can be compared with those for the standard and conclusions drawn. Sadly, a reliable standard is not always available, particularly in the case of a rare compound and that was the predicament I found myself in with regards to mercuric pyro-antimonate. 27 11. Neutron diffraction Similar in both theory and experiment to X-ray diffraction, its importance arises from the significant differences in the scattering of the two types of radiation. Two important interactions dominate neutron scattering, analogous to light-wave interference processes. 1. The short-range, nuclear interaction of the neutron with the atomic nucleus. This is similar for different elements since the strong resonances associated with the scattering process prevent any regular variation of the nuclear scattering wave amplitudes with atomic number. 2. The interaction of the magnetic moment of the neutron with the spin and orbital magnetic moments of the atom. The amplitude of the interaction varies with the size and orientation of the atomic magnetic moment and the intensity of scattering depends on the angle of spin of the magnetic electrons in the atom. The angular distribution of the scattered neutrons is measured when determining the structure of many materials. Both polycrystalline and single-crystal specimens can be examined but single crystal techniques provide much better resolution of the diffraction peaks. However, a significant application in chemical crystallography is the structure determination of composite crystals which contain both heavy and light atoms (and the ratio of the relative atomic masses of Hg to O ≈ 25:2 and of Sb to O ≈ 15:2). Crystal analysis by the neutron interferometer (invented 1974) is facilitated by growing huge, essentially perfect, crystals (up to 10 cm.) Fortunately, the alchemists’ reports suggest Red Mercury has a tendency to imitate Kermesite, mineral antimony oxysulphide, in its propensity for crystallization. 28 PART II 1. Introduction, containing a relation of the new influences that were brought to bear on my researches after April '96. In April 1996 two things happened which gave new direction to my researches into mercuric pyroantimonate. One was that a correspondent to the '<dejanews>' Internet website, Erick Singley, provided the International Chemical Register (ICR) Number for it; 20720-76-7. The other was that a book published in '95, 'The Mini-nuke Conspiracy', came to my attention. It contained the ICR number plus the name of the chemist, Dr. Sleight, who had synthesized one or more allotropes of it for the American explosives manufacturer Du Pont de Nemours, in 1968. Using this information I easily found the chemical abstract (or note concerning the experimental report) in volume 69 of the Chemical Abstract Services (CAS) output, abstract number 71239v. The description appearing against the ICR number would not inspire much confidence in anyone unfamiliar with the one available in 'The Mini-nuke Conspiracy', where it is described as 'a mercury salt of antimonic acid': 20720-76-7 Antimonic acid (H4Sb2O7 ), mercury (2+) salt (1:2) H4O7 Sb2 .2Hg However, anyone who had attempted to produce the compound using reaction (2) on page 3 of Part I* would recognise the reactants referred to. Unless they had a supply of oxygen available they would also recall their observation of the ease with which mercury is liberated from a compound when it is heated in solution. My own experiences with this method were so disappointing that I did not even include it in my test reports. The thing to remember about its limitations is that they only obtain for the thermally unstable allotropic forms of the compound. Another situation hardly calculated to inspire confidence in the procedure is J.R. Partington's reference to antimonic and antimonious acids in his 'Textbook of Inorganic Chemistry', where he states that their existence is 'extremely doubtful'. Antimonic acid's formula appears against 'Antimony oxyhydrate' in R.C. Weast's 'Handbook of Chemistry and Physics'. Now, if the ICR description is considered inconclusive what may be said of the one in the abstract? I had already examined the CAS Subject Index for 1967-71 before April '96 during the course of a trawl through the service's indices, looking for mercury salts of all possible descriptions. The sought-after compound appeared as: mercury (2+) salt (1:2)[20720-76-7], crystal structure of, 69 :71239v * (2) 2HgO + H4Sb2O7 → Hg2Sb2O7 + 2H2O 29 2. Dr. Sleight's report to the Journal of Inorganic Chemistry of April '68. Referring to the abstracts one finds: 71239v New ternary oxides of mercury with the pyrochlore structure. Sleight, A.W. (E.I. du Pont de Nemours and Co., Wilmington, Del.) Inorg. Chem. 1968, 7(9), 1704-8 (Eng). Three new ternary oxides of Hg- Hg2Nb2O7, Hg2Ta2O7 and Hg2S2O7 (sic) - have been prepd. and characterized....... Perhaps unsurprisingly, I had not considered it worth my while to take a look in volume 7 of the Journal of Inorganic Chemistry for '68 in order to find out if the CAS were mistaken in referring to a pyrosulphate (hardly a likely compound given the valency of sulphur). Of course, a cross-reference to their number index would have confirmed this, as the CAS were to do when inquired of, calling the misprint a 'typographical error'. In any case, I had no good reason to follow up such an old lead when the 'red mercury' scare appeared only to have started in '93, particularly since I would have had to rely on such a prestigious organisation as the CAS making a mistake with a short chemical formula. Further research, after April '96, failed to find any more references, indirect or otherwise, to Hg2Sb2O7 in CAS literature, wherefore it might be said that there is no specific reference to the formula in scientifically respectable literature outside of Dr. Sleight's report and the reference to its structure in Well's 'Structural Inorganic Chemistry'. As to the practical significance of Dr. Sleight's report, suffice it to say that has served me as a source of information for the 3 years in which I have refined my experimental procedures and sought to account for the discrepancies between the results of his X-ray analysis of his version(s) of the compound and mine. The final product was a pasty brown powder, thermally stable to some temperature above the melting point of Pyrex glass, which stains the melting glass an orange-brown colour without appearing to melt. It turns a yellow-ochre colour as it adsorbs onto the surface of molten lead (doubtless litharge is added to its composition) and it also adsorbs onto the surface of mercury at room temperature, but not to the extent that anyone could call the resultant amalgam viscous. The one positive result of the process has been the achievement of the 'fixation of mercury' and if that is what grabs you then read on. 30 3. The production of pyro-antimonic acid (H4Sb2O7) and mercuric oxide (HgO) (from ‘A textbook of Pure and Applied Chemistry’- Garside & Phillips) 'Various hydrated forms of (antimony pentoxide), corresponding in composition to the ortho-, pyro-, and meta-antimonic acids, have been prepared....Thus hydrolysis of antimony pentachloride by boiling water, followed by drying the resulting precipitate at 1000C, produces the hydrate corresponding to pyro-antimonic acid, H4Sb2O7 : 2SbCl5 + 7H2O → 10HCl + H4Sb2O7 The hydrochloric acid is filtered off after precipitation has occurred.’ Heating mercury in a partially evacuated, round-bottomed flask until it is mostly deposited as a condensed vapour all over the interior and then adding nitric acid before repeating the procedure will produce mercuric nitrate. Further heating whilst distilling the fumes from the compound with a Leibig's condensor gradually yields mercuric oxide. The reactions are: 2HNO3 + Hg → Hg(NO3)2 + H2↑ followed by 2Hg(NO3)2 → 2HgO + 4NO2↑ + O2 ↑ 31 4. Masses involved in preparation of Hg2Sb2O7 [Error = 0.02gm throughout unless otherwise specified] Reactants: - Required molar mass ratio of Oxide:Acid = 434:360 = 1.206:1 Mass of beaker 1 + H4Sb2O7 = 65.34 gm – Mass of beaker 1 = 54.86 gm = Mass of H4Sb2O7 = 10.48 gm ±0.03gm Mass of beaker 2 + HgO = 19.33 gm – Mass of beaker 2 = 7.14 gm = Mass of HgO = 12.19 gm ± 0.03 gm Measured masses have an Oxide to Acid ratio of 1.163:1 Mass of boiling tube 1 + reactants = 68.00 gm − Mass of boiling tube 1 = 45.33 gm = Mass of reactants = 22.67 gm ± 0.03g Product: - Molar mass ratio of reactants to desired double oxide = 794:758 = 1.048:1 Therefore, expected mass of Hg2Sb2O7 = 22.67 gm/ 1.048 = 21.63gm (ignoring the discrepancies between required and measured mass ratios for now). Final mass of boiling tube 2 + product, after heating under oxygen and expulsion of steam from tube = 63.95 gm – Mass of boiling tube = 43.74 gm = Mass of Hg2Sb2O7 = 20.21 gm (Error in these last values is ± 0.05g) 32 The amount of water lost due to evaporation of the water generated during the reaction may be calculated from the masses of the reactants and expected product and is 1.04gm. The remaining difference of 1.42gm between the expected mass of the product and that found is readily attributable to Hg being lost through the oxygen outlet tube along with any nitrate remaining as an impurity from the HgO production process. Likewise it would also be due to the discrepancy in the required to measured mass ratios of the reactants, the acid being the determining (or limiting) constituent and the surplus HgO subliming, with Hg, as a 'frost' onto the inside of the boiling tube. It has something of the character of the nitrate but is powdery rather than having the whiskery, needle-like appearance of the latter. FURTHER PROCESSING OF THE PYRO-ANTIMONATE AND THE MASSES FOUND, TOGETHER WITH AN INTERPRETATION. By repeatedly heating the product under oxygen and returning any further sublimate to it, also heating it in the partially evacuated boiling tube over a candle, and overnight, it gradually approached a condition in which it was thermally 'semi-stable' Having repeated this procedure on the several occasions when I have carried out this experiment, with variations, I can state with confidence that this never takes less than 3 weeks. Following this stage, the product was heated over a candle for a lengthy period during which it gradually turned from a yellow-ochre to a cream-white colour. Heating it again over a Bunsen burner turned it a chalk-white colour. There was much sublimate and this was collected. Mass of sublimate from Hg2Sb2O7 + petri dish = 13.090 gm _ Mass of petri dish = 6.953 gm Mass of sublimate = 6.137 gm ± 0.03g Mass of residue + boiling-tube = 63.751 gm _ Mass of boiling tube = 52.369 gm Mass of residue = 11.382 gm ± 0.03gm 33 5. The interpretation of X-ray scans of my oxide samples, the adjustments in my experimental approach and the final results of the experiments. If you are unfamiliar with the principles of X-ray Crystallography, refer to APPENDIX D. BASIC CRYSTALLOGRAPHY. There you will notice that the last equation in the section 'The Law of Rational Indices' is: h2/a2 + k2/b2 + l2/c2 = 1/d2 The most important thing to note at this point is that Dr. Sleight identified mercuric pyroantimonate as a compound with a cubic pyrochlore structure. As lengths a, b and c are identified with the orthogonal axes of the unit cell, which is, in this case, a cube, a = b = c. The equation therefore simplifies to: h2/a2 + k2/a2 + l2/a2 = 1/d2 (h2 + k2 + l2)/a2 = 1/d2 At this point, refer to the equation for first-order reflections, which appears in the section 'X-rays and the atoms in a crystal lattice': sin2θ B = (λ 2/4)(1/d2) Next, substitute the previously derived value for 1/d2 in this equation, to give: sin2θ B = (λ 2/4)(h2 + k2 + l2)/a2 This is the equation from which the values of the Bragg angles,theta B, are to be derived. The squared length h2 + k2 + l2 is the square of the hypotenuse for the 3D equivalent of Pythagorus' Theorem. It is equal to S2, S being referred to as the Structure Factor. Dr. Sleight determined that the structure of mercuric pyro-antimonate was face centred cubic, with Cell Edge, a = 10.349 Ångströms. (The Ångström = 1 × 10-10of a metre). Now refer to the Bragg formula for a cubic crystal structure: sin2θ B = (λ 2/4)(h2 + k2 + l2)/a2 34 Substituting for 'a' and using lambda = 1.54 Ångströms, (taken to 3 s.f.s), gives a value for lambda /a of 0.1488066, denoted 'r' in the following lists. The Bragg angles and Scattering angles are then, by my calculation: h k l sin θ B = [S/2]r θ B θ S = 2 θ B(to 3 s.f.s) 111 (3/4) r 7.40 14.8 311 (11/4) r 14.29 28.6 222 (3) r 14.94 29.9 400 2r 17.31 34.6 331 (19/4) r 18.92 37.9 511 (27/4) r 22.74 45.5 440 (8) r 24.89 49.8 531 (35/4) r 26.12 52.2 622 (11) r 29.57 59.2 444 (12) r 31.03 62.1 711 (51/4) r 32.10 64.2 553 (59/3) r 34.86 69.7 35 Dr. Sleight's observed intensities Iobs for Hg2Nb2O7 sample, standing in for Hg2Sb2O7 (both having a pyrochlore structure 'with the same positional parameter') expressed as ratios of the smallest peak, reflected from the {444} planes: All these peaks are above 1,000 c.p.s. hkl Iobs {222} 10.26 {400} 3.51 {440} 4.06 {622} 3.94 {444} 1.00 Equivalent data (Iobs) for scans obtained using data from my own samples. All the peaks used for the purpose were with ± lº of the angles derived using Dr. Sleight's value of 10.349 Å for the relevant lattice planes: Scan 15 16 hk1 Hg2Sb2O7 17 19 20 21 → |Hg2Sb2O7 + Hg2Sb2O6 {222} 3.40 2.02 2.40 4.64 6.40 5.51 {400} 1.42 1.43 1.77 2.44 2.36 {440} 1.62 1.22 1.14 2.03 2.75 2.37 {622} 1.12 1.31 2.23 2.60 2.10 1.00 1.00 1.00 1.00 1.00 - - {444} 1.00 36 6. Conclusions drawn from comparisons of my samples to those described in Dr. Sleight's report. As the sublimate from the Hg2Sb2O7 has every appearance of being impure HgO and has a mass = 0.503 of the mass of HgO originally added it might be supposed that the residue was HgSb2O6. Now, diffraction scans 17 to 21 demonstrate the compatibility between the scattering angles for the residue and those calculated using Dr. Sleight's data for Hg2Sb2O7. The mass of the residue and that calculated for the product of the principle reaction are in the ratio 0.526:1, suggesting that, within an allowable error of ± 0.5g, half of the Hg2Sb2O7 produced has been subsequently lost but the residue is still the pyro-antimonate. However, scan 22 confirms the first impression given by the sublimate; it is predominantly HgO and the residue cannot, therefore be pure pyro-antimonate, experience having in any case shown that antimony compounds, like the element, are less volatile than mercury compounds. The high thermal stability of the residue in its cream-coloured form, as it is observed to convert eventually to a reddish-brown substance when heated strongly, suggests that Dr. Sleight, or rather, his assistants, misdiagnosed the latter compound. He considered that 'in samples apparently slightly deficient in mercury and oxygen the cell size was decreased' so, as the FCC structure and unit cell edge dimension that he quotes appear to apply to the residue, it cannot be a pure compound with the formula Hg2Sb2O7. Speculating that the residue is a combination of Hg2Sb2O7 and HgSb2O6 in the molar ratio 1:1, the mass ratio of HgO to the remaining oxide is that of 3HgO to 2Sb2O5 or 650:647. This is 1:1 within the error margins involved. Add half the mass of the residue (5.69g) to that of the sublimate (6.14g) and the sum (11.83g) is within 0.5g of the mass of HgO originally introduced (12.19g). The equivalent loss of Sb2O5 is seen to be 9.44g - 5.69g = 3.75g. Given the relative volatility of the metals, the ratio of the oxide losses suggested here, 1.64:1, is certainly in line with expectations. An FCC structure with the compound formula Hg3Sb4O13, comprising 80 atoms per unit cell, i.e. with Z = 4, and arranged as alternating lattices of SbO6 octahedra plus HgO chains and SbO6 octahedra plus Hg chains in four-fold symmetry would seem to fit the bill. Anything else would most likely be a mixture, at least in part, so that it would have a lower thermal stability and exhibit many more peaks on the X-ray diffraction scan. Of course, only mass spectroscopic analysis could confirm the mass ratios of the elements present but the diffraction analysis does at least point to a credible alternative to Dr. Sleight's interpretation of the differently coloured samples of Hg2Sb2O7 with their variable purities. THE CRYSTAL STRUCTURE OF MERCURIC PYRO-ANTIMONATE BY REFERENCE TO THE UNIT CELL. 1. As per Dr. Sleight's report. 2. Including only 'axial' oxide ions, i.e. those directly linking the mercury and antimony ions. 3. With 'construction lines' added to highlight the octahedra. 37 7. Note on Dr. Sleight's work after 1968, including his contribution to the development of superconductors and Arne Magnéli's contribution to the study of the structure of transition metal oxides. Dr. Sleight continued his study of new ternary oxides after 1968. He reported results for platinum and palladium pyrochlores (1969), tantalum and platinum pyrochlores (1977 and 1995) and rhenium, osmium, iridium and platinum cubic crystal ternary oxides (1981). Also on potassium metaantimonate (1985), zirconium and vanadium pyrophosphates (1996) and numerous other ternary oxides. Over the same period, he took an active interest in high-temperature superconductors, which were all complex oxides containing copper sesquioxide octahedral units at that time. He found other metals could be used in place of the copper, but only for oxides that became superconductive below the boiling point of nitrogen. He studied superconductive barium plumbate bismuthate, Ba Pb1-x Bix O3 (report published 1983) and published 'Oxide superconductors: a chemist's view', 'Crystal chemistry of oxide superconductors' and (with Uma Chowdry) 'Synthesis of oxide superconductors'(1987-9). A distinguished crystallographer, Arne Magnéli, interested himself in one of the mercury antimony oxides. He analysed the structure of the meta-antimonate in 1941, finding it to consist of layers of linked antimony sesquioxide octahedral separated by layers of mercury (see B.J. Aylett's 'Chemistry of Zn, Cd and Hg'). The date of this analysis, 27 years before Dr. Sleight reported his X-ray analysis of mercuric pyro-antimonate, is significant as it accurately suggests that Magnéli had an early insight into the structure of these mixed oxides. Magnéli (1914-1996) was a Swedish crystallographer and solid state chemist. He specialised in X-ray crystallography, particularly with regards to its application to complex oxides with unusual atomic ratios. Most compounds involve simple ratios between the quantities of the elements they contain, i.e. the number of atoms representing one element relative to those of another is typically 2:1, 3:1, 4:1 or the like; maybe 5:3 but not usually anything more complex. These are termed stoichiometric compounds. However, there also exist compounds with highly incommensurate relationships between the constituent elements, such as 59:23 or worse. These are termed nonstoichiometric compounds, or are said to possess unusual stoichiometry. Crystalline substances with these unusual stoichiometries are frequently found to contain recurrent structural dislocations. Magnéli discovered that the crystals had been subjected to pressures that caused them to exhibit stress characteristics, distorting them from structures that would otherwise have contained atoms of different elements in a simpler ratio to each other. This is termed crystallographic shear. From 1953 he and his students at Stockholm University worked on the structural chemistry of transition-metal oxides and alloys, such as vanadium and titanium oxides. These studies led to the clarification of the distinction between stoichiometric and non-stoichiometric compounds. In 1970, he was elected a member of the Royal Swedish Academy of Science. 38 In 1962 Dr. Sleight and Arne Magnéli worked together to determine the structural relation between niobium and tantalum-tungsten oxides and the tetragonal crystal form of potassium tungsten bronze. Note that they were examining an alloy, with its loose mixture of compounds and unbonded atoms and crystalline compounds in which the atoms are all bonded into the structure. An important feature of mercuric meta- and pyro-antimonates is that they comprise alternating layers of antimony sesquioxide octahedral in long criss-crossing chains and mercury or mercuric oxide, in long criss-crossing lines of linked mercury atoms or alternating mercury and oxide ions. Neither the mercury and antimony atoms nor their associated oxide ions are actually bonded to each other. They occupy stable structures but do not depend on electron bonding to do so. It is as if they have been forced into the arrangements by the sort of forces that exist between connected layers of molecules, the Van de Waals forces. Such is the nature of crystallographic shear. It is also perfectly possible that the two sets of layers interleave themselves gradually under the action of a low but steady heat, as seems from experience of the production process to be the case, and then only dissociate again when the heat reaches temperatures in excess of the boiling point of mercury and the melting point of antimony. In a sense they are rather like the atoms of different metals, loosely bonded to form an alloy. Oleg Sadykov, the Russian chemist who discovered mercuric pyro-antimonate in the same year as Dr. Sleight, 1968, thought that it could be used to produce new high temperature superconductors, though it is not at all clear why he thought this was so. Magnéli's insight into the structure of the mixed oxides showed that they should not be regarded as simply connected ionic forms and sometimes possessed special properties. Maybe one of those properties, for the correct choice of metals, was that a unique type of amalgam could be formed with one of these oxides, one that could reflect neutrons far more effectively than mercury on its own once the oxide ions had been expelled from it. 39 8. The use of neutron reflectors in nuclear reactors; mercury as a neutron mirror. The neutron cross-section of an atomic nucleus is σ = πR2, where ‘R’ is the radius of the effective target area presented to an incoming neutron per atom of the reflecting material. Also, σ = Rs/Φi, where Rs is the neutron scattering rate and Φi is the incoming neutron flux (i.e. number of neutrons flowing in towards the atom/second) per unit of the effective target area. The neutron cross-section for a nuclear interaction is a measure of the probability of the occurrence of that interaction, P(O). Indeed sigma is directly proportional to P(O). Also, sigma equals the inverse of the probability density (i.e. the probability of the event per unit volume). Nuclear fission, as its name implies, involves the splitting of atomic nuclei, releasing a large amount of energy and one or more neutrons per nucleus. The neutrons sustain a fission process by battering other nuclei, causing them to split, releasing more energy and neutrons, which batter other nuclei in their turn, producing a self-sustaining chain reaction. The average lifetime of a free neutron is 900 seconds, after which it decays, typically into a proton (p), electron (e) and electron's antineutrino (¯νe). This is a long time in nuclear reaction terms. Whether or not a fission reactor can continue to operate depends on the persistence or otherwise of a chain reaction requiring free, fast-moving neutrons. The progress of this reaction is governed by the effective multiplication factor ke: ke = neutrons into the system/sec/ neutron gain rate = P , neutrons out of the system/sec/ neutron loss rate A + L where P = the average number of neutrons emitted per second = vF neutrons/sec, where 'v' is the number of neutrons per fission event and 'F' is the fission rate, A = the rate of absorption of neutrons by the reactor, and L = the rate of neutron leakage by the reactor. The size of the reactor is measured, for operational purposes, in terms of the neutron cross-section of each fissile atom, in Barns per atom, where 1 Barn = 10-24cm2, a measure of the effective target area per atom exposed to an incoming, thermal (i.e. relatively slow-moving) neutron. As the size of the reactor increases, assuming its shape to be roughly spherical, the rate of neutron leakage through the surface, L, decreases because the volume of the reactor, represented by the number atoms it contains, increases at a greater rate than does its surface area. The probability of a fission event due to the neutron-nucleus interaction depends on the number of atoms between a neutron and the reactor's surface. As this increases the chance of the neutron leaving the reactor without initiating or participating in the fission chain reaction, generating more neutrons, diminishes and the multiplication factor increases. Since ke= P. 1 . A(1 + L/A) = vF. 1 . A (1 + L/A) 40 Then ke= vF (Lim L/A→0) A There is a reactor size, in Barns, for which ke= 1. This is called the critical size of the reactor. The fissile mass associated with the critical size is called the critical mass of the reactor. The region containing the fissile material is called the reactor core. If Red Mercury performs as reported it reflects neutrons back into the core of the fission bomb, which is, of course, an explosive version of a fission reactor. In so doing it must effectively increase the critical mass of the bomb core. As shown on p.292 of 'The Mini-Nuke Conspiracy' the fuses placed with the RM capsules are exploded, causing implosion of the RM into the radioactive fissile core and activating the bomb by suddenly increasing the quantity of neutrons reflected back into the core, with the subsequent development of a fission chain reaction. However, if there is insufficient fissile material or an excess of absorbing material in the core, i.e. vF/A < 1, always, then there is no reactor/bomb size for which a steady chain reaction can be produced, irrespective of the presence or otherwise of RM. For a nuclear fission reactor using uranium (U) as the fissile material, with neptunium (Np) as a transition product and plutonium (Pu) as the final product, the process can be expressed in symbols representing the 3 transitions. The symbols n, γ, β-, and ¯νe stand for neutron, photon, beta particle (i.e. electron) and electron’s anti-neutrino, respectively. For an atom of the element AZX, the Z number represents its atomic number and the A number its atomic mass number. (1) 23892 U + n → 23992U(unstable)→ 23992U + γ (2) 23992U → 23993Np + β- + ¯νe (3) 23993Np → 23994Pu + β- + ¯νe In order to make the universally popular (other than for its victims) fission bomb it is only necessary to pack 2 blocks of plutonium, representing 2 sub-critical masses, separately, in a nuclear warhead, with a third compartment holding a chemical explosive. When the latter is detonated it blasts one block of the plutonium into the other, causing the rapid conversion of 2 sub-critical masses into one supercritical mass and producing an uncontrollable fission chain reaction for each fission reaction: (4) 23994Pu → 23592U + 42He. The only atomic by-product of the explosion, apart from the uranium, is stable helium, so at least the process itself is carbon neutral. In order that a reactor should maximise its efficiency it is essential to provide the container vessel with a neutron reflecting barrier or shield. The elements comprising the shield are therefore critical to its effectiveness as they are required to have a high 41 neutron cross-section with respect to the absorption or reflection process. The mercury nucleus presents a relatively high cross-section to thermal (i.e. slow-moving) neutrons, 380 Barns per atom or 1.14 cm 2 of the area presented by the metal per gram of its mass. Only 8 naturally occurring elements present a higher cross-section to such neutrons, lithium, boron and 6 rare earth metals unknown to the alchemists. Antimony has a thermal neutron cross- section of 9.3 Barns per atom so is unlikely to play much of a part in the fission process. The amalgam containing mercuric pyro-antimonate, identified by the term Red Mercury, would have a lower density than mercury itself, 7.57 gm cm-3 as opposed to 13.6 gm cm-3, due to the presence of the low density antimony and oxide ions. This RM, used as a packing material in a small fission bomb, can only serve one purpose; to cause a fixed mass of plutonium to pass from the sub-critical mass condition to the super-critical one. As this can only be achieved rapidly by a sudden increase in the neutron cross-section of the neutron shield, the density of the RM must increase to that of mercury, as it is the mercury nuclei next to the bomb’s plutonium core that provide the neutron reflection characteristic of the super-critical mass condition. The illustration of a fission device featured on p. 292 of ‘The Mini-Nuke Conspiracy’ indicates capsules of Red Mercury embedded in high explosive surrounding a spherical plutonium shell containing the plutonium core, the container for the high explosive having detonators embedded in its surface. To quote from the accompanying note: ‘When the explosive is detonated, the red mercury is injected into a gap around the plutonium. It acts as a neutron reflector, increasing the efficiency of the nuclear fission process, and as a tamper, preventing the plutonium from disintegrating too quickly. Neutron rich elements known as actinides (e.g. Californium 252) in the red mercury also give a boost to the fission process, increasing the yield of the bomb for a given quantity of plutonium.’ The gap in the plutonium container appears to be created by firing a ‘neutron gun’ situated inside the warhead casing. Thus a small nuclear warhead containing one core can simulate the explosive power of a large one containing a core comprising two sections. This is not so unusual. The first Abomb ever made was a single core implosion device, maximising the impact of the bomb’s warhead, with its core of scarce plutonium. 42 9. The muon as an agent for atomic fission. When beginning any consideration of the problems facing alchemists who opted for the conversion of mercury into gold (lead to gold represents an even less likely transmutation) it is natural to consider the release of neutrons due to naturally occurring processes. 1.7% of water, H2O, is heavy water, D2O, in which the mono-hydrogen isotope, 11H, is replaced by deuterium, 2 1H, also denoted D, with a nucleus comprising one proton and one neutron. Two of these nuclei, called deuterons, individual symbol d, d-d representing a pair, can fuse naturally to produce a helium nucleus and a neutron, a rare event, represented symbolically as: 1) d + d → 32He + n Bombardment with a slow-moving neutron can be a sufficiently destabilising condition to cause a mercury 200 nucleus to split, or undergo fission, producing a gold 198 nucleus and a tritium nucleus. Gold 198 is atomically unstable (radioactive) and decays to give stable gold 197, losing a neutron in the process: 2) 20080Hg + n → 19879Au* + 31H 3) 19879Au* → 19779Au + n This last condition is important for the development of a chain fission reaction as the neutrons produced replace those lost in creating the initiating reactions, continuing the process until all the mercury 200 has been converted to gold 197. Ambient electrons are always available to convert nuclei into atoms. It is always important to consider the quantities involved, in particular, the maximum possible rate at which the neutrons would be produced. 5 Litres of water could be boiled down, carefully and slowly, to leave 100ml of heavy water, the process being the result of the lower boiling point of water, H2O, with respect to heavy water, D2O. 100 ml D2O contains 3.0115 ×1024 pairs of deuterium atoms. The subject of cold fusion produced much speculation concerning the maximum deuteron fusion rate possible, with or without the intervention of some exotic mechanism. One of the two teams that reported finding evidence for it, in the form of unexpectedly high temperature rises and neutron fluxes in electrolytic cells, was that led by S.E. Jones and E.P. Palmer. They calculated the normal deuteron pair (d-d) fusion rate to be ~ 10-74 fusions per heavy water molecule per second, much too low to account for the reaction rate of R = ~ 10-23 fusions per second reported by their team. Critics A.J. Leggett and G. Baym produced a letter in which they calculated R = ~ 3 × 10-47 fusions per second to be an exact upper limit. Whether it is true that, as they asserted, ‘the necessary enhancement cannot be achieved without a totally incredible value’ for the deuteron pair random interaction rate is another matter. However, even with the unexpected enhancement, Jones, Palmer et als’ fusion/neutron production rate is only 0.27 × 10-20 n s-1 d-d-1. 43 It is interesting to consider the implications of the foregoing for alchemy. The 3.0115 × 1024 pairs of deuterium atoms (D2O) would generate neutrons at a maximum rate of about: 3.0115 × 1024 × 0.27 × 10 -20 = 0.8131 × 104n s-1 1 mole of mercury has a mass of ~200gm. Therefore 1gm of mercury represents: NA / 200 = 6.023 × 1023 / 200 = 3.0125 × 1021 mercury atoms Assuming bombardment with one thermal neutron apiece, slowed down by the heavy water to ~2.5 MeV is sufficient to destabilise all the atoms, causing them to undergo the fission reaction 2), the time taken to transmute 1 gm of mercury into 1 gm of gold is : T = 3.0125 × 1021 / 0.8131 X 104 seconds = 3.705 × 1017s = 1.029 × 1015hours T = 1.178 × 1011 years. Clearly, this is not a practical method for the transmutation of anything, whether by alchemists or anyone else. A more realistic approach would be to consider the interaction between a byproduct of the decomposition of the cosmic ray muon (μ-), the electron’s anti-neutrino (¯νe ) and a proton (p) in the mercury nucleus: 3) μ- → e- + ¯νe + νm, where νm represents the muon’s neutrino. 4) ¯νe + p → n + e+, where e+ represents a positron. 5) e- + e+ → γ + γ, where γ represents a photon. The interaction of the electron’s anti-neutrino with a proton in the nucleus of a mercury 198 (natural abundance = 10.00%) follows: 6) ¯νe + 19880Hg → 19879Au → 197 79Au + n The important aspect of this process is the production of the free neutron, the vital particle in the development of a fission chain reaction, once the neutron has been slowed down by energetic interactions with other mercury nuclei. However, if merely exposing mercury to a cosmic neutron source was a sufficient condition for cold fission then all the mercury obtainable would have disappeared into the process of gold production during the medieval period of reliance on heavenly forces for transmutation and much of that since extracted from Cinnabar. The theft of massive amounts of gold from the New World in the C16 would have reduced the incentive for this process but not for long, surely. Of course, mercuric pyroantimonate could act as a moderator, slowing the neutrons down to interactive velocities and reflecting them back into the mercury. It would not long remain a compound in the presence of mercury so I suspect its main purpose in this context would be to introduce the antimony atoms into the spaces between the mercury atoms, increasing the effective neutron cross section of the 44 latter in spite of the antimony nucleus’ low cross-section, simply due to the elimination of some of the gaps between nuclei. Again, it is important to consider the quantities involved in order to make sense of the proposition. Cosmic ray muons are only detectable because they are observed to survive for ~20 times as long as they would were they generated in a laboratory, when travelling to sea level from their origins in the upper atmosphere, due to their velocity with respect to ourselves, which approaches that of the speed of light. Time for the muons is, however, the same regardless, it is their observed average lifetime that varies with the variations in their motion. Their proper (i.e. own) lifetimes average 2.2 microsecs., their observed lifetime, 44 microsecs. Consequently, the incidence of cosmic muons at sea level, termed the muon flux (i.e. flow) is about 180 muons m -2s-1, passing vertically through everyone and everything unobstructed, whereas, without the time dilation factor, there would be none. Typically, the area of the mercury exposed, in a crucible, to these muons, would have been about 50 cm2 in the Renaissance so it would have been penetrated by ~9 muons every second, on average, not all of which would decompose to yield electron’s anti-neutrinos in the process. The cold fusion reactions reported by Pons and Fleischmann, as well as by Jones, Palmer et al, could not be accounted for by a neutron production rate of 0.27 × 10-20ns-1d-d-1 as calculated by Leggett and Baym. The process, which requires the presence of heavy water was interaction 1): 1) d + d → 32He + n However, the deuteron fusion probability was determined as if the deuterium atoms were isolated from all exterior influences, including cosmic muons. Muons facilitate fusion. A muon has the same charge as an electron but ~200 times the mass. It can replace the electron in a hydrogen atom, producing the exotic muonium atom. If the latter combines with another hydrogen atom it expels that atom’s electron to give the exotic, positively charged, ionic molecule, H2+, in which the protons are closer to each other than in the H2 molecule. Consider the impact of this process on two deuterium atoms, compressed within the ‘mossy’ surface of a negative palladium electrode. It would be the same with regards to the proximity of the nuclei of proton-neutron pairs, greatly increasing the probability of reaction 1) and thus the rate of neutron production, adjusting Leggett and Bayms’ calculations in such a way that cold fusion becomes a practical possibility. Nuclear fusion is a far more energy intensive process than nuclear fission so, by inference, the muon should suffice to produce the necessary neutron production rate to cause reaction 2) to occur at a detectable rate: 2) 20080Hg + n → 19879Au + 31He There is one remaining possibility for cold fusion that bears some relation to the Standard Model; the ‘many-body’ problem, as yet unsolved. Jones, Palmer et al used palladium negative electrodes and gold positive electrodes in their ‘jam-jar’ electrolytic cells, passing a DC current of 10 to 500mA between them and through the heavy water solution of volcanic type salts. 45 They reported that ‘Hydrogen bubbles (formed) on the palladium foils only after several minutes of electrolysis, suggesting the rapid absorption of deuterons into the foil; oxygen bubbles formed at the (gold) anode immediately.’ Both electrodes were usually of metal foil but sometimes the 0.025 mm thick palladium foils were each replaced by 5 gm of ‘mossy’ palladium, maximising the electrodes' surface area with respect to their volume. Noticing surges in heat and neutron production at this electrode the team concluded that helium (He) was being emitted there as well as hydrogen: - ‘a significant (neutron) signal appears above the background (neutron radiation) with the correct energy for d-d fusion neutrons (with energy ~2.5 MeV) (providing) strong evidence that room-temperature nuclear fusion is occurring at a low rate in the electrolytic catalysis cells.’ That rate had an estimated maximum of 0.27 ×10-20 fusions s-1, still far too low for the practical conversion of mercury into gold by neutron bombardment. The team’s explanation for their unexpectedly large numbers of observations of relatively high neutron counts was, basically, that trapping heavy water molecules between palladium atoms caused additional compression of those molecules relative to normal conditions at a gas liberating electrode, so bringing the paired deuterium atoms unusually close together and inducing fusion between their nuclei (i.e. the deuterons). Indeed, the team’s conclusion begins with the remark that a correspondence of ideas ‘regarding cold piezonuclear fusion with observations of excess 3He in metals and in geothermal areas of the Earth led to our experimental studies of fusion in electrochemical cells’. A situation in which an assembly of atoms can be arranged in such a way that they produce conditions radically different from straightforward conventional ones represents one aspect of the ‘many-body’ problem. The model of the electrolytic liberation of neutral atoms from ionic compounds in solution or, as considered here, the liberation of the gases contained in solution at the charged electrodes, may need to be replaced by a more complex one. Nuclear interactions may appear where only chemical ones are expected, the essential pre-condition for the existence of medieval cold fission. However, it is worth noting that Professors Leggett and Baym took account of this in a second analytical letter concerning Jones, Palmer et als’ reported observations, ‘Can solid-state effects enhance the cold-fusion rate?’ In particular, they commented that their upper bound value (i.e. maximum value) for neutron production (R = ~ 3 × 10-47 s-1) ‘makes no assumption whatever about the nature of any many-body mechanism involved’ because ‘the necessary enhancement cannot be achieved without ‘a quite incredible value’ for the sum of the heliumatom affinity and the zero-point energy of the alpha particle, namely, ~100 eV, and this would have other ‘easily observable consequences’. Regardless of these foregoing considerations, there is one that outweighs any ‘cold fission derived from cold fusion’ hypothesis. Alchemists had no conception of heavy water and no reports of transmutations emerging from their community included any mention of the use of water residues in the final ritual, although these frequently feature in ‘recipes’ for the production of the Philosopher's Stone. Maybe they utilised radioactive mercury, 20380Hg, natural abundance = 10.437% (or maybe not). 46 Like the muon, this undergoes β- decay: 7) 20380Hg → 20481Tl + e- + ¯νe , followed by reaction 6), above 6) ¯νe + 19880Hg → 19879Au (unstable) → 19779Au + n The problem with this approach to the question is that it would lead, at best, to equal quantities of gold and thallium atoms being produced or, much more likely, given the natural abundance of 19880Hg, 10.0%, to detectably large quantities of thallium as compared with negligible quantities of gold. As there is no record of an unidentified metal suddenly appearing during an attempted transmutation in chemistry’s prehistory it seems we can discount this possibility. More to the point, 20380Hg has a half-life of only 47 days, so even a natural abundance of 10.437% doesn’t indicate that a random sample of the element would contain a sufficient quantity of the isotope to produce reaction 7). The alchemists certainly could not acquire any radioactive isotopes that did not originate from natural sources so the procedure should be discounted as a realistic example of a transmutation. Realistically, the remaining candidates for a process that produces the apparent transmutation of mercury to gold using a compound containing mercury and antimony come down to one. This would be the extraction of gold from an imperfectly analysed gold amalgam, one that contains so much mercury that the gold content is unsuspected until extraction occurs. It is important to remember the role of mercury in the industrial process prior to the introduction of cyanidation in the C19 and the propensity for antimony to form gold antimonide, Au3Sb. Pliny (23 - 79 AD) recorded the use of mercury amalgamation in the extraction of gold from ore bearing rocks by the ancient Romans. Their mercury source then was, principally, the cinnabar found around Almaden in Spain, which has continued to be a source of mercury ever since. Consequently, unrefined mercury reused for various purposes over the centuries contains currently detectable quantities of gold. Given the proportion of mercury employed to gold produced as recorded by James Price in his 1782 proof of concept demonstration to an audience of dignitaries that included 4 members of the Royal Society, 30:1, the use of gold amalgam must be suspected. In a subsequent experiment the ratio was 4:1, indicating he must have known he was introducing as much gold into the process as he could without suspiciously colouring the amalgam. Analysis, using nitric acid to dissolve away the mercury followed by the application of tin chloride solution to the residue to find out if the Purple of Cassius (first recorded by Andreas Cassius in 1684) precipitated from the solution, would have caught Price out, but it appears that no such test was employed. The other ‘acid test’ is his inclusion of the supposed transmutation of mercury (atomic number 79) to silver (atomic number 47). No known fission process could account for this and the description of the changing condition of the mercury, from ‘bright and fluid’ to a thickened liquid that ‘poured grouty’, after ‘standing for about 45 minutes’, after heating, indicates that some type of extraction of silver from an amalgam was taking place. The Philosopher's Stone in this case was a white powder. Mercuric meta-antimonate is white. 47 How would a gold or silver amalgam be made to yield the precious metals in a matter of minutes? Principally by the action of a metal/metalloid that forms alloys/compounds readily with another metal if it is already in an ionised condition and the reactants are heated. Heating also tends to decompose an amalgam, a dangerous procedure as the rate of loss of mercury as vapour, which occurs slowly at room temperature anyway, rapidly increases with the increase in temperature. The crucial point concerning any experiment in which both the decomposition of the amalgam providing the metal for the compound followed by the formation of the compound occur together is that the sequence can only proceed in that given order; it is irreversible. Mercury atoms display a much greater affinity for other mercury atoms than they do for those of other metals and mercury cannot be induced to form ionic compounds with them unless it is first ionised to give acidic salts by the application of strong acid. Both mercuric meta-antimonate and mercuric pyro-antimonate are really intimate combinations of mercury and antimony oxides, existing as separate layers within the same crystalline structure. There are no electron bonds linking the antimony and mercury ions so the oxide layers are free to separate once they enter liquid mercury. Antimony forms compounds with both gold and silver and these are found as minerals. Aurostibnite, Au3Sb, is gold antimonide and Dyscrasite, Ag3Sb is silver antimonide, found in Canada and Australia, but rarely. Gold amalgam is also found in nature but is extremely rare. Typically, both antimony and mercury are found as their sulphides, Stibnite and Cinnabar, their naturally occurring oxides, such as the mineral Montroydite (mercuric oxide), being alteration products of the sulphides. Antimony, like mercury, is a volatile element at room temperature but much less so, and if you heat a combination of mercury and antimony salts in solution it is the mercury which is seen to be released first, as a precipitate. Antimony compounds forming in an amalgam would be unstable under the application of heat and the antimony ions released would react with more metal atoms/ions (but not the mercury) releasing them from the amalgam in a one way process that would only take a matter of minutes for the quantities quoted, 10 grains of gold for Dr. Price’s demonstration given before members of the Royal Society. As a reasonable hypothesis, I propose that mercuric meta- and pyro-antimonates could be added to silver and gold amalgams to replicate his demonstration. The mercury and antimony oxides separate in a gold amalgam. The oxides dissociate, the mercury ions associating with those in the mercurous gold, HgAu, found in such amalgams, causing decomposition of the latter, whilst the antimony ions form gold antimonide with the released gold ions. This is reduced to neutral gold and antimony atoms but the antimony forms more gold antimonide as more gold ions are released from the amalgam, until all the gold has been precipitated out of the mercury, the oxide ions combining to form, and be released, as oxygen gas, O2. I therefore propose that Dr. Price used a combination of mercuric meta- and pyroantimonates as his ‘transmuting agents’, precious metals concealed in amalgams by means of excessive quantities of mercury and fraud. His subsequent suicide, due to stress occasioned by the Royal Society’s insistence that he repeat his experiments as demonstrations, using larger quantities and his friends insisting he conform to expectations, in spite of his excuse that his ‘supply of (transmuting) powders (was) used up’, was carried out in front of those he considered to have driven him to it. 48 10. Observations of transmutations in ancient China; the ‘Out of China’ Theory of alchemy’s origin ‘When the chhi of the southern regions (lit. the 'bull-lands') ascends to the Red Heavens, they give birth after 700 years to chhi tan (red cinnabar). This in turn produces after 700 years red mercury, red mercury after 700 years produces red metal (copper), and red metal in 1,000 years gives birth to a red dragon. The red dragon, penetrating to the treasuries (of the earth) gives rise to the Red Springs. When the dust from the Red Springs ascends and becomes red clouds, the Yin and Yang beat upon one another, produce peals of thunder, and fly out as lightning. The (waters) which were above thereupon descend (as rain) and the running streams flow downwards uniting in the Red Sea.' From the fourth chapter of the 'Huai Nan Tzu' (2nd. Century BC) Eric Holmyard, introducing the third chapter of his classic treatise on the subject, 'Alchemy' (1949), wrote of Chinese alchemy that, previously, 'the available data gave little information about the paths of development it had followed. At the present time, however, largely owing to the work of O.S. Johnson, T.L. Davis, L.C. Wu, K.F. Chen, and particularly H.H. Dubs, the facts are beginning to emerge - and very interesting facts they are.' The massive task of analysing and arranging the translations of Chinese writings on alchemy fell to Joseph Needham, representing just a small part of his massive oeuvre 'Science and Civilisation in China', published, in 42 parts, in 1970. In the process he completely rewrote the history of Western alchemy, which had been thought to derive and date from Aristotle's theory of the four elements of the 1st Century BC. The proportions of Earth, Air, Water and Fire contained by base metals existing in minerals within the earth was supposed to modify over hundreds of years as the metals 'grew', developing a 'more perfect' form as silver or gold. Aristotelians used the growth of plants from bulbs and roots in the earth as an analogy. However, Needham found that 'The Chinese theory of the metamorphosis of minerals is … fully developed by 122 BC, and probably goes back to 350 BC or before. It is extremely difficult to believe that Tsou Yen and his School (of Naturalists) derived it from Aristotle or the pre-Socratics.'1 With reference to the two metals central to this book it should be noted that whilst antimony was not referred to in its elemental form in a Chinese document until 1584, only 16 years before the publication of Basil Valentine's 'Triumphal Chariot of Antimony' in Germany, references to mercury go back to antiquity in China, as in the West. Cinnabar was of particular interest to the Chinese, already being associated with gold prospecting by the 4th Century AD. A book of that period, the Kuan Tzu, mentioned that superficial Cinnabar was considered a sign of deeper gold. The theory behind this reasoning was given by that most celebrated of all Chinese alchemists, Ko Hung, who wrote, in about 300 AD,: 1 Vol. 3, Section 25, p.641. 49 'When the manuals of the immortals (hsien ching) say that the seminal essence of cinnabar gives birth to gold, this is the theory of making gold from cinnabar. That is why gold is generally found beneath cinnabar in the mountains.'2 It is worth noting at this point that Greek and Arabic documents referring to Western alchemical writings of c. 100 BC to 100 AD did not themselves appear until the 8th and 9th Centuries AD together with the notion of the Philosopher's Stone as a red powder. Writing in his 'Clerks and Craftsmen in China and the West', Needham states that 'by 20 AD the idea of the 'philosopher's stone' makes its appearance for the first time in a story of Huan Than's transmitted to the Arabic world by about 700 AD, Chinese lien tan shu set the definitive alchemical style which lasted in European culture from c.1200 AD till the time of Boyle, Newton and Lavoisier .Thus Chinese alchemy long antedates Arabic alchemy and even Hellenistic 'alchemy'.' Where did the word come from anyway? When C19 British writers and ethnographers came to consider the matter they postulated that its most likely derivation was 'al khem', 'khem' meaning 'earth' in Egyptian but not, they reasoned, just any old earth. No, it must refer to the rich alluvial mud of the Nile delta, early Egyptian chemists having supposedly learned how to extract gold from it by means of 'alchemy'. Alternatively, it could refer to the name of Egypt, Khemt. The superficial plausibility of this ad hoc argument is challenged as soon as one considers the original spelling of the word 'chemistry' (describing the 'art of chem'). It was spelt 'chimistry' from the time of alchemy's introduction to this country in 1100AD until Boyle's 'Sceptical Chymist' appeared, in 1667, wherefore it would more precisely be said to represent the 'art of chim' and this focuses one's attention on the actual pronunciation of 'alchemy'. In 'Clerks and Craftsmen in China and the West' Needham proceeds as follows: - 'The origin of the word 'alchemy' has been much disputed. I suggest that the word is really Chinese in origin and comes from the words lien chin shu, the art of transmuting gold. This would be pronounced in Cantonese lien kim shok. Now it is known that Arabic people and Syrians were trading with China as early as 200 AD so that Arabs would naturally put the prefix al on to it, and get al kimm [actually al-kimiya] 'pertaining to the making of gold'.' It is not simply a matter, therefore, of considering which noun serves as the most likely origin for the term describing transmutation to noble metals, 'earth' or Egypt or 'gold'. In order to refute Needham's suggestion it would be necessary to show that the ancient Chinese had taken a foreign word, taken off its prefix, always assuming they knew it had one, spelt it using a phoneticised version of a non-existent Cantonese word and then applied it to a process that they had been engaged in hundreds of years before any Egyptian began to take an interest in it. Furthermore, the word just happened to correspond with their word for gold. It is the sheer implausibility of these circumstances that seems to give both alchemy and, by extension, chemistry itself, a specifically Chinese origin. 2 From Section 33. 50 As it is with the basic concepts, so it appears to be with matters related to the experimental research involved. The 'Huai Nan Tzu' (C2 BC), from which the introductory quotation was drawn, 'mentions many of the inorganic substances which later became so important in alchemy - arsenic sulphide, sulphur, arsenious acid, mercuric sulphide, mercury and the metals (of antiquity)'. It also deals with what it refers to as yellow, green, red, white and black mercury, indicating how metallic elements could be confused with their compounds, a practice that became all too common in the West, but only a major influence in Western alchemical literature hundreds of years after the writing of the 'Huai Nan Tzu'. What was the impetus towards gold production that caused alchemy to become increasingly popular in China up to the time of its prohibition by imperial edict in 144 BC? Needham relates how Chhen Chih (1955) (argued) that gold became increasingly scarce in the course of the Han (a dynasty lasting from 202 BC to 220 AD) and later, attributing this growing scarcity to the gradual exhaustion of many of the most easily worked deposits as well as a siphoning off of much gold into the gilding of Buddhist statuary.3 Certainly, gold substitutes were well known by that time. By the Warring States (Chan Kuo) period (480 to 221 BC), liquid or pasty mercury-gold amalgams were widely used for gold-plating metal objects (liu chin); after the amalgam was applied, the object would be heated, driving off the mercury and leaving the gilding.4 The extraction of gold using mercury was already practised, also the use of antimony in a cupellation process designed to separate gold from silver 'by the use of stibnite (naturally occurring antimony sulphide); here the melt (in the cupel) forms two layers, the upper one containing the sulphides of silver and any other base metals present Below there is gold with metallic antimony, and the latter is driven off by further heating afterwards.'5 Eric Holmyard quotes a commentator on the imperial edict of 144 BC, who provides the background to the prohibition. 'The Emperor Wen had allowed such practises, and much alchemistic gold had been made; however, alchemistic gold is not really gold, and the alchemists thus lose their time and money and are left with nothing more than empty boasts. When they become poor through wasting their substance on their experiments, they turn to brigandry or robbery, and hence the Emperor Jing (Ching) issued his edict against them.' Specifically, the edict 'enacted that coiners and those who made counterfeit gold should be punished by public execution.'6 Bearing in mind that Ching was a ruthless bloody tyrant, this still seems a little harsh and gives an idea of the seriousness of the situation. Comparison with the approximate date (300 AD) of the Emperor Diocletian's edict against alchemy, in which it is again treated as a way of counterfeiting gold, serves to illustrate the enormous lead that China had on the West in this field. 3 Science & Civilisation in China (SCC) Vol. 13, p.123. 4 Ibid p.146, from Lins & Oddy (1975): - The Origins of Mercury Gilding. 5 Vol. 5, Section 33, p.39. 6 Alchemy, Chapter 3, p31. 51 Also, Holmyard relates how, in 133 BC 'an alchemist was received by the Emperor Wu because he claimed that he had discovered the secret of immortality .The alchemist said that the Emperor must first worship the goddess of the stove in his own person; this would enable him to invoke spiritual beings who, when they appeared, would render possible the conversion of cinnabar into gold;...'7 Apparently alchemy was thought worthy of consideration by the most elevated of individuals and the notion that all of its procedures were fraudulent was just for public consumption. The number of gold substitutes continued to proliferate. Joseph Needham provides a list of different 'types' of gold and silver, contained in the 'Thang Liu Tien' (Administrative Regulations of the Six Ministries of the Thang Dynasty), completed in 739 AD, making no distinction between the real and the false. It lists chhuang chin as 'made' or 'created' gold, interpreted to mean artificial or alchemical gold.8 The 'Pao Tsang Lun' (Discourse on the Contents of the Precious Treasury of the Earth) of 918 AD lists 15 artificial kinds of gold and 5 genuine, all under the heading of chin hsiao (gold powder). Number 15 is chu sha chin or Cinnabar 'gold', interpreted by Needham as either a form of gilding or copper 'whitened with mercury then yellowed by sulphides.' Needham expatiates at some length on the subject of cupellation and cementation, rightly drawing attention to the 'antiquity and universality of the testing and assay methods for the precious metals.'9 He then asks a question of fundamental importance to my entire hypothesis. 'How then, in such a situation, could 'alchemy' -aurifaction- ever have arisen? How could goldsmithery ever have turned into 'alchemy'?'10 To state it differently, how did the notion of aurifaction ever originate if a) nobody had ever achieved it and b) there was no reason to believe anyone would ever achieve it? No amount of theorising concerning the acceleration of a natural process could establish a practice when the only possible evidence of success was of an obvious, practical nature. Due to the (necessarily) well developed art of assaying, any fraud ran the risk of instant detection. Needham quotes the pioneering scientific archaeologist Berthelot, who concluded that 'In ancient times, the precise analytical means of today were not known. Hence it was a step to the idea that it was possible to make the imitation so perfect that it would be identical with the reality. This was the step that the alchemists took.' However, Berthelot then rationalised the continuation of the confusion that this process involved by supposing that 'the artisans for whom these (fraudulent) recipes were written probably became real alchemists later'. Needham comments, almost superfluously, that 'this is what we might call 'the theory of the dupers duped' and it is really impossible to believe.' 7 Ibid, p32. 8 SCC, Vol. 5, Section 33, p274. 9 SCC, Vol. 5, Section 33, p41. 10 Ibid, p44. 52 Let us now turn to the subject of Cinnabar, regarded by Chinese alchemists as central to their craft and, like Stibnite, a natural resource common to many parts of China. Needham mentions the famous rich deposits of Cinnabar at Chhen-chou in Hunan.11Concerning Cinnabar as a source of 'yellow silver' (huang yin) he writes: - 'Now Thang Shen-Wei in the Cheng Lei Pen Tshao (Classified Pharmaceutical Natural History, 1249 AD edition) quotes (Chhing) Hsia Tzu (either the author of the Pao Tsang Lun or an earlier alchemical writer) as saying that 'when cinnabar is subdued by fire it turns into huang yin; this can be heavy or it can be light, with spiritual or with magic powers'.' A Thang dynasty writer had listed 'yellow silver' with 'cinnabar silver' (tan sha yin), 'realgar silver' (hsiung huang yin) and 'orpiment silver' (tzhua huang yin).12 'Fang Shao, in his Po Choi Pien (written in 1117 AD), says: 'Huang yin comes from Szechuan, and few Southerners know about it. The courtier of the former dynasty (i.e. the Thang) Yen Ching-Chin once found himself in charge of the Treasury and noted that there were ten hairpins (of huang yin). These were made of some metal with a colour and weight no different from that of the finest gold'.' However, Needham then goes on to state that 'There can be no question that this 'yellow silver' refers to the whitening or silvering of surface-layers of copper and dark copper-containing alloys, by mercury and mercury vapour (so as to form a superficial amalgam), and by the formation of silvery or golden-looking surface films containing arsenic and sulphur '13 He then adds that 'Chhing Hsia Tzu goes on to say: - 'It (the huang yin) can be dark or light, and it can be dull or shining. A man can hardly lift a hu bushel of it [~79 lbs] but if ten thousand catties [~10,000 lbs] of it are subjected to the furnace it all soars aloft in a trice (as vapour) and even if the gods and spirits were to set out to seek for it they could not tell where it had gone'.' Needham then expresses the opinion that it must have comprised volatile metals and oxides.14 Quite apart from the contradiction between this and his previous analysis, it is at variance with Dr. Sleight's and my own experiences with double oxides of mercury. The late Roman Empire developed a huge trade deficit with the Seres, large enough to account for its fall, but there was one popular trade item that the Romans had access to that no Chinese had, coloured glass. Originating in Sumeria, it was produced by adding powdered metals to molten soda glass and annealing. Needham observes that gold-ruby glass was glass fused (and annealed) with the 'Purple of Cassius', colloidal gold adsorbed onto colloidal stannic oxide. He mentions that: 'W. Ganzenmuller [in his 'Zukunftsaufgaben der Geschichte der Alchimie', 1953] has drawn attention to the fact that there is a strangely close connection between the gold-ruby glass and the 'philosophers' stone' of medieval Europe. He shows how often this was referred to as dark red in colour, 'glowing like the carbuncle or the ruby', and he suggests that the discovery of the colouring properties of colloidal gold had a very long hidden history '15 11 SCC, Vol. 13, p139. 12SCC, Vol. 5, p205. 13 Ibid, p206.14 Ibid, p207. 15 Ibid, p268. 53 My own researches have shown me that stable combinations of mercuric and antimonic oxides always colour glass red, excepting in the case of mercuric meta-antimonate, which colours it silvery white. In the circumstances I cannot imagine that Chinese alchemists would not have noticed this property of their mixed oxides (or possibly sulphides) of mercury and antimony had they developed the practice of colouring glass. As they were importing coloured glass from an empire that was depleting its gold reserves in order to pay for all the goods it was importing from them there was simply no incentive for them to develop the technique. If anything can be said to represent the parting of the ways between Chinese and Western alchemy, it is this. 54 APPENDIX A. Atoms and fundamental particles. The smallest entities comprising any elementally defined substance are termed atoms, from the Greek 'atomos', meaning 'indivisible'. This they are clearly not, even in the case of chemical reactions, which are electrical processes involving easily accessible energy levels, because the electrons, the negative electrical particles that surround atoms central features and represent electric current, form or break the bonds that link atoms to other atoms. Chemical elements represent substances that cannot be compounded out of other substances. Atoms are divisible in a way that turns them into different atoms but only if the heart of the atom, the nucleus, is divided. This represents a less familiar situation, even though many atoms do it spontaneously. The result may be a different version of an element, termed an isotope, or a different element. The latter case is described as transmutation. Deliberate, artificial, conversion of one element into another is an energy intensive process where any appreciable amounts of the elements are involved, a problem for traditional alchemy. The fundamental constituents of atoms are just three types of particle, analogous to the arabic Tria Prima of traditional alchemy; sulphur, salt and mercury. They are the proton, the positively charged fundamental particle, the neutron, or neutral one, which, like a salt, can divide into oppositely charged constituents, and the negatively charged electron. The neutron can decay outside the nucleus, or be caused to decay within it, into the positive and negative principles, the proton and the electron. The charges are responsible for all chemical interactions. The proton, which is ~10-10 m, a femtometre or Fermi, in diameter and 1.6725 × 10-27 kg in mass and the neutron, of similar size and slightly greater mass, are confined to the atomic nucleus. The electron, of negligible size and with 1/1836 the mass of the proton (9.109 × 10-31 kg), orbits the nucleus. The diameter of the orbit of the electron, for the element hydrogen, defines the diameter of the atom, ~10-10 m, or one Ångström. Each element is defined by the numbers of protons in its atomic nucleus. The numbers of electrons must always match the number of protons in each atom and the electrons occupy different orbits around their nuclei, two electrons per orbit. The atoms of different elements have diameters defined by the orbital diameter of their outermost electrons. The 92 naturally occurring elements have atoms with 1 to 94 protons in their nuclei (the element technetium, having 43 protons per atom, is purely artificial, whilst all the naturally occurring neptunium, having 93, has decayed to form other elements). These units of positive charge are therefore surrounded by from 1 to 94 electrons on a one for one basis, producing neutral, uncharged atoms. The outer orbit for the largest atom, uranium, with 92 electrons, has a diameter of 3 × 10-10m/ 3 Ångströms. The principal events leading to the discovery of the atom and an understanding of its nature can be summarised as follows:1896 Henri Bequerel identifies 3 types of radiation coming from the element radium; alpha and beta, found to be oppositely charged, and gamma, which comprised photons, i.e. particles of light. 1897 J.J. Thomson finds that beta radiation consists of negatively charged particles and calls them 'electrons'. 55 1909 Professor E. Rutherford finds that the alpha particle has twice the charge of a hydrogen ion (H+). 1911 Prof. Rutherford and team establish the existence of the atomic nucleus. 1912 Prof. Rutherford identifies the alpha particle with the helium 4 ion (He++), the helium nucleus. 1919 Prof. Rutherford bombards nitrogen 14 (147N) with alpha particles, converting a bit of the gas to oxygen 16 (168O) and ejecting protons, one from each nitrogen nucleus converted. This became the first accredited case of artificial transmutation. It was also the first instance of cold nuclear fusion. 1932 J. Chadwick discovers the neutron. Postulates the existence of the positron. 1933 The existence of artificial radioactivity is confirmed by I. and F. Joliot-Curie. 1934 F. Joliot-Curie and Gibaud demonstrate the mutual annihilation of the electron and positron. 1939 L. Meitner, O. Hahn, F. Strasner and R. Frisch confirm the existence of nuclear fission. On learning of this, Einstein writes to F.D. Roosevelt urging the development a 'uranium bomb' by the U.S., to preclude the Germans' doing it first. 1943 Roosevelt finally authorises the Manhattan Project, leading to the production of a nuclear fission reactor and the world's first atomic bomb. As the U.S. had entered the Second World War by then, military, geographical and racist considerations led to the bomb being used against Japan rather than Germany. We are still living with the consequences of that decision. Broadly speaking, there are only 3 categories of fundamental particle, matter particles of 2 kinds and the force-carrying particles. The matter particles are termed Fermions and comprise those that experience the strong nuclear force and other strong interactions, termed Hadrons and those that do not, termed Leptons. The force carrying particles are called Bosons. The Hadrons are subdivided into Baryons and Mesons. The Baryons include the nuclides, i.e. the Proton and Neutron, and are all made up of 3 Quarks per particle, the Quarks being the most fundamental of the matter particles. These are unable to exist singly and are bound together by Gluons, Bosons that carry the strong nuclear force. The Leptons include the Electron. Along with the matter particles that make up our universe, particle experiments also bring into existence anti-particles, belonging to the anti-universe. The first of these to be discovered was the Positron, in 1932, and antiparticles have been pretty well accounted for and researched up to the present time. The Mesons are extremely short-lived Hadrons, each comprising a Quark and Anti-quark. Most Baryons also have extremely short lives too, 2.90 × 10-10 to 7 X 10-23 seconds. 56 Although the sub-atomic particles rarely interact with the atomic ones outside of particle accelerators there are a few notable exceptions. Photons constantly interact with Electrons, representing electromagnetic quanta, whilst Gluons represent the strong nuclear force that keeps the quarks in the nucleons together. In order to interact with nucleons, matter particles (Leptons and Hadrons) need to live long enough and have a mass of high enough value (~100 Mega-electron volts (MeV)/c2) relative to that of the nucleons (mass = ~939 MeV/ c2). Only 7 particles qualify, 2 Leptons, namely, the negatively and positively charged Muons, μ- and μ+, and 5 Hadrons, the Mesons π- and π+ (charged Pions), the 2 charged Kaons, K+/- and the uncharged Kaon, KL0). The Muons are the best candidates, with an average lifetime of 2.197 × 10-6sec, making them the longest lived Hadrons apart from the nucleons, and a mass of 105.659 MeV/c2. The Pions have an average lifetime of 2.60 × 10-8sec and a mass of 139.569 MeV/c2. They decay to produce Muons. The charged Kaons have a lifetime of 1.24 × 10-8sec and a mass of 493.67 MeV/c2 and the uncharged a lifetime of 5.18 × -8 2 10 sec and a mass of 497.72 MeV/c . They decay to produce Muons and Pions. As a result of these initial conditions the Muons are the most plentiful free Fermions at any given time and therefore those most likely to interact with atomic nuclei. This they do via the weak nuclear force. Muons originate, in nature, from the decay of Pions of cosmic origin in the Earth's upper atmosphere. N.B. As this is only intended as an introduction to the subject I have capitalised the first letter of each particle name, for clarity. They would not ordinarily be so. 57 APPENDIX B The conventional representation of chemical reactions. Chemical nomenclature and symbols. In principal, chemical elements are represented symbolically according to a simple rule. The most abundant elements are represented by the initial letter of their name, provided they were discovered before others with the same initial letter, as will usually be the case. The others are denoted by the first two letters of their names, where the initials alone have already been claimed by other elements. Although this maximises the efficiency with which scientific accounts of experimental results can be recorded and the Periodic Table requires no more than two letters per element for all the naturally occurring elements, there are several exceptions to the rule. The metallic elements of alchemy, having been known from antiquity, were symbolised by images denoting their ruling planet and by the initial letters of their Latin names plus one other, Latin becoming the scientific language of Europe, after the original, Greek, had been displaced. Hydrogen and hydrargyrum (mercury) are symbolised by H and Hg respectively. No element is indicated by the letters 'Hy'. Antimony wasn't discovered until 1664 but its symbol is Sb, for stibium, the Latin name for Stibnite, antimony sulphide. Phosphorus was discovered ~1670 but is represented by the letter P, even though potassium was known, in compound form, from antiquity, as potash (impure potassium carbonate) or kalium, giving it the symbol K. Similarly, natrum, sodium carbonate, also known from antiquity, gives sodium the symbol Na, even though potassium and sodium were not isolated as elements, by electrolysis, until 1807. Consequently, the letter S is reserved for sulphur, known in its elemental form since antiquity, which retains its Latin name. Boron was not isolated until it could be obtained by heating boron trioxide with elemental potassium or sodium. However, it is denoted B whilst metallic bismuth, identified under the name bisemutum in 1530, is symbolised by Bi. Nickel, whose name derives from the C16 German mining term 'kupfer-nickel' (false copper) was recorded as such in 1694, but the name nitrogen was only given to 'foul air' in 1790, yet the latter has the symbol N whilst nickel is Ni. However, nitrogen is much more abundant and, along with the other principal gases of air was identified at the beginning of modern chemistry so maybe that should give it, and them, a certain primacy. Many single letters remain unused. Although eight elements have names beginning with an A that letter is not used to represent any element. Only one element's name begins with an X but Xenon is indicated by Xe. Much latinisation of place and personal names took place when honouring discovery locations or famous discoverers related to certain elements, or even science in general (cf 'Einsteinium'and 'Fermium'). The use of symbols for recording chemical reactions A chemical element’s symbol represents: (1) The name of the element. (2) One atom of the element. (3) One mole of the element. This is a standard quantity of atoms, called Avogadro's number, NA = 6.023 × 1023. It is also used to refer to a mole of molecules. 58 (4) The quantity of the element equal in weight to its atomic weight. The latter is therefore the weight of Avogadro's number of atoms of that element. Compounds, representing as they do combinations of elements, are indicated by combinations of their symbols. Each of these represents: (1) The name of the compound. (2) One molecule of the compound. (Strictly speaking this is only the case for covalently bonded atoms but the term is also used for ionically bonded, i.e. non-molecular, ones as well). (3) One mole of that compound's molecules. (4) The quantity of the compound equal to its formula weight. This is therefore the weight of Avogadro's number of molecules of the compound. The term molecular weight is used interchangeably with formula weight. Chemical reactions expressed as equations. The elements and compounds engaged in chemical reactions are recorded using their symbols and a connecting →, =>, <=> or just =. The arrows indicate the direction of the process, which may be reversible (<=>). The term equation is used to describe it because the number of atoms engaged in the process remain the same after the reaction as before it, as do the masses involved, represented by atomic or formula weights. Therefore, in a reaction involving the oxidation of copper to copper oxide: 2Cu + O2 → 2CuO, the equation takes account of the fact that oxygen gas consists of pairs of atoms. The doubling of the number of copper atoms and copper oxide molecules balances the equation, ensuring they remain the same in the experimental record, as they do in reality. The oxygen gas consists of molecules, sharing the electrons of their atoms' outer shells in covalently bonded atomic pairs but the copper oxide is ionically bonded, the copper atoms yielding outer electrons to the oxygen atoms, producing oxide ions. Take the example of the combination of mercuric oxide and pyro-antimonic acid to form mercuric pyro-antimonate and water: 2HgO + H4Sb2O7 → Hg2Sb2O7 + 2H2O In formula/molar weights, this would be represented as: 2(201 + 16) + (4 + 2 × 122 + 7 × 16) → (2 × 201 + 2 × 122 + 7 × 16) + 2(2 + 16), in grams, to the nearest gram. 434 + (248 + 112) = (646 + 112) + 2(18) 794 = 758 + 36 59 Therefore, whatever the actual masses involved in the experiment, the ratio of the total mass of oxide and acid, termed the reactants, going into the reaction, to the mass of the solid pyro-antimonate, called the reaction's solid product, is 794:758. Understandably, there is usually a small surplus of one reactant or the other. This simply remains outside the reaction process. Compounds are held together by the same electromagnetic force that holds atomic nuclei and electrons together. Breaking and forming the electron bonds that keeps atoms combined in compounds is an energetic process but does not represent a measurable interchange of mass and energy, which is why the total masses in chemical reactions remain the same. This is in accordance with the Principle of the Conservation of Mass. In nuclear reactions the gluons are the bonding particles, the bosons that carry the strong nuclear force to maintain the combinations of quarks that make up the nucleons, as well as keeping the nuclides together. Breaking these releases a huge amount of energy relative to the mass lost but there is a measurable loss of mass with the loss of nucleons from atomic nuclei. Thus, the transmutation of one element into another involves a re-distribution of mass-energy, as it is termed, so a nuclear reaction equation is not one in which the masses before and after the reaction are expected to balance out. It is the mass-energy that remains constant, in keeping with the Conservation of Energy Principle. 60 APPENDIX C The Periodic Table and the proximity of alchemy's 'metallic elements'. Chemical elements lying close to one another in the Periodic Table tend to have more in common, in terms of their relative atomic masses*, densities and atomic radii, than those far apart. As might be expected, this situation is closely related to their atomic numbers (Z), representing as these do the numbers of protons in the atomic nucleus, these being equalled or exceeded by the numbers of neutrons accompanying them, other than for hydrogen 1 (Z = 1, A = 1) and helium 3 (Z = 2, A = 3). The atomic number also indicates precisely the number of electrons orbiting each nucleus, two per orbit, and the more of these there are the more groups of orbits, called shells, there will be. This clearly increases the overall atomic radius. However the decisive factor, once these trends are taken account of, is the chemical grouping of the elements and this is solely determined by the number of electrons per atom that will engage in chemical processes. The solid element with the lowest atomic number, lithium (Z = 3, so it may also simply be referred to as 'element 3') has a relative atomic mass of 6.941, a density of 0.53 gm cm-3 and an atomic radius of 152 picometres (pm), i.e.152 × 10-12m. It belongs to Group IA (Chemical Abstract Service notation is used throughout). This means that it will yield one outer electron per atom to bond with another atom that will receive the electron into its outer orbit. The naturally occurring non-radioactive element with the highest atomic number, bismuth (Z = 83) has a relative atomic mass of 208.98037 and a density of 9.80 gm cm-3 but an atomic radius of only 154.5 pm. It belongs to Group VA. The element with the highest atomic radius, 265.5 pm, is caesium (Z = 55) and, like lithium, it belongs to Group IA. The densest elements are transitional metals, transitional because their groups contain elements whose atoms lose or, occasionally, even gain, indeterminate numbers of outer electrons as chemical reactants. Manganese (Z = 25) can lose 2,3,4,6 or 7 electrons or gain 1 during a chemical process. The densest element is iridium (Z = 77), at 22.65 gm cm-3. The density of an element in its solid state isn't all down to its relative atomic mass but also, as might be expected, to the arrangement of its atoms in a solid structure. Those with the most closely packed atoms for a given relative atomic mass will be the densest. Elements/compounds in liquid form are usually of lower density than when solidified (water being a notable exception). The transitional metal mercury (Z = 80), being liquid at room temperature (nominally 20 degrees C/ 293 Kelvins), has a lower density, 13.55 gm cm3 , than transitional elements 73 to 79. However, elements 81, 82, and 83, tantalum, lead and bismuth respectively, which belong to the non-transitional groups IIIA, IVA and VA, all have lower densities than mercury. The interactions of the metals of alchemy, elements 26, iron, 29, copper, 47, silver, 50, tin, 79, gold, 80, mercury and 82, lead, illustrate well the effects of atomic similarities and temperature related changes of state for different elements. Lead and silver have similar densities at room temperature, 11.34 gm cm-3 and 10.49 gm cm-3, indicating similarities in their atomic packing within their solid structures that outweigh the differences in their atomic weights, 107.8682 and 207.2. *Also termed 'atomic weight'. The average of the atomic mass numbers (protons + neutrons) for the element's different isotopes, weighted for their relative abundances. 61 This means that a molten mixture of the two is likely to cool to form an intimate combination of the metals, an alloy, because an atom of lead can readily substitute for an atom of silver and vice versa. Therefore, lead could be used to extract silver from its ore and, having a relatively low melting point, 327.5 K, would prove more convenient than the alternatives, as indeed it did. Silver and lead ores were melted ('fused') together and the resulting alloy subjected to cupellation. This means that it was fused in a flat dish called a cupel or test, formed of bone-ash, clay and limestone or barytes (barium sulphate) or cement. When air was blown over the metal the lead oxidised to lead monoxide, PbO, which was driven off as a vapour or absorbed by the cupel. Having a higher melting point (961.9 K) than lead, silver was left behind as a solid. The method was in use by the ancient Romans, as recorded by Pliny (23-79 AD). Mercury, being liquid at room temperature and only definitely established to be a metal when observed frozen to a malleable solid by Braune in 1759, is able to dissolve other metals, forming alloys called amalgams. The only alchemical metal it will not dissolve is iron. Silver amalgam is formed when mercury is poured into a solution of silver nitrate. Silver itself could be extracted from finely crushed silver ore by adding mercury, together with copper and iron sulphates in roasted pyrites, the resulting mixture being trodden, by mules, on a muddy brine covered patio for from 15 to 45 days. Silver chloride formed and the mercury then removed the chloride to form mercuric chloride, leaving the silver: AgCl + Hg → Ag + HgCl Excess mercury would then amalgamate with the silver (like the amalgam formed with the silver ions in the silver nitrate), being pressed out again in canvas bags. This process was invented by Bartolomeo de Medina, in 1557. Both mercury and lead used to feature in the extraction of gold from auriferous gravel. After crushing with water jets and batteries of stamping mills, mercury would amalgamate with the gold in the resulting slime and the amalgam would be collected on the surfaces of copper plates. This was then scraped off the plates and the mercury distilled off by heating the amalgam in iron retorts. Alternatively, potassium cyanide solution could be added to the crushed ore and the precipitate of potassium aurocyanide melted with lead to form a gold alloy. The alloy would then be cupelled to remove the potassium lead cyanide, as in the case of the silver-lead alloy. A downside to the processes was that both the mercury and lead commonly available would increasingly derive from that used in the silver and gold extraction industries. As the principle alchemical objective was to transmute mercury, though sometimes iron or copper, into silver and mercury and/lead into gold, it was a bad idea to start with samples that might already contain traces of the precious metals which were the target products of the experiments, not that, in the absence of mass spectrometers or even strong acids (for most of the alchemical period), they were able to check the samples out. This meant that positive results were always subject to challenge on the basis of sample contamination. 62 Fortunately, neither the alchemists nor their increasingly vocal critics were aware of the energy required to artificially generate neutron induced fission or the former would have been too depressed to pursue their researches. Gold is only slightly soluble in mercury, reducing the likelihood of a false positive for aurification. It would, however, have been as well if the challenge facing anyone trying to convert element 80 (mercury) to element 47 (silver) could have been understood, but the very existence of atoms wasn't fully recognised until ~1900. The ease with which lead permeates gold is indicated by the fact that 1 part lead in 1,000 parts gold is sufficient to render the latter brittle. In this case the proximity of the two elements in the Periodic Table is still significant, but the relative softness and malleability of both metals represent decisive factors in their combination. Gold is the most ductile of metals and lead, although much more friable, is plastic, i.e. readily deformed, especially when heated. The lack of a rigid crystalline structure makes it relatively easy for the one metal to permeate the other. Antimony (Z = 51) was confused with its sulphide, but also with lead and, although well known to the alchemists, remained mysterious until Basil Valentine's exposition of the element in his 'Triumphal Chariot of Antimony' of 1604. Known as 'Our Lead' by the hermeticists, it was used as a substitute for the lead used in the gold extraction process. It's unremarkable that they should have confused the two silver-grey metals. The melting points of the two are significantly different, 327.5 K for lead, 630.7 K for antimony, but both are sufficiently far below that of gold (1064.4 K) for them to function in a similar way during the extraction process. Separating out the antimony afterwards was facilitated by the fact that, even in solid form, let alone as a powder or when molten, antimony is surprisingly volatile at room temperature. One indication of antimony's suitability for the extraction of precious metals is the existence of an important silver ore containing it, Pyrargyrite, or ruby-silver, Ag3SbS3 and 2 minerals, Dyscrasite, Ag3Sb, and Aurostibite, Au3Sb. Antimony sulphide was used to separate the metals in gold-silver alloys by cupellation, in ancient China, during the Chan Kuo period (480-221 BC). Melting them together in the cupel produced a layer of silver sulphide above a layer of gold-antimony alloy, probably containing gold antimonide, Au3Sb. Scraping off the upper layer and heating the lower drove off the antimony as stibine gas, SbH3, and as a vapour, leaving the gold. 63 APPENDIX D BASIC CRYSTALLOGRAPHY The use of Miller indices These are used to define the planes of a crystal lattice for the purposes of determining how these planes will interact with X- or neutron rays at different angles of incidence and thereby building up a picture of the crystal structure. The numbers represented by the letters h, k and l define a plane to which a symbol (hkl) may be given, and are called its Miller indices, after Miller, who introduced them. The Law of Rational Indices. ‘A face which is parallel to a plane whose intercepts on the 3 axes are Ha, Kb, Lc, where H, K and L are whole numbers, is a possible face of a crystal and, for the planes which commonly occur, H, K, and L are small whole numbers.’ The greater number of the many problems associated with crystal identification are undoubtedly due to the word 'possible', and, strange to say, the word 'commonly' also. For the planes are always associated with line intervals, for powder camera scans, and peak intervals, for computer-recorded powder layer scans. Taking any one type of crystal lattice, there will be such a multitude of substances referable to lines/peaks which are similarly spaced that any distinction between a line/peak range supposedly common only to one substance and a line/peak range associated with another is very easily lost. Furthermore, if there are many lines/peaks crowded into the observation space a particular isomorph of one element, for example, becomes difficult to associate with its standard reference scan when comparing indices. It may become associated with some atypical version (or adulterated sample) of a completely different element whose indices derive from an equally crowded diffraction pattern. Note concerning the axial intercepts. For a given axis ratio a:b:c, the Miller indices of a plane are inversely proportional to its intercepts on the axes h/a, k/b, l/c and the direction cosines of the normal to the plane. The normal to a plane defines that plane crystallographically. It follows, from the definition of rational indices, that: OA' : OB' : OC' = Ha : Kb : Lc = a/KL : b/LH : c/HK = a/h : b/k : c/l. 64 The magnitude of the perpendicular to the face A'B'C' from the origin to that face, shown as the line ON = d. SEE DIAGRAM OVERLEAF. So cos α = d/(a/h) = dh/a , cos β = d(b/k) = dk/b and cos γ = d/(c/l) = dl/c . These are the direction cosines of ON, so: cos2 α + cos2β + cos2γ = 1 d2h2/a2 + d2k2/b2 + d2l2/c2 = 1 h2/a2 + k2/b2 + l2/c2 = 1/d2 Now, treat the atoms of the crystal lattice as similar, equally spaced, parallel planes. Any diffracted X-ray beam which does occur must therefore be in a direction corresponding to reflexion of the incident beam from a set of crystal planes. There will, however, be no high intensity diffracted beam unless the waves reflected from the different planes are exactly in phase. The X-ray glancing angles, called Bragg angles, are indicated on the above illustration of the relationship between the atoms and the beams. The path difference between beams 1 and 2 is BC + BD and where the beams are in phase this represents a whole number of wavelengths, n = 1. Therefore: BC + BD = n λ = 2d sin θ B where d = the spacing between the planes lambda = the wavelength of the X-rays. theta B = the Bragg angle. For first-order reflections, i.e. the strongest, n = 1: Sin θ B = λ /2d. So sin2θ B = (λ 2/4)(1/d2) 65 Now, refer to the last equation relating to the Law of Rational Indices, above: h2/a2 + k2/b2 + l2/c2 = 1/d2 Put h = k = l = 1 So 1/a2 + 1/b2 + 1/c2 = 1/d2 Next, substitute for 1/d2 in the equation for sin2θB giving: sin2θB = (λ2/4)(1/a2 + 1/b2 + 1/c2) or sin2θB = λ 2/4a2 + λ 2/4b2 + λ 2/4c2 This represents the most important equation in the process of determining the scattering angles at which peaks in the intensity of reflected X-rays may be found, using the unit cell dimensions for the relevant crystal type of a particular chemical compound. APPENDIX E. Scans of samples taken using the PW1720 17. 18. 19. 20. 21. 22. 66 APPENDIX F. Atomic decay sequences. Natural radioactivity is the result of the spontaneous decay of unstable atoms, those with a neutron surplus in their nuclei. The decay (or 'disintegration') of atomic nuclei is usually accompanied by the emission of alpha, beta or gamma radiation. The alpha particles are helium 4 nuclei so consist of 2 protons bonded to 2 neutrons, the beta particles are electrons from the division of neutrons into protons and electrons and the gamma particles are photons, but more energetic than standard daylight photons. The product or daughter nucleus left after the alpha decay of an unstable nucleus is that of an element with atomic number (Z number) two below that of the parent nucleus. The product nucleus of the beta minus decay process has a Z number one above that of the parent nucleus and the same atomic mass number (A number), because a neutron has converted to a proton so the number of nucleons remains the same. Atoms in which this A number remains constant during transmutation are termed isobars: n → p + β- + ¯νe The product nucleus of the beta plus (positron) decay process has an A number one below that of the parent nucleus but, again, the atoms are isobars, because a proton converts into a neutron: p → n + β+ + νe Instead of this, a proton could convert to a neutron by way of electron capture: p + e- → n + νe As a result, an element, number Z, decaying by electron capture, would transmute into the one below it in the Periodic Table, with Z - 1 protons. As before, the atoms are isobars. However, extra-atomic electrons are repelled by those orbiting the nucleus, which represent an electric force termed the Coulomb barrier. As a result, only ground level energy electrons in the first orbit (that closest to the nucleus) can be captured by a proton. As electrons only have a very low probability of being far enough out of their orbits for this to happen, due to regulations imposed by quantum mechanics, the probability of electron capture is also very low. In fact, it requires the density and temperature of a white dwarf star collapsing gravitationally to form a neutron star for such a reaction to promulgate at an appreciable rate. Therefore, no measurable number of mercury 196 atoms could become gold 196 atoms in this way. Even if they could, due to some other cause, they would soon decay back into mercury 196 atoms again by beta minus decay because gold 196 has a halflife of only 6.18 days. Even if it were in the form of solid gold, it would decay to a reddish powdered mixture of gold and mercuric oxide, as suggested by the accounts of fairy or leprechaun gold, draining from the victim's pocket whilst, presumably, irradiating them with protons. 67 The spontaneous fission ('splitting') of a nucleus into 2+ parts of comparable size, due to the impact of neutrons derived from cosmic rays, is normally accompanied by the emission of a neutron or neutrons or gamma rays. Spontaneous fusion can only occur with high energy input, as occurs in the Sun, or due to the tunnelling of nucleons through the high potential energy barrier separating their nuclei. Both spontaneous processes are very rare, being accompanied by the emission of gamma radiation, light energy released as the nucleons fuse to form different nuclei. This produces a decrease in their potential energy, released in the form of the light as they reach their new rest mass energies. Both of these spontaneous processes are very rare under standard (terrestrial) conditions. There are 4 radioactive decay series, the thorium, beginning with thorium 232, the neptunium, beginning with neptunium 237, the uranium, beginning with uranium 238 and the actinium, beginning with uranium 235. All terminate at bismuth or lead. This indicates that lead does not decay spontaneously into either mercury or gold. These decay series proceed by way of alpha or beta minus decay. As beta minus decay causes an element's Z no. to increase by 1, whilst alpha decay causes it to reduce by 2, but the series represent irregular reductions in Z no. throughout, the maximum reduction being from Z = 93(U) to Z = 81(Pb), it is easy to see that alpha decay predominates. The discovery of nuclear radiation was due to the examination of the 14-stage uranium 238 series' decay products. Some of these were found in pecheblende (or 'pitchblende'), the 'bad-luck mineral' discovered as a by product of the German and Bohemian copper and silver mines from the early C16 onwards. The name given to it was due to the absence of copper or silver in the mixture. However, it contained radium 226 (half-life = 1,600 years), which emits alpha radiation to become radon 222, an unstable gas with a very low half-life, meaning that it is a rapid emitter of, in this case, alpha particles. This made it an unseen menace to the miners who breathed and ingested it as it decayed to polonium 218, creating the first victims of industrial radiation poisoning in Western Europe. Now, pitchblende was black and the first stage of the production of the Philosopher's Stone (PS) is that of 'perfect blackness', termed 'the nigredo', in which 'the whole substance resembles molten pitch, or a bituminous substance.... resting in one entire black substance at the bottom of your glass.' according to Sendivogius. Alchemists may, therefore, have recognised pitchblende's positive potential. They certainly appear to have suffered from symptoms associated with its negative effects after drinking a solution of whatever version of the PS they came up with in the pursuit of immortality, though the effects have also been attributed to mercury poisoning. 68 APPENDIX G. Cosmic rays, the pion and the muon. The energy density of the cosmic background radiation is ρ = 2.5 × 105 eVm-3 or 4.0 × 10-14 Jm-3. Starlight accounts for most of it. However, there are also numerous energetic sub-nuclear particles, such as the kaon. Cosmic kaons decay to give pions and muons, and pions decay to give muons, in the Earth’s upper atmosphere, a few kilometres above sea level. A large flux of these cosmic ray muons are observed at sea level; ~180 particles m-2s-1. Indeed they account for most of the cosmic rays detectable at that level. ‘Long-lived’ neutral kaons have an average life of 5.18 × 10-8s, referred to as their ‘lifetime’, decaying to pions and electrons or muons, with their neutrinos: K0L → π+ + e- + νe or π of the π 0. + + μ- + νµ or π - + π - + π0 or π 0 + π 0 + π 0, but you’ll get no muons out The charged pions (lifetime = 2.6 × 10-8s) decay in the same way: π - → μ - + νµ π 0 → μ + + νµ The muons, μ -, (lifetime = 2.6 × 10-6s, observed lifetime = 4.4 × 10-5s) are then able to interact with deuterium directly: μ - + 21 H → 21 H* + β The 21H* represents an exotic deuterium atom, the muonium atom created by the substitution of the muon for the electron. This may then interact with an ordinary deuterium atom: 2 1 H* + 21 H → H2+ + e- This represents the chemical bonding of deuterium with exotic deuterium to give an exotic, ionised, covalently bonded hydrogen gas molecule with ejection of an orbital electron, displaced by the muon. Then, maybe: d + d → 32He + n This time the bonding is nuclear; the deuterons bond to give a helium 3 atom, emitting a neutron. Alternatively, the antimuons, μ +, can interact with protons indirectly, via their decay products, principally the electron’s antineutrino: μ + → e+ + ¯νe + νµ ¯νe + p → n + e+ 69 Appendix H. An analysis of Ripley's 'Bosome-Book' from a modern chemistry perspective. A copy of the book itself, published in 1683, can be seen at http://www.levity.com/alchemy/bosom.html. The following is based both on current chemical identities and their observed relationship to the results of my own experiments using the same substances as Ripley refers to. The only differences arise from the fact that I had the choice of compounds of a higher purity than Ripley had access to. Paragraph 1. The antimony referred to would be almost pure stibnite (Sb2S3). Even today it is very difficult for laboratories to produce pure antimony on anything approaching a commercial scale. The distilled vinegar is, of course, as close to acetic acid as was then practically attainable. The antimony acetate produced by their combination is only a transitional compound, yielding on oxide of lower purity than is achieved using hydrochloric acid. The C16 chemists simply had no access to concentrated strong acids. Paragraph 2. "...our Sericon will be coagulated into a green Gum called our greene Lyon". This process had great mystical significance for alchemists. In fact a solution of antimony in an excess of acid, whether it be acetic, hydrochloric, nitric or a combination of these acids, will appear as an oily yellow liquid, the green colour indicates the presence of the sulphide ions as an impurity. The only practical significance of its appearance here is as an indicator that the weak acid has put part of the stibnite into solution; the sulphide must be released, in the form of hydrogen sulphide, before a pure oxide can be produced. Paragraph 3. "...when you see a white Smoak or fume issue forth, then put too a Receiver of Glass..." The acetic acid could not be wasted, so would be recovered as the antimony acetate was converted to oxide. The fume becoming reddish as the heat applied to the retort was increased might indicate the release of red antimony sulphide ('antimony vermilion') but antimony trioxide (Sb2O3) is also volatile so a proportion of the vapour would effectively be a solution of Kermesite, a mineral that combines the sulphides and trioxides of antimony. The condensed vapour would be known, from experience, to contain useful substances, though it is unlikely that the presence of antimony was assumed. "...a white hard Ryme…a Frosty vapour" The description is wholly consistent with that of antimony trioxide, sublimed. So far the process is identical with that required for the production of mercuric pyro-antimonate using minimal resources, so that the intermediate reagent, antimony oxyhydrate, cannot be generated and a less efficient route must be taken. 70 Paragraph 4. This deals with the roasting of a portion of the remaining precipitate to impure antimony trioxide. Due to the appearance of the 'clean', white, colour, it is unlikely that an alchemist would realise that the white calx, "the Basis and Foundation of the Work", was of a lower purity than the sublimate previously obtained. Paragraph 5. The rest of the stibnite is 'calcined' to the flame-orange isotropic form, antimony vermilion, my own experiences suggesting that it would contain antimony pentoxide as an impurity. If nothing else, the distracting experiments with these sulphides and impure trioxide of antimony would have yielded a full range of the thermally stable allotropes of these compounds. Paragraph 6. The antimony vermilion is redistilled to separate out more of the antimony and sulphide ions in solution with the acetic acid. The acetates must precipitate out of this if "the Fire of the Stone", presumably sulphurous acid, is to develop. Paragraphs 7 and 8. By carefully and repeatedly distilling the solution, a "yellow Oyl" of pure antimony in acid solution is obtained, leaving behind "Ardent Water", a strong acid, though most likely it is sulphurous rather than sulphuric acid. The latter could be extracted by repeated distillation. I must admit that I have not had the patience to attempt to replicate this part of the alchemical process since, like so many of its kind, it serves no useful purpose if you already have strong acids to hand. "....put upon (Sublimate) some of the Ardent Water". This would be a good idea if the mercury was available as a pure metal, but where, as in this case, it is already ionised, with a valency of +2, it might as well be heated slowly, replacing the chloride with oxide. The process described simply degrades the purity of the mercury by introducing its sulphate into an acid solution that resembles the green solution produced by the dissolution of antimony sulphide in excess acid. Now, if the acetic acid were introduced directly to the purified mercury there might be some useful purpose served since a helpful internet correspondent, writing in the 'alt.engr.explosives' forum of the Deja.com website, Henri Lehn, has pointed out to me that a Russian method for producing mercuric pyro-antimonate involves combining mercury in acetic solution with a complex of potassium and antimony hydroxides. I am assuming an identity between the pyroantimonate and the 'Stone' for this purpose. The only progress achieved by adopting the course described here is that it adds hydrochloric acid to the "Ardent Water", which at this point would comprise sulphate, chloride, mercury, antimony and sulphide ions, all in solution. Paragraph 9. Heating mercury compounds in water always reduces them back to mercury, eventually. Evaporating the sulphide to a thick solution produces black cinnabar mixed with finely divided mercury, a dense black mixture. "Note when the Liquor cometh white, ..." indicates the contribution of white mercuric sulphate (HgSO4) to the "Ardent Water". None of these should be "taken inwardly" any more than should a mild solution of bleach, but this recommendation may represent an origin for the use of mercury in the cure of syphilis. 71 Paragraph 10. Recombination of sulphuric acid with mercury and mercuric sulphide would produce, though only at one stage in the heating process, a mixture of red mercuric sulphate and the red allotropic form of cinnabar ("Mans blood rectified"?). This is really of no importance to the end result, merely an indicator of the tendency of alchemists to be distracted by any red compound or solution. Paragraphs 11, 12 and 13. The remaining black cinnabar is subjected to oxidation by the sulphuric acid recovered using distillation from the previous stage. Heating and breaking down the black concretion produced (trituration) produces a powder which can be more readily heated to mercuric oxide with finely divided mercury. Unlike its sulphide equivalent, this appears as a white powder. Paragraph 14. The mixture of chloride, sulphate and antimony ions in solution is added to the impure mercuric oxide. "...distil it with a strong Fire ..... and then distil it again .... and thus distil and Calcine 7 times." Ripley may have forgotten to add "and imbibe it again with the Fiery Water". Certainly, if this is what he meant, the process would add all the mercury to the acidic solution. Vapourising the mercury together with the steam from the solution in this way would have been safer than vapourising mercury on its own and collecting it in the solution. The penetrative properties of the liquid metal serve to reinforce the oxidising effect of the acid radicals. Antimony also penetrates most metals if finely powdered and heated with them. Thus the "Water of Life rectified" would appear to "dissolve all (metallic) Bodies" since, if it was too low in the reactivity series to be attacked by the acids a metal would probably amalgamate and/or be alloyed with the antimony. "Take the Cerus or Cream of the finest and purest Cornish Tinn ...." The recipe described is effectively one for producing tin amalgam, long used for 'silvering' mirrors, but with antimony as an impurity. This would give it the desired 'matt effect', the better to simulate silver, but any qualified assayer would have spotted the presence of copper in the form of its yellow and blue compounds in solution (visible as green) when applying the acid test. Presumably the fraud was only intended to pass casual inspection. Paragraphs 15 and 16. Firstly, the mercuric and antimony sulphides and sulphates precipitated from the "Flood", or less volatile substances remaining in solution after the distillation described in paragraph 10, are removed by further distillation. This would render the solvent more effective by eliminating 'buffer' compounds. Then the all important combination of the antimony trioxide with the acid solution containing all the mercury introduced as 'sublimate' in paragraph 8 is described. There are two ways in which this vital feature may be missed. Firstly, a casual reading of the recipe would miss the connection between the 'sublimate', the fact that "all the Substance of the Calx be lifted up ... and then hast thou the Water of Life rectified" (para.14) and Ripley's use 72 of the term "our Ardent Water rectified" in paragraph 16. Since introducing the principle solvent as "our Ardent Water rectified" in paragraph 8, he has redefined it three times during its 'fortification', on the final occasion as "our Mercury", which is how he describes it in the rest of his book. This is therefore the only description he should have used and his consistency with respect to his other terminology makes me think that he wanted to confuse the inexperienced rather than sell them the 'secret' of his method for the price of the book. This was just the sort of practice that Boyle was later to condemn but it is a crucial feature of my case that Ripley was detailing the early laboratory production of the meta- and pyro-antimonates of mercury. As he would not have realised this, I am assuming that experience taught him how unstable the resultant products were if this stage of the process was omitted. Of course, he could not carry out the reaction under oxygen and therefore it was vital to confine the volatile metals in a hermetically sealed vessel while they oxidised. Paragraphs 17, 18 and 19. "... the Stone within the Glass become(s) first Russet, and after whitish green, and after that very white ..." This description is easily identifiable as the oxidation of mercury and antimony to their russet-coloured mixed ternary oxide, the pyro-antimonate, followed by the reduction to the white secondary oxide or meta-antimonate, accompanied by the loss of mercuric oxide contaminated with mercury from the lower portion of the vessel. The meta-antimonate is the only compound I have encountered that stains glass a silverish white. Other compounds, in particular those of mercury or of antimony alone, simply decompose at temperatures that are too low to allow them to remain stable until the surface of the soda glass melts. I use pyrex glass in the test process, for good measure. Evidently, the white compound and its associated sublimate are divided so as to produce a silver amalgam (the "white work") and a gold amalgam (the "Red-work"). This was standard alchemical practice. Heating one of these portions in a sealed vessel would reproduce the unstable pyro-antimonate as the sublimed mercuric oxide re-entered the meta-antimonate. Paragraphs 20, 21, 22, 24 and 25. Basically, these do no more than describe how to make and implement the silver and gold amalgams. The 'matt effect' produced by the antimony disguises the mercuric 'sheen' of the resultant silver and gold substitutes. They are of no relevance to the topic of cold fission, though the yellowing of molten lead by the reddish-brown pyro-antimonate is an interesting phenomenon. It seems that the gold just augments an effect that is easily generated without its inclusion. Paragraph 26. The process of 'Multiplication' appears, in this case, to involve the repeated "dissolution" and "congelation", i.e. separation and recombination of the oxides by heat, without the addition of any exterior substance. However, the soda glass on the surface of these "Viols" would gradually flake away into the compounds due to thermal stress during these sessions even though nobody seems to have realised this at the time. 73 Paragraph 27. The further amalgamation of silver or gold amalgams with a mass ratio of 1 part amalgam to 100 of mercury might seem unusually unconvincing as versions of solid metals. Of course, the term "converted into Medicine" may easily be an indication that the compound must once again be heated until it forms another crystalline powder, through oxidation. The greatest limitation on the alchemists' understanding of the actual processes involved is seen to be their belief that all calxes had to be white. In the current context, the calx was red, provided that my analysis of the reactions occurring up to this point is correct. Paragraph 28. Ripley's "Accurtation of the great Work" exhibits, more plainly than in the rest of his book, the clear parallels between what he is trying to describe and the chemical reactions currently utilised in producing mercuric pyro-antimonate, as exemplified by Professor Arthur Sleight in his report of 1968 to the 'Journal of Inorganic Chemistry'. "The white Frosty Ryme" is Sb2O3 (see paragraph 3) and it is "sealed up" with the silver amalgam and heated to oxidise the antimony and mercury (Sb3+ ions becoming Sb5+ ions). This is the "fixation" of mercury, that is to say, its stabilisation as a mixed oxide. Adding "our Mercury" to it adds the remainder of the mercury from the mercuric chloride referred to (as sublimate) in paragraph 8. The conversion of mercuric meta-antimonate (HgSb2O6) to mercuric pyro-antimonate (Hg2Sb2O7) is achieved as before. Presumably, as silver amalgam is used (for the "white Work") gold amalgam is also employed in reproducing "the Stone" in this abbreviated version of the experiment. Paragraph 29. Various permutations of the substances previously prepared appear here but no explicit mention is made of additional reactants. It is difficult to believe that soda glass (Na2SiO3) has not entered into the process when the final result is described as being "transparent in Colour like a Ruby ..." Ruby glass was produced by heating gold in its colloidal particulate form until it adsorbed into glass. As the colour would only appear after the glass was reheated, expanding the colloidal particles, this circumstance might account for the Stone's vitreous characteristics only becoming apparent towards the end of the process. By way of support for this hypothesis, I can testify to the opacity of all the antimony and mercury compounds I have produced, likewise to the effect of heating the meta/pyro-antimonate of mercury in Pyrex glass boiling tubes until the surface of the glass melted (i.e. up to ~ 9500C) at which point the glowing oxide adsorbed into it to give a fine ruby-glass (substitute) without my having recourse to gold. 74 APPENDIX I. Circumstantial evidence for the existence of Red Mercury referred to in 'The Mini-Nuke Conspiracy'. The book was written by two investigative British journalists. Peter Hounam researched a number of TV documentaries for Channel 4's 'Dispatches' series, probably including 'The Hunt for Red Mercury' and 'The Pocket Neutron', both of which deal with the trade in the mystery substance. Steve McQuillan worked in Johannesburg, becoming deputy editor of the Sunday Star and then the Weekend Star. He was therefore well placed to witness the series of revelations that led to the discovery of the South African Red Mercury (RM) trade, the principle subject of the book, as indicated by its subtitle, 'Mandela's Nuclear Nightmare'. One of the best examples of evidence for the substance's existence is Appendix 1, on page 285, the list of export documents associated with the trade, as these are the sort of items that could be traced; they are not just anecdotal. Of particular interest is the transaction for 6/3/1992, authorised by B.N. Yeltsin on 21/2/1992, 10,000 kg of RM supplied by Promecology in Ekaterinburg. A former soldier with the South African Defence Force told the researchers (p.242) that he saw RM inside a military complex in Pretoria: 'On one occasion I decided to have a closer look at what we were guarding and took one of the bottles from the packing tray .... The bottles (had) a narrow neck opening to a broad base and (were) 12 cm to 15 cm tall. Inside was a thick liquid, (it was) just below half full. In the top was what I later learned was a detonator. I now know it was red mercury. I believe what I was holding was the detonating device for a nuclear shell. The devices with wires at the top of the bottles were the pre-detonators, and sensitive to electricity (sic).' This first-hand account is the sort that provides vital clues to the appearance of RM in transit, usually lacking in journal accounts. The British expert Frank Barnaby discovered (p.126) that: 'Specifications faxed from Russia showed that red mercury was a compound of mercury, antimony and oxygen with the chemical formula Hg2Sb2O7. Delving through databases at his local college, King Alfred's at Winchester, Hampshire, he traced only one reference, an abstract of an article written in 1968. The British Library's Science Reference Department in Holborn, London, provided a copy of the original report, which showed that Dr. Arthur Sleight of the American chemical giant E.I. Dupont de Nemours, in Wilmington, Delaware, had synthesized the material as a red-brown powder. Sleight predicted no special properties for his creation of so long ago, but Barnaby was delighted to discover the reference: it could no longer be said that the basic chemical, defined in the Russian specifications, was a complete sham.' 75 He also learned (p.127) that: 'in Russia a very pure form of the powder was dissolved in ordinary mercury metal..... It was then put in containers which were placed in the heart of a nuclear reactor for about twenty days. Under intense neutron bombardment, and perhaps with the addition of catalysts, the material was transformed and became a very thick and heavy cherry-red liquid.' On pages 60-61 there is a footnote which appears to confirm this account of RM's appearance: '(Oleg) Sadykov was later interviewed for a Dispatches programme aired by Channel 4 Television in Britain and produced two jars which he said contained the basic material from which red mercury was synthesized. One bottle, which was supposedly fresh, appeared to contain a dark treacle-like substance. The other, which Sadykov said needed refreshing, was partly liquid and partly granular.' Oleg Sadykov was the co-discoverer of mercuric pyro-antimonate in 1968 and head of Promecology, which supposedly manufactured RM. Most likely he was interviewed in 1995. Unfortunately, Channel 4 do not keep videos of programmes submitted to 'Dispatches', even where these have been accepted for transmission. Accounts of issues related to RM are a lot more plentiful in the book than references to tangible evidence of it. On pages 56-57 there is an account of how Peter Hounam and John Large, a nuclear engineer advising Greenpeace, met someone he calls ‘George’, who claimed to be a nuclear physicist, on a train bound for Ekaterinburg in July 1992. George said that: 'When it is made, (RM) is a powder which is dark red in colour. But we irradiate it in a nuclear reactor which turns it into a very heavy liquid, the colour of wine. It is very, very expensive, because it is very difficult to make.' Later he added: 'Most people are still glad the communist regime has fallen...but it has led to many bad things, like the growth of the Russian mafia who control things like the red mercury black market.' Once in Ekaterinburg Peter Hounam and John Large met with Yevgeny Korolev(p.55). Korolev was an Ekaterinburg city councillor and a local hero. He said (p.59) that: '...the smuggling trade in the chemical was a major problem for the authorities, because the Russian mafia had penetrated the military industries and could control the supply.' Later on: 'George took us to Vitaly Mashkov, who was People's Deputy for the Sverdlovsk Region and a political ally of Yeltsin. (Mashkov said) that Russian scientists had a 76 unique method of separating plutonium from irradiated uranium. Then ....he linked this to Red Mercury: 'It is a great scientific advance - something that Russia can be proud of..... You must realize it is also a grave proliferation threat.' If true this would account for the lack of corroborative evidence in the Western media. 77 APPENDIX J. Useful Internet addresses. news.bbc.co.uk/2/hi/uk_news/5176382.stm News report of the notorious incident in which three suspected terrorists were on trial for trying to acquire Red Mercury and the Crown prosecutor, Mark Ellison: ‘admitted the police had no idea if there even was such a thing as red mercury - supposedly the main ingredient for a "dirty bomb" which could have devastated London. But he told the jury at the outset: "The Crown's position is that whether red mercury does or does not exist is irrelevant." He warned the jury not to get "hung up" on whether red mercury actually existed at all.’ www.theregister.co.uk/2006/07/31/red_mercury_trial/ Reference to the News of the World’s part in encouraging belief in the existence of an ‘Islamofascist’ terrorist trade in Red Mercury. www.levity.com/alchemy/e_mail_g.html A site devoted to ongoing discussion of the alchemy concept and its history. http://www.homelandsecurityus.net/jill?s%20comments/Red%20Mercury/ red_mercury.htm Provides references to two articles, one in the Tribune Review, the other in the Tribulational Institute, bearing upon RM’s existence. http://trade-leads.rusbiz.com/123161.html One worth checking out just to determine if it's for real. http://www.csicop.org/si/#science_and_reason The URL of the Committee for the Scientific Investigation of things they don't like the look of. Skeptic's corner. http://wsj.com/tour.htm The Wall Street Journal occasionally has useful references to the Red Mercury issue. http://www.cas.org The online home of the Chemical Abstract Service. 78 http:// medinfo.wustl.edu/~ysp/MSN/ The Mad Scientist Network URL. Every bit as plausible as CSICOP regarding entities for which it has no direct proof. http://www.alchemywebsite.com/dr_price.html The Transmutations of Dr. Price, on The Alchemy Web Site. Unfortunately, they weren't genuine nuclear transmutations. http://en.wikipedia.org/wiki/Red_mercury http://www.imdb.com/title/tt0443619/plotsummary A topical dramatic use of the Red Mercury concept, likely to attract the curious to the question of its existence. BIBLIOGRAPHY The Sceptical Chymist: R. Boyle Alchemy, the Ancient Science: N .Powell The Alchemist's Handbook: "Frater Albertus" The Timetables of Science: A. Hellemans and B. Bunch Science in the Enlightenment: T .L. Hankins The Hunt of the Greene Lyon; The Foundations of Newton's Alchemy: B.J.T. Dobbs The Newton Handbook: Derek Gjertsen Textbook of Inorganic Chemistry: J.R. Partington (1931) Experimental Chemistry: Stockhardt and Heaton The Chemistry of Zinc, Cadmium and Mercury: B.J. Aylett Macmillan's Chemical and Physical Constants The Mineral Kingdom: Paul E. Desautels The Collector's Encyclopaedia of Rocks and Minerals: edited A.F.L. Deeson Mineralogy: Berry , Mason and Dietrich Inorganic Chemistry: A Modern Introduction: T. Moeller Introduction to Advanced Inorganic Chemistry: Durrant and Durrant The Handbook of Chemistry and Physics: R.C. Weast The McGraw-Hill Encyclopaedia of Science and Technology Chemistry Data Book: T.G. Stark and H.G. Wallace Tables of Physical and Chemical Constants: Kaye and Laby Alchemy: E.J. Holmyard Science & Civilisation in China: J. Needham The Origins of Mercury Gilding: Lins & Oddy (1975) The Mini-nuke Conspiracy-Mandela's Nuclear Nightmare: P. Hounam & S. McQuillan 'New Ternary Oxides of Mercury with the Pyrochlore Structure' in The Journal of Inorganic Chemistry; Vol. 7: Dr. A. Sleight(1968) Chemistry Made Simple: F.C. Hess and R. Care 'Observations of cold nuclear fusion in condensed matter.': S.E. Jones, E.P. Palmer et al, in Nature, Vol. 338, p. 737. 'Exact Upper Bound on Barrier Penetration Probabilities in Many-Body Systems: Application to "Cold Fusion".': A.J. Leggett and G. Baym, in Physical Review Letters, Vol. 63, Number 2, p. 191. 'Can solid state effects enhance the cold-fusion rate?': A.J. Leggett and G. Baym, in Nature, Vol. 340, p.45. Any enquiries about this webpage should be addressed to: - [email protected] See also 'Red Mercury' by Mark Fabi, published 2004-09-30. ISBN-13: 9780553378757 ISBN-10: 0553378759 INDEX A A-bomb 41 acetic 70 acetic acid 69 acetate(s) 70 acid 2, 4, 7-9, 15, 16, 23, 29, 30, 31, 46, 47, 59, 61, 69, 70, 71 acidic salts 47 actinide 3, 41 actinium 67 Agricola 12 alchemical 3, 12, 23, 48, 50-52, 61, 70, 72 alchemistic 50 alchemist(s) 3, 11, 12, 15, 16, 23, 27, 41-46, 50, 51, 53, 62, 67, 69, 73 alchemy 11-13, 15, 43, 48-54, 57, 77,78 al kohol 12 alcohol 12, 13 alkali metals 23 allotrope 70 alpha 5 alteration product(s) 6, 7 amalgam 7, 27 analogous 5, 27 anions 4 Ångström 33 antimonates 4 antimonic acid 9, 26 antimonic oxides 53 antimonide 46, 47, 62 antimonite 8 antimony 2, 3, 6, 10-12, 15, 20-23, 36, dia 9 acid 2 amalgam 23 glass 17 hexoxide 7 hydroxide 7 oxide 2,6,7 oxyhydrate 26 antimony oxysulphide 6, 27 pentachloride 30 pentoxide (Sb2O5) 4, 7, 21, 28, 35, 70 dia1 salts4 sulphide(s) 6, 22, 47, 50, 57, 62, 69-71 trioxide (Sb2O3)6, 8, 15, 16, 22, 69-71 trisulphide (Sb2S3) (antimony vermilion) 69, 70 antimuon 68 antineutrino(s) 39, 40, 43, 44, 68 antiparticles 55 antiquark 55 Arabic 48, 49 Arabs 49 Aristotle 15, 48 Aristotelian 11 arsenates 10 arsenic sulphide 50, 52 arsenious acid 50 atomic 60, 66 decay 66 fission 41, 42 nucleus(ei) 39, 55, 59, 60 mass number 40 number 46, 60, 66 radius 60 weight 58 masses 60 atom(s) 33, 35, 38-47, 54, 57-62, 64, 66, 68 atomic mass number 40 aurifaction 51 aurification 51 Ashmole, E. 18 Avicenna 19 Aylett, B.J. 37 B ‘bad-luck mineral’ 67 barium sulphate 61 Barn, the 39 Barnaby, Dr. F. 2 Barns 39, 40 Bartolomeo de Medina 61 baryons 54 barytes 61 Beauvais, Vincent of 19 beta 5 beta-minus decay 66, 67 beta-minus particle 66 beta-plus decay 66 beta radiation 54, 66 Bindheimite 9 bipyramidal 4 bismuth 23, 57, 60, 67 pentoxide dia 1 bituminous 67 bombs 41 bone-ash 61 Bonus, Petrus 19 boron 57 boron trioxide 57 bosons 54 Boyle, R. 11, 12, 14, 15 Bragg angles 31 Bragg equation 25 Braune 61 C cadmium 35 caesium 60 calomel 6 calx(es) 70, 71, 73 Cantonese 49 Carneades 11, 16 catalysis 45 catalyst 75 Cavendish, H. 16 Chadwick, J. 55 Channel 4 74, 75 Chan Kuo period 50, 62 Charnock, T. 18 chemical 45, 57-60, 68, 69, 74, 75 Chemical Abstract Services (CAS) 7, 26, 27 chemistry 57, 69 chemists 69 Cheng Lei Pen Tshao 52 Chhen Chi 50 Chhen-chou 52 chhi 48 Chhing Hsia Tzu 52 chhi tan 48 chhung chin 51 ‘chimistry’ 49 China 7, 48-50, 52, 62 Chinese 48, 49, 52, 53 Christian II of Saxony 13 chu sha chin 51 Cinnabar 6, 7, 12, 16, 22, 48, 51, 52, 70, 71 cold fission 45, 72 nuclear fusion 44, 45, 55 colloidal gold 52, 73 stannic oxide 52 Conservation of Mass 59 Energy 59 copper 11, 13, 15, 51, 57, 58, 60, 61, 67 oxide 58 sulphate 61 cosmic ray(s) 67, 68 Coulomb barrier 66 covalently bonded critical mass 40 size 40 cross-section 41, 44 crucible 44 crystal 63-65 faces 63 lattice 63, 64 crystalline 37, 38, 62, 73 compounds 73 crystallography 33, 37 crystallographically 63 crystal structure 63 cubic 33 cupel 50, 61, 62 cupellation 50, 62 D Debye-Scherrer camera 25 density(ies) 41, 58 detonator(s) 41, 74 deuterium 42, 44, 68 atoms 42, 43, 45 deuteron(s) 42, 44, 45, 68 fusion 44 diffracted 64 Dispatches 3 distillation 70, 71 Du Pont de Nemours 28 Durrant & Durrant 9 Dyscrasite 62 E Einstein, Albert 25 Ekaterinburg 74, 75 electrical 54 electric force 66 electricity 74 electrochemical cells 45 electrode 45 electrolysis 57 electrolytic catalysis cells 45 cells 42, 45 liberation 45 electromagnetic 56, 58 electron(s) 39, 40, 42, 54-56, 58, 60, 66, 68 electron's anti-neutrino 38 electron shells 26 elemental 57 element(s) 40, 41, 54, 57, 60, 62, 63, 66, 67 Eleutherius 11 energy 59, 62, 67, 68 experimental 57 experiment(s) 69 extraction 61, 62 F Face-centred cubic(FCC) 34 Fermi 54 Fermions 55 ferric sulphide 15 fission 42, 55, 72 bomb 40, 41 chain reaction 40, 43 device 41 process 41 reaction 40, 43 reactor 40, 67 fusion 42, 45 rate 42, 67 G gamma 66 gas 67 Germany 55 Gibaud 55 gluon(s) 55, 56 gold 12, 13, 15 Greek 57 H hadron(s) 55, 56 Hahn, O. 55 hairpins 52 half-life 46, 67 Han dynasty, the 50 heat 45, 47, 72 heavy water 42, 44, 45 helium (He) 40, 42, 44, 45, 55, 60, 66 atom 45 Hellenistic 49 Helvetius 14 hermetically sealed 72 hermeticists 62 hexagonal mercuric oxide dia 5 high explosive 41 high-temperature superconductors 37, 38 Holmyard, E. 48, 50, 51 Hounam, P. 74, 75 hsuang huang yin 52 'Huai Nan Tzu' 48, 50 huang yin 52 Hunan 52 Hung, K. 48 hydrate 30 hydrochloric acid (HCl) 11, 12, 15, 30, 68, 70 hydrogen 44, 45, 55, 60, 68 sulphide 15, 68 hydrolysis 30 hydrous antimony oxide 7 I immortality 51 implosion device 41 indices 63 inorganic 50 intensity(ies) (Iobs) 35, 36, 65 International Chemical Register (ICR) 28 iodine 23 ionic 47 compounds 45 molecule 44 ionised 47, 68,70 ion(s) 47, 55, 61, 68, 70, 71 iridium 60 iron (Fe) 4, 11, 12, 15, 61 retorts 61 sulphate 61 isobars 66 isomorphs 63 isotope(s) 42, 46, 54 J Japan 55 Jing (Ching), Emperor 50 Johnson, O.S. 48 Joliot-Curie, F. 55 Joliot-Curie, I. 55 Jones, S.E. 42, 44, 45 journalists 74 Journal of Inorganic Chemistry 29, 73 K kalium 57 kaon(s) 56, 68 Kermesite 6, 7, 15, 16, 21, 27, 68 Kermes mineral 15 khem 49 Khemt 49 Korolev, Y. 75 kupfer-nickel 57 L Large, J. 75 Latin 57 lattice 62 planes 36 Lavoisier, A. 18, 49 Law of Rational Indices, The 63 lead 11, 29, 42, 60-62, 67, 72 acetate 9 antimonate 9 antimonite 9 monoxide 61 nitrate 9 pyro-antimonate 9 titanate 9 Leggett, A.J. 42, 44, 45 Lehn, H. 68 Leibig’s condensor 30 lepton(s) 55, 56 lien chin shu 49 kim shok 49 tan shu 49 lifetime 39, 44, 56, 68 light 44, 54 limestone 61 litharge 29 lithium 41, 60 liu chin 50 Livingstonite 6 London 77 M MacQuillan, S. 74 Mad Scientist Network (MSN) 78 Magnéli, Dr.A. 37 manganese 60 meta-antimonate 5 Manhattan Project, the 55 Mars 15 mass-energy 59 Mercurial Water 12 mercuric chloride 20, 21, 61, 73 iodide 23 meta-antimonate (HgSb2O6) 35, 36, 46, 47, 53, 72, 73, dia 6, 8 oxide(s) (HgO) 6, 13, 16, 20, 22, 23, 35, 37, 53, 57, 66, 71, 72 phosphate 23 pyro-antimonate (Hg2Sb2O7) 1, 4-7, 9, 10, 23, 26, 29, 31, 33, 35-38, 43, 47, 56, 57, 69, 70, 72-74, dia 9, 10 pyro-niobate 35 pyrophosphate 9 sulphate 70, 71 sulphide 6, 50, 71 Mercurius Fixatus 13 mercurous oxide 4, dia 7 gold 47 mercury (Hg) 3, 6, 10-17, 20-23, 27, 28, 30, 32, 35-37, 41-48, 50-54, 57, 60-62, 66, 67, 70-75 -antimony 7 fulminate 13 meta-antimonate(s) 4, 9, 10 nucleus 41 orthophosphate 4 oxide(s) 3, 13, 47 pyro-phosphate 4 salt 26 salt of an oxy-acid of antimony 13 ’sophic’ 16 mesons 55, 56 meta-antimonic acid 2 meta-phosphoric acid 8 military complex 74 military complex 74 Miller indices 63 ‘Mini-Nuke Conspiracy, The’ 28, 40, 41, 74 moderator 43 monoclinic crystal system 5, 6 Montroydite 6, 47 Moseley, H. 26 Multiplication 72 multiplication factor 39 muon(s) 42-44, 46, 56, 68 muonium 68 ‘muriatic acid’ 11 N natrum 57 natural radioactivity 66 Needham, J. 48-52 negative electrode 44 neutral atoms 45, 47, 54 neutrino 68 neutron(s) 2, 27, 38, 39, 41-45, 54, 55, 60, 62, 66-68, 75 bomb 2, 3 cross-section 39, 41, 43 diffraction 26,27 flux 42 flux rate 39 ‘gun’ 41 leakage 39 production 42, 45 radiation 2, 45 rays 63 reflection 41 shield 41 star 66 warhead 41 Newton, I. 11, 49 Nile delta 49 nitrate ions 16 nitrates 16 nitric acid 16, 30, 46, 69 nitrogen 54, 57 non-stoichiometric 37 nuclear bonding 68 bomb 3 fission 40, 41, 44 force 54, 56 fusion 44, 55 interactions 45 physicist 75 nuclear radiation 67 reaction(s) 39, 59 reactor(s) 39, 40 warhead 40 nucleon(s) 56, 59, 66, 67 nucleus(ei) 42, 44, 45, 54, 60, 66, 67 nuclide 59 O octahedra 10, 36, dia 10 octahedral 10 units 37 oil of vitriol 11 orbit 54 orpiment silver 52 ortho-antimonates 10 orthophosphates 8 orthophosphoric acid 8, 23 orthorhombic crystal system 5, 6 oxide(s) 3, 23, 29-31, 36, 37, 41, 47, 52, 53, 59, 72, 73 oxy-acid of antimony 13 oxygen 21, 31, 32, 36, 45, 47, 58, 72, 74, dia 9 P palladium 45 Palmer, E.P. 42, 44 ‘Pao Tsang Lun’, the 51, 52 Paracelsus 12, 13, 17 Partington, J.R. 8 peche-blende 67 Philalethes, E. 16 Philosopher’s Stone (PS) 7, 13, 23, 45, 46, 49, 52, 67 phosphates 8, 10 phosphorus 4, 20, 23, 57 photon(s) 43, 54, 56, 66 piezonuclear fusion 45 pion(s) 56, 68 pitchblende 67 Planck’s constant 25 Pliny 46, 61 plutonium (Pu) 40, 41, 76 Po Choi Pien 52 Pocket Neutron, The 74 polonium 67 Pons 44 positron 55, 66 potassium 23, 57 antimonite 8 potassium aurocyanide 61 carbonate (potash) 13, 22, 57 cyanide 61 dichromate 7, dia 2 hydroxides 70 lead cyanide 61 meta-antimonate 37 powder camera 63 Pretoria 74 Price, Dr. J. 15, 46. 47, 78 Priestley, Dr. H. 18 Principle of the Conservation of Mass, the 56 Promecology 74, 75 proton(s) 39, 42-44, 54, 55, 60, 66, 68 proton-neutron pairs 44 prussic acid 15 Purple of Cassius 46, 52 Pyrargyrite 62 Pyrex glass 73 pyrites 61 pyro-antimonate(s) 9, 10 pyro-antimonic acid 2, 4, 7, 8, 28, 30, 56, dia 2 pyrochloreite 9, 10 pyrochromate ions dia 7 pyrophosphoric acid 8 pyroxenes 5 Q quantum mechanics 66 quark(s) 55, 56, 59 quicksilver 13 quintessence 7, 12 R radioactive 45, 46, 67 radioactivity 55, 66 radium 54, 67 radon 67 reagents 69 ‘realgar silver’ 52 red cinnabar 48 Red Mercury (RM) 2, 3, 7, 11, 27, 40, 41, 74-78 red mercury 48 Ripley, G.15, 69, 71-73 Ripley Wheel, The dia 8 Romans, the 46, 52, 61 Roosevelt, F.D. 55 Rosicrucians 14 Royal Society, The 15, 46, 47 Royal Swedish Academy of Science 37 ruby-glass 52, 73 Rudolph, Emperor 14 Russia 74-76 Russian 38, 70, 74, 75 Rutherford, Prof. E. 18, 55 S Sadykov O. 38, 75 Salt 54 Saxony 14 scattering angles 33 ‘Sceptical Chymist, The’ 49 Scheele, C. 18 Schlippe’s salt 22 Schweitzer, Dr. J. 14 ‘Science and Civilisation in China’ 48 Senarmonite 6 Sendivogius, M. 14, 67 Seres, the 52 Seton, A. 13, 14 silicates 24 silver 13, 46-48, 50-52, 60-62, 67, 71, 72 amalgam 61, 72, 73 antimonide 47 chloride 61 nitrate 61 sulphide 62 Sleight, Dr. A. 3, 28, 29, 33, 35-37, 52, 73 soda glass 23, 72 Soddy, F. 18 sodium chloride 22 hydroxide 22 peroxide 3, 21 thioantimonate 22 South African 74 Standard Model, the 44 Stibiconite 6, 7 stibine 62 Stibnite 6, 7, 12, 16, 17, 47, 50, 52, 57, 70 stoichiometric 37 stoichiometry 37 Stone, the 23 Strasbourg 13 Strasner, F. 55 strong acid(s) 47, 61, 70 strong nuclear force 54, 56, 59 structure amplitude 26 Structure Factor 33 sulphate ions 70 sulphide ions 16, 69, 70 sulphide(s) 3, 50, 51, 53, 69-71 Sulphur 54 sulphur 11, 12, 50, 52, 57 sulphuric acid 70, 71 sulphurous acid 70 Sumeria 24, 52 Sunday Star 74 superconductors 35 Swedish 35 Syrians 49 Szechuan 52 T tantalum 60 tantalum pyrochlores 37 technetium 54 tetragonal crystal structure 5 Textbook of Inorganic Chemistry 28 thallium 46 Thang dynasty 51, 52 Thang Liu Tien 51 Thomson, J. 12 Thomson, J.J. 54 titanium oxides 37 transmutation(s) 18, 19, 42, 45, 46, 49, 55, 59, 66, 78 transmuting powder 24 Tria Prima 54 triclinic crystal system 5 trirutile dia 6 Trismosin, S. 12, 13 tritium 42 Tsou Yen 48 U uranium 40, 55, 67, 76 V Valentine, B. 12, 48, 62 Valentinite 6 vanadates 10 vanadium oxides 37 pyrophosphates 37 Van de Waals forces 38 Van Helmont 14, 24 Venus 15 Vermilion 16 Vincent of Beauvais 19 vitriol, oil of 11 W Warring States (Chan Kuo) period 50 Weast, R.C. 28 Well’s Structural Inorganic Chemistry 29 Wen, Emperor 50 William III 15 Wu, Emperor 51 X xenon 57 X-ray crystallography 37 X-ray(s) 25, 26, 33, 63-65 X-ray diffraction 25, 27 Y Yeltsin, B.N. 74 Z zirconium 37