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Gemmology TheJournal of - GEMMOLOGICAL ASSOCIATION OF GREAT BRITAIN - Gem-A
Volume 21 No. 4.                   October 1988

                   The
                    Journal of
                   Gemmology

GEMMOLOGICAL ASSOCIATION OF GREAT BRITAIN
Gemmology TheJournal of - GEMMOLOGICAL ASSOCIATION OF GREAT BRITAIN - Gem-A
OFFICERS AND COUNCIL

                President: *Sir Frank Claringbull, Ph.D., E l n s t P , FGS
                          Vice-President: R. K. Mitchell, FGA
                           Chairman: *D. J. Callaghan, FGA
                          Vice-Chairman: *N. W Deeks, FGA
                        Honorary Treasurer: *N. B. Israel, FGA

                               Members elected to Council:
*A. J. Allnutt, M.Sc,              J. W Harris, B.Sc,               *J. B. Nelson, Ph.D.,
 Ph.D., FGA                            M.Sc, Ph.D.                 FRMS, E l n s t E , FGA
*E. M. Bruton, FGA             J. A. W Hodgkinson, FGA                W Nowak, CEng.,
*C. R. Cavey, FGA                  D. Inkersole, FGA                      ER.Ae.S., FGA
 E J. E. Daly, B.Sc,                 B. Jackson, FGA                  M. J. O'Donoghue,
 FGA                          *E. A. Jobbins, B.Sc, G Eng.,               MA, FGS, FGA
*A. E. Farn, FGA                       FIMM, FGA                     *P G. Read, CEng.,
 A. J. French, FGA             *G. H. Jones, B.Sc, Ph.D.,          MIEE, MIERE, FGA
 G.Green, FGA                              FGA                         *K. Scarratt, FGA
*R. R. Harding, B.Sc,                D. G. Kent, FGA                       E. Stern, FGA
 D. Phil, FGA                      D. M. Larcher, FGA                *C. H. Winter, FGA
                               A. D. Morgan, FIBF, FGA

^Members of the Executive Committee

                                  Branch Chairmen:
                           Midlands Branch: J. Leek, FGA
                         North-West Branch: R. Perrett, FGA
                 South Yorkshire & District Branch: G. A. Massie, FGA

                                   Examiners:
A. J. Allnutt, M.Sc., Ph.D., FGA                                        D. G. Kent, FGA
E. M. Bruton, FGA                                             P Sadler, B.Sc, FGS, FGA
A. E. Farn, FGA                                                         K. Scarratt, FGA
R. R. Harding, B.Sc, D.Phil., FGA                           M. Virkkunen, M.Phil., FGA
E. A. Jobbins, B.Sc, C.Eng., FIMM, FGA                        C. Woodward, B.Sc, FGA
G. H. Jones, B.Sc, Ph.D., FGA

                   Editor: E. A. Jobbins, B.Sc, C.Eng., FIMM, FGA
                          Editorial Assistant: Mary A. Burland
                               Curator: C. R. Cavey, FGA
                     Secretary: Jonathan P Brown, FGA, Barrister

               Saint Dunstan's House, Carey Lane, London EC2V 8AB
              (By Goldsmith's Hall)            Telephone: 01-726 4374
Gemmology TheJournal of - GEMMOLOGICAL ASSOCIATION OF GREAT BRITAIN - Gem-A
TheJournal of
Gemmology
                    VOLUME 21
NUMBER FOUR                            OCTOBER 1988

                      Cover Picture
   The Airoldi Chalice; silver and gold plate, decorated with red
  coral carved as angel and cherub heads and leaf motifs. Sicilian
            workmanship, XVII century; height 230mm.
               Photograph courtesy CISGEM, Milan

                         ISSN: 0022-1252
Gemmology TheJournal of - GEMMOLOGICAL ASSOCIATION OF GREAT BRITAIN - Gem-A
210

          The .
          Buckingham
             Award
             Award
         Mr   w.e. Buckingham,
         Mr W.C.    Buckingham, FGA,  FGA, hashas very
                                                  very generously
                                                         generously
      donated his
      donated    his fine
                      fine collection    of zircon
                             collection of   zircon rough
                                                       rough to
                                                              to the
                                                                 the
      Gemmological       Association of
      Gemmological Association          of Great
                                           Great Britain    to mark
                                                   Britain to  mark
      his retiral
      his  retiral after  fifty years
                   after fifty  years from
                                       from thethe firm   of George
                                                    firm of  George
      Lindley &
      Lindley       Co. Ltd.
                 & Co.   Ltd. HeHe is
                                    is also
                                       also offering
                                             offering anan award
                                                           award toto
      newly-qualified
      newly-qualified Fellows of the Association who
      carry  out research
      carry out   research on on samples
                                 samples from      the collection.
                                            from the    collection.
         The criteria for the research are:
      1. The rough specimens originate from various
      1.
         localities, mostly Indo-China, and the research
         might be
         might   be directed
                     directedtowards
                                towardsdetermining
                                           determining     any
                                                         any    vari-
                                                             variation
         ation in properties from the different
                                              different localities.
         However, other
                      otherresearch
                               researchtopics
                                          topics   would
                                                would       be con-
                                                        be considered.
         sidered.
      2. Having carried out the research programme, the
         Fellow must present the results in the form of a
         paper which would, in the opinion of the Editor,
         be worthy of    of publication in The Journal   Journal ofof
         Gemmology.
         Gemmology.

                                             3. A Fellow whose research and paper satisfy
                                                                                        satisfy these
                                                criteria will be awarded the sum of £100 or books
                                                and/or instruments to that value.
                                             4. The Fellow must first apply in writing to the
                                                Secretary ofof the Association, setting out his
                                                proposed research and methodology and the
                                                instruments he proposes to use. The time to be
                                                taken must also be specified.
                                                                      specified.
                                                Research materials provided by the Association
                                             must be returned within the time stipulated.
                                                The Association reserves the right to authorize or
                                             reject research projects at its sole discretion and will
                                             not enter into the reasons for any decision made.
                                                Those interested in the Award are invited to write
                                             to the Secretary of of the Gemmological Association,
                                             Saint Dunstan's House, Carey Lane, London EC2V
                                             8AB, giving the information
                                                               information set out in item 4 above.
Gemmology TheJournal of - GEMMOLOGICAL ASSOCIATION OF GREAT BRITAIN - Gem-A
J. Gemm., 1988,21,4
          1988,21,4                                                                                                       211
                                                                                                                          211

                                    Imitation pearl coatings

                               S.J.
                               S.J. Kennedy*,J.G.
                                    Kennedy* J.G. Francis**
                                                  Francis** andG.C.Jones**
                                                            and G.C. Jones**

                                                             27 Greville Street, London ECIN
                   *Gem Testing Laboratory of Great Britain, 27                         E O N 8SU.
                    **Dept. of Mineralogy, British Museum (Natural History), London SW7 SW7 5BD.
                                                                                             5BD.

Abstract                                                           that these were not nacreous pearls. The radio-
   The coating on an imitation pearl was studied by a              graph (Figure 2) shows that the 'pearl' consists of a
variety
variety of techniques.
           techniques. The
                        Thenacreous
                             nacreouseffect
                                       effectof
                                              ofthe
                                                 thecoating
                                                     coat-         bead that is partly transparent to X-rays, sur-
was   found
ing was       to to
          found  be bedue
                        duetotominute
                                 minute platy
                                         platy hexagonal
                                                hexagonal          rounded by an X-ray opaque coating. This
                                                                                                          This coating
crystals of basic lead carbonate suspended in a clear              shows up as a lighter rim to the greyish disc of the
nitrocellulose lacquer. The form of the crystals was               bead.
studied by scanning electron microscopy while their
composition was revealed by infrared
                               infrared spectroscopy and                   information would normally be sufficient,
                                                                     This information                        sufficient,
electron microprobe analysis.                                      and a report would be issued to the effect
                                                                                                        effect that the
                                                                   beads were imitation pearls. However, in this case,
                                                                   because questionable claims had been made about
Introduction                                                       the composition ofof the imitation pearls, it was
                   ungraduated bracelet of
   A single-row, ungraduated               of 24 'pearls'                        identify the materials used in their
                                                                   necessary to identify
and 6 round, black beads with 3 colourless, stone-                                                subjected to further
                                                                   manufacture. One 'pearl' was subjected       further
set metal spacers (Figure 1) was submitted to the                  examination.
                                                                   examination.
Gem Testing Laboratory
                Laboratory of  of Great Britain by a
trading standards authority with the request to test               Glass bead
both beads and 'pearls'.
                  'pearls:                                                            formed the body of
                                                                      The bead which formed             of the 'pearl'
   Identification  of the black beads as onyx was not
   Identification of                                                                                 diffraction and
                                                                   was found to be glass by X-ray diffraction
difficult
difficult - the X-ray powder diffraction
                                    diffraction pattern                                                            of
                                                                   electron microprobe techniques. The only point of
obtained was that of of quartz. A cursory examination              interest here was that the glass was semi-
of
of the pearls with a lOx loupe showed a form of    of the          transparent to X-rays, whereas coated imitation
                                                                   transparent
granular structure typical of   of imitation
                                   imitation pearls. A             pearls have tended to be made ofof a glass that is
radiograph ofof the necklace demonstrated
                                 demonstrated clearly              opaque
                                                                   opaque to X-rays. This difference
                                                                                                difference can be

Fig. 1.
     I. Imitation
        Imitation pearl and onyx bead
                                   bead bracelet
                                         bracelet - the milky
                                                          milky    Fig. 2. Radiograph of
                                                                                      of imitation
                                                                                         imitation pearl from bracelet.
        white bead next
                   next to an onyx bead (top right)
                                             right) is the
                                                       the glass
        bead from
              from which the nacreous coating
                                         coating has been
                                                       been re-
                                                             re-
        moved.

© Copyright
© Copyright the Gemmological
                Gemmological Association                                                                      ISSN: 0022-1252
Gemmology TheJournal of - GEMMOLOGICAL ASSOCIATION OF GREAT BRITAIN - Gem-A
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Fig . 3. X-ray powder diffraction patterns of: (top) material coating imitation pearl ; (middle) commercial grade 'white lead'; (bott om) hydrocerussitc ; Ashover, Derbyshire, UK .
                                                                                                                                                                                       -
Gemmology TheJournal of - GEMMOLOGICAL ASSOCIATION OF GREAT BRITAIN - Gem-A
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        Scanning
Fig. 4. Scan      electron
             ning electro n microscope image of                      imitation
                                             of nacreous filler from imit              coating (left)
                                                                          ati on pearl coaling                       SOOOx.
                                                                                               (left) 2000x, (right) 5000x.   W
                                                                                                                              W
Gemmology TheJournal of - GEMMOLOGICAL ASSOCIATION OF GREAT BRITAIN - Gem-A
214                                                                                             J. Gemm., 1988,21,4

accounted for by the relatively low lead content         Further background
(approx. 1% PbO) as found by electron microp-               After these investigations were completed, M.
robe analysis.                                           Jean Paul Poirot presented a paper at the Interna-
                                                         tional Gemmological Conference in Brazil in 1987
Coating                                                  entitled 'Imitation pearls and their coatings'. He
   The X-ray powder diffraction pattern of the           noted the following crystalline materials as being
pearl coating obtained at the Gem Testing Labora-        present in the nacreous coatings of imitation pearls
tory (Figure 3a) was close to that of the mineral        and visible on microscopic examination of an
hydrocerussite (Figure 3c), but did not match it         acetone extract of the coating:
exactly. The use of hydrocerussite as an imitation
pearl coating has been documented1, but the              (1) rods of guanine approx. 5 x 30 micrometres -
anomaly in the diffraction photograph led us to          this is a component of the well-known 'essence of
pursue the matter further, using a variety of techni-    orient' extracted from fish scales and one of the
ques available at the Department of Mineralogy,          longest-used pearl simulants; or
BM(NH).                                                  (2) square plates of bismoclite (bismuth oxychlor-
   An infrared spectrum of the coating material          ide) approx. 10 micrometres across - this com-
showed a mixture of nitrocellulose and another           pound is also used in 'pearl' cosmetics such as nail
component. During an unsuccessful attempt to             varnish, etc.; or
dissolve the coating in dichloroethane, it separated     (3) hexagonal plates of hydrocerussite approx. 15
into two layers, i.e. a nitrocellulose 'sandwich' with   micrometres across; or
nacreous inner surfaces. Acetone dissolved the           (4) fragments of mica crystals, sometimes coated
nitrocellulose lacquer completely and allowed            with titanium dioxide.
further infrared spectra to be run on the separated
soluble and insoluble materials (approx. 56 wt%          Conclusion
insol.). These spectra confirmed the identification         The imitation pearls in question are coated with
of nitrocellulose and a hydrocerussite-like filler.      a synthetic, basic lead carbonate in the form of
Under the optical and scanning electron micro-           minute hexagonal plates, suspended in and coated
scopes, the acetone-insoluble nacreous filler            by clear nitrocellulose lacquer.
appeared as minute hexagonal plates of average              The anomalies in the X-ray powder diffraction
size 15 x 0.25 micrometres (Figure 4). These             patterns and infrared spectra are the result of the
plates were also examined in the electron microp-        variable nature of the basic lead carbonate, the
robe, which revealed lead as the only detectable         exact composition of which depends on its method
element (elements lighter than sodium are not            of production.
detectable by this instrument).
   Hydrocerussite or lead dihydroxydicarbonate
has been produced synthetically by many different
methods, some of which are quoted as giving rise
to hexagonal nacreous plates2.
   The exact chemical composition of these synthe-
tic products is in doubt, as is the composition of       References
the pigment 'white lead' which is another form of        1. Webster, R., 1983, Gems, their sources, descriptions and
hydrocerussite3. A specimen of white lead gave an           identification. Butterworths, London. 557 pp.
X-ray diffraction pattern and an infrared spectrum       2. Mellor, J.W ., 1930. A comprehensive treatise on inorganic and
                                                            theoretical chemistry, VII, 836-9.
both of which matched much more closely those of         3. Ibid. 846-7.
the pearl material than the mineral hydrocerussite
(see X-ray patterns, Figures 3b & 3c).                   [Manuscript received 3 July 1988.]
Gemmology TheJournal of - GEMMOLOGICAL ASSOCIATION OF GREAT BRITAIN - Gem-A
J. Gemm.,1988,21,4                                                                                                          215

                      Alexandrite: natural or synthetic?
                            H. Bank*, E. Gübelin**,              U. Henn* and J. Malley†

                                              *Idar-Oberstein, West Germany
                                                  **Meggen, Switzerland
                                                  †Mainz, West Germany

   Since the appearance on the market of great                    the presence of chromium lines. Yet the question
quantities of rough and faceted alexandrites from                 of natural versus synthetic still remained unsolved.
Brazil (Bank et al, 1987a; Bank et al, 1987b;                        Microscopically, step-like growth striations were
Gübelin and Schiffmann, 1988), the differentiation                observed - which are also no indication of natural
between these (to a great extent relatively inclu-                origin - as well as 'fingerprint-feathers' of bizarre-
sion-free) gemstones, and synthetic alexandrites,                 shaped cavities (Figure 1). Some of the latter
has naturally been pushed into the foreground of                  contained a solid substance which between crossed
gemmological investigations. Recently a dark                      polars displayed interference colours, and was thus
green-to-violet changing to red-violet stone of 1.34              founded to be doubly-refractive. With overhead
ct (faceted, oval, 7.2 x 6.4 x 3.5 mm) arrived for                illumination, these inclusions reflect strongly (Fi-
investigation, which had been identified by a                     gure 2) and are thus reminiscent of the flux
laboratory as a synthetic alexandrite. Yet the owner              residues in synthetic alexandrite (Gübelin and
of the stone doubted this outcome, since he had                   Koivula, 1986, Trossarelli, 1986, Henn, 1987).
purchased it personally in the rough at the mine in                  Several inclusions were exposed to the surface of
Brazil and had also cut it himself (which, however,               the faceted stone, allowing further investigations as
does not prove that it is genuine).                               to their identity with the help of more sophisti-
   The stone was doubly-refractive on the polari-                 cated methods. Qualitative energy-dispersive
scope and biaxial on the conoscope. The standard                  analyses with the aid of a scanning electron micro-
gemmological values were as follows:                              scope (SEM), identified very diverse substances in
n x = 1.745, n y = 1.748, n z = 1.754, A n = 0.009,               the fissures surrounding the exposed inclusions.
D = 3.71 g/cm3.                                                   Figure 3 shows such an area of fissures; the white
These all indicate the mineral variety chrysoberyl                streak measures 50 /mi. The white spherical grain
(BeAl 2 0 4 ), which crystallizes in the orthorhombic             could be identified as tin. Similar solid substances
system. With the aid of spectroscopic analyses, the               present in these fissures proved to be copper,
stone could be identified as an alexandrite through               nickel and lead. Lead-oxide was detected by means

    1. Bizarre-shaped cavities, partly filled with solid subst    Fig. 2. Bizarre-shaped cavities, partly filled with solid subst-
       ance. 15x.                                                         ance. Reflected light. 20x.

© Copyright the Gemmological Association                                                                      ISSN: 0022-1252
Gemmology TheJournal of - GEMMOLOGICAL ASSOCIATION OF GREAT BRITAIN - Gem-A
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                                                                                                                                                                                                                                                                                                                             -
216                                                                                                                                                                                                                                                                                                         J. Gemm., 1988,21. 4

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         ::   ::::                              :::.:::                                                                                              :::   :   •••   ••••••••   0   •   ••   ••   ••
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J.J.Gemm.,
    Gemm., 1988,21,4
           1988,21,4                                                                                                           217
                                                                                                                                217

                                                                discs, which
                                                               discs,   which were
                                                                              were forced
                                                                                    forced into
                                                                                            into the
                                                                                                  the fissures
                                                                                                       fissures during
                                                                                                                during
                                                                theseprocesses.
                                                               these   processes.
                                                                  AAmore
                                                                      more precise
                                                                             precise investigation
                                                                                      investigation ofofthe
                                                                                                         the solid
                                                                                                              solid fillings
                                                                                                                     fillings
                                                                of these
                                                               of   these fît
                                                                           fitsures   revealed the
                                                                              sures revealed    the presence
                                                                                                      presence ofof potas-
                                                                                                                      potas-
                                                                sium-rich aluminium
                                                               sium-rich      alarninium silicates
                                                                                           silicates -- probably
                                                                                                         probably potas-
                                                                                                                      potas-
                                                                siumfeldspar
                                                               sium   feldspar(Figure     4). This
                                                                                 (Figure4).   Thisdefinitely
                                                                                                    definitelyproves
                                                                                                                proves thethe
                                                                naturalorigin
                                                               natural   originofofthe
                                                                                    thestone.
                                                                                        stone.

                                                                Acknowledgements
                                                               Acknowledgements
                                                                  Scanning electronic
                                                                  Scanning    electronic microscope
                                                                                          microscope analyses
                                                                                                        analyses were
                                                                                                                   were
                                                               carried
                                                                carriedout
                                                                        outatatthe
                                                                                theMax-Planck-Institut
                                                                                   Max-Planck-Institutfür fur Chemie,
                                                                                                               Chernie,
                                                                Abt. Kosmochemie,
                                                               Abt.     Kosmochernie, Mainz,
                                                                                           Mainz, West-Germany.
                                                                                                       West-Germany.
                                                                Financial support
                                                               Financial   support waswas given
                                                                                           given by by grants
                                                                                                       grants ofof the
                                                                                                                    the
                                                                Wirtschaftsrninisterium des
                                                               Wirtschaftsministerium      des Landes
                                                                                                 Landes Rheinland-
                                                                                                           Rheinland-
                                                               Pfalz,
                                                                Pfalz,FRG,
                                                                       FRG,within
                                                                              withinaaproject
                                                                                       projectfor
                                                                                               forapplied
                                                                                                   applied research.
                                                                                                            research.

                                                               References
                                                               References
                                                                Bank,H.,
                                                               Bank,    H.,  Henn,
                                                                          Henn,   U. &U.Bank,
                                                                                          & Bank,     F.H., 1987a.
                                                                                               EH., 1987a.           EinAlexandritvorkommen
                                                                                                              Ein neues   neues Alexan-
                                                                     dritvorkommenininBrasilien.
                                                                                            Brasilien.Goldschmiede
                                                                                                         GoldschmiedeZeitung,      Heft 9,9,
                                                                                                                        Zeitung, Heft
                                                                     90-1.
                                                                    90-1.
                                                                Bank,F.H.,
                                                               Bank,    F.H.,  Bank,
                                                                            Bank,   H., H., Gube1in,
                                                                                        Gübelin,         E., Henn,
                                                                                                  E., Henn,          U. Alexandrite
                                                                                                             U. 1987b.   1987b. Alexan-
                                                                           von einem
                                                                     dritevon    einemneuen
                                                                                         neuen Vorkommen
                                                                                                 Vorkommenbei    beiHematita
                                                                                                                     Hematitainin Minas
                                                                                                                                    Minas
                                                                     Gerais, Brasilien.
                                                                    Gerais,   Brasilien. Zeitschrift
                                                                                          Zeitschrift der
                                                                                                        derDeutschen
                                                                                                            Deutschen Gemmologischen
                                                                                                                        Gemmologischen
                                                                                    36,121-31.
                                                                     Gesellschaft,36,
                                                                    Gesellschaft,        121-31.
                                                                Gube1in, E.,
                                                               Gübelin,     E., Koivula,     J.I., 1986.
                                                                                  Koivula, J.I.,    1986. Photoatlas
                                                                                                            Photoatlas ofof inclusions
                                                                                                                             inclusions inin
                                                                    gemstones.ABC
                                                                   gemstones.     ABCEdition,
                                                                                        Edition, Zürich.
                                                                                                   Zurich.
                                                                Giibelin, E.,
                                                               Gübelin,     E., Schiffmann,
                                                                                  Schiffmann, C.A.,
                                                                                                  C.A., 1988.
                                                                                                           1988. Alexandrite
                                                                                                                   Alexandrite from
                                                                                                                                  from aa
                                                                     Newly Discovered
                                                                   Newly      Discovered Occurrence
                                                                                             Occurrence in   in Brazil.
                                                                                                                 Brazil. Schweizerische
                                                                                                                          Schweizerische
                                                                     Uhrmacher und
                                                                    Uhrmacher      und Goldschmiede
                                                                                        Goldschmiede Zeitung,       International issue,
                                                                                                          Zeitung, International     issue,
                                                                    2/ 1988.
                                                                   2/1988.
Fig. 3.3. SEM-photograph:
Fig.      SEM-photograph: fissure
                           fissurewith
                                  withsolid
                                       solid substances.
                                              substances.       Henn, U.,
                                                               Henn,    U., 1987.
                                                                             1987. Inclusions
                                                                                    Inclusionsinin yellow
                                                                                                      yellowchrysoberyl,
                                                                                                              chrysoberyl, natural
                                                                                                                              natural and
                                                                                                                                       and
                                                                    syntheticalexandrite.
                                                                   synthetic     alexandrite.Australian
                                                                                               AustralianGemmologist,
                                                                                                            Gemmologist, 16,16,217-20.
                                                                                                                                217-20.
                                                                Trossarelli,C.C.(1986):
                                                               Trossarelli,       (1986):  Synthetic
                                                                                        Synthetic       alexandrite
                                                                                                    alexandrite fromfrom
                                                                                                                      USSR. USSR.    Gem-
                                                                                                                               Gemmologia,
ofthe
of  the Raman
        Raman spectroscope.
                 spectroscope. The The latter
                                         latter was
                                                was quoted
                                                      quoted        mologia, ll, 6--22.
                                                               11, 6-22.
as proof
as proofthat
          that the
                the investigated
                     investigated stone
                                     stone was
                                            was aa synthetic
                                                   synthetic
alexandrite. These
alexandrite.  These spherical
                       spherical metal
                                   metal grains,
                                           grains, however,
                                                    however,
 were not
were   not securely
            securely lodged
                       lodged in in the
                                     the fissures,
                                          fissures, and
                                                     and are
                                                         are
 probably remnants
probably   remnants left     by the
                        left by  the cutting
                                      cutting or
                                               or polishing
                                                   polishing                 received 33May
                                                                [Manuscript received
                                                               [Manuscript              May /988.]
                                                                                             1988.]
218                                                                                                  J. Gemm., 1988,21,4

              A
              A new type of twinning in natural
                                        natural sapphire
                                                    Dr Karl
                                                    Dr Karl Schmetzer
                                                             Schmetzer

                    Institute of Mineralogy and Petrography, University of Heidelberg, West Germany

Abstract                                                              never in synthetic rubies or sapphires of different
                                                                                                                    different
   A new type of twin structure in natural sapphire                   producers.
from Sri
from    Sri Lanka
             Lanka isisdescribed.
                        described.TheThesamples
                                             samplesreveal
                                                       revealinserted
                                                               in-       The new type of twin structure was observed in
serted   irregularly
   irregularly        shaped
                 shaped       bodies
                         bodies         of subordinate
                                  of subordinate          corun-
                                                      corundum        the course of microscopical examination of some
dum individuals, which are confined to intercalated
                                                                      hundreds of light yellowish or bluish untreated
lamellae parallel to rhombohedral faces r (lOll)      (1011) and
related to the dominant crystal by reflection across                  (i.e.  non-heat treated) natural sapphires from Sri
(1011).
(1011).                                                               Lanka. In about 50 of these cabochon cut samples,
                                                                      bodies of corundum crystals were found to occur
                                                                      in an orientation different
                                                                                            different from the dominant
   In some cases, the recognition of certain types of                                                      different crystal-
                                                                      sapphire individual. Due to their different
twinning in ruby and sapphire is applicable to the                    lographic orientation, these corundum crystals in-
distinction of natural and synthetic corundum. In                     serted into the dominant individual are clearly
general, aadetailed
               detailed   knowledge
                       knowledge    about   about
                                              twin twin   struc-
                                                    structures        recognizable under crossed polarizers, but not in
tures occurring in natural ruby and sapphire as                                                          1-6). Part of these
                                                                      plane polarized light (Figures 1-6).
well as in different
              different types of synthetic corundum is                inserted bodies reveal only irregular surfaces as
necessary in order to avoid misinterpretations of                     boundaries between dominant and subordinate
structuralproperties
structural    propertiesduring
                            during   microscopic
                                 microscopic           examina-
                                                   examination        corundum individuals (Figures 1, 2).  2). Both crystals
tion of samples of unknown origin. A general                          differing in orientation, in general, are not related
                                                                      differing
survey dealing with twin structures in natural                        by reflection
                                                                           reflection across the positive rhombohedron r
rubies    fromdifferent
rubies from                 localitiesis isgiven
                 differentlocalities         givenbyby  Schmet-
                                                     Schmetzer        (lOTl) and, at present, it is unknown to the author
                                                                      (lOTI)
     (1987), and the results described in the paper
zer (l987),                                                           if both parts of the crystals are connected by an
cited are also valid for natural sapphires without                    unknown twin law or not-not.
any restriction.
      restriction.Twinning
                     Twinningininflux-grown
                                    flux-growngem    gem  quali-
                                                        quality          Samples of the second part of sapphire crystals
ty synthetic ruby and sapphire was described in                       with inserted bodies of corundum reveal at least
detail byby Schmetzer
             Schmetzer(1987)       andKiefert
                           (l987)and       Kiefert&&    Schmet-
                                                     Schmetzer        one plane surface as boundary between dominant
zer(1988).
     (l988).                                                          and subordinate individuals (Figure 3). A thor-
   In natural corundum, three types of twinning                       ough microscopic examination indicates that, in all
are observable: contact twins on the basal plane c                    cases, these contact planes are parts of intercalated
(0001) or on the positive rhombohedron r (lOTI)           (lOTl)      lamellae on r (lOTI)
                                                                                      (1011) [Figures 4, 5, 6].
                                                                                                            6]. The remain-
with two macroscopically developed individuals      individuals       ing boundaries between main crystals and inserted
are rare. Repetitive twinning on r (lOTI),      (lOTl), on the        irregular bodies, i.e. those boundaries which are
other hand, is common in natural ruby and sap-                              confined to an intercalated lamella on r, may
                                                                      not confined
phire but, in general, only thin lamellae of corun-                   consist of either irregular surfaces or of plane
dum in twin position are intercalated parallel to                                             3-6).
                                                                      crystal faces (Figures 3--6).
one, two or three rhombohedral faces of the domi-                        In part of the crystals investigated, up to five
nant ruby or sapphire crystal. In some samples,                       inserted bodies of corundum were observed, which
intercalated lamellae were found to end irregularly                   are confined
                                                                            confined to several intercalated lamellae para-
within the dominant corundum individual. The                          llel to one rhombohedral face r (lOTI).(lOTl). In two
new type of twin structure to be described in this                    samples, inserted bodies of corundum in twin
            confined to intercalated lamellar twinning
paper is confined                                                                                      confined to interca-
                                                                      position were found which are confined
       (lOTl). Up to now, twinning of this particular
on r (lOll).                                                          lated lamellae parallel to two rhombohedral faces r
type was observable only in natural corundum, but                     andr'r' {lOTI}.
                                                                      and      {lOTl}.

©
© Copyright the Gemmological Association                                                                 ISSN:
                                                                                                         ISSN: 0022-1252
J. Gemm., 1988,21,4                                                                                                         219

Figs. 1, 2. Natural sapphire from Sri Lanka; inserted bodies of corundum revealing irregular surfaces as boundaries between
            subordinate crystals and the dominant individual. Fig. 1, plane polarized light; Fig. 2 crossed polarizers. lOOx.

Fig. 3. Natural sapphire from Sri Lanka; inserted bodies of      Fig. 4. Natural sapphire from Sri Lanka; inserted body of
        corundum revealing plane boundaries between domi-                corundum [below] confined to an intercalated lamella
        nant and subordinate individuals. Crossed polarizers.            on the positive rhombohedron r (1011) [above] as
        30x.                                                             boundary between dominant and subordinate indi-
                                                                         viduals. View almost perpendicular to the intercalated
                                                                         lamella, crossed polarizers. 20x.

Fig. 5. Natural sapphire from Sri Lanka; inserted body of        Fig. 6. Natural sapphire from Sri Lanka; inserted bodies of
         corundum confined to an intercalated lamella on the             corundum confined to an intercalated lamella on the
         positive rhombohedron r (10Ï1) as boundary between              positive rhombohedron r(1011)as boundary between
        dominant and subordinate individuals. View parallel to           dominant and subordinate individuals. View almost
        the intercalated lamella, crossed polarizers. 20x.               parallel to the intercalated lamella, crossed polarizers.
                                                                         40x.
220                                                                                        J. Gemm., 1988,21,4

   According to its properties, the new type of twin   References
structure in corundum
               corundum described combines both        Kiefert, L., Schmetzer, K., 1988. Morphology and twinning in
single types of rhombohedral twinning, i.e. contact       Chatham synthetic blue sapphire. Journal
                                                          Chatham                            Journal of
                                                                                                      of Gemmology,
                                                                                                         Gemmology,
                                                          21, 16-22.
                                                          21,16-22.
twinning on r (lOTI)
                (lOTl) [consisting of two macrosco-    Schmetzer, K. 1987. On twinning in natural and synthetic
pically developed individuals] and lamellar twin-         flux-grown ruby. Journal
                                                          flux-grown                of Gemmology, 20, 294-305.
                                                                           Journal of
ning on r (lOTI)                of intercalated thin
             (1011) [consisting of
lamellae]. Consequently, this type of twinning is
classified as combined rhombohedral twinning.
classified                                             [Manuscript received 22 February
                                                       [Manuscript received    February 1988.]
                                                                                         1988.]

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                               Gemmological
                               Gemmological Associa  tion of
                                              Association of Grea
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J. Gemm., 1988,21,4

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                      Cables: Geminst, London EC2
222                                                                                                         J. Gemm., 1988,21,4

                                An unusual ruby from Nepal*
          H. Bank1, E. Gübelin2, R.R. Harding3, U. Henn1, K. Scarratt4 andK.                                Schmetzer5
                            1
                            Deutsche Stiftung Edelsteinforschung, Idar-Oberstein, West Germany
                                                    2
                                                     Meggen, Switzerland
                                         3
                                          British Museum (Natural History), London
                                   4
                                     The Gem Testing Laboratory of Great Britain, London
                    5
                      Institute of Mineralogy and Petrography, University of Heidelberg, West Germany

Abstract                                                                 Introduction
   A high quality ruby from Nepal is described. The                        A purely gemmological routine investigation can
stone, weighing 1.288ct, revealed extraordinary growth                   sometimes result in a false diagnosis, or at least
structures connected with colour zoning as well as                       create difficulties, especially when the problem
mineral inclusions (phlogopite), feathers consisting of
two- and most probably three-phase inclusions and                        concerns the differentiation between natural gems
ultra-fine fluid films, as diagnostic characteristics.                   and synthetic stones. This is particularly so if the
                                                                         inclusions observed are not clearly indicative, but

Figs 1 and 2. Growth structures and colour zoning in a natural ruby from Nepal; view aimost perpendicular to the c-axis; broad
              alternate colourless and red bands parallel to the basal pinacoid c (0001) forming the lower edge of the sample,
              colourless parts confined to growth structures parallel to the hexagonal prism a (1120) on the left side of the sample
               and parallel to the hexagonal dipyramid v (4481) on the right of the sample, spindle-like growth structures in the
              dark red central part of the stone. Transmitted light using methylene iodide as immersion liquid. 22x. (Photos by K.
              Schmetzer.)

 *The Editor received two papers on this subject on the same day. They
have been combined to form this paper.

© Copyright the Gemmological Association                                                                        ISSN: 0022-1252
J. Gemm., 1988,21,4                                                                                                           223

Fig. 3. Growth structures and colour zoning in a natural ruby      Fig. 4. Spindle-like growth structures in the dark red central
        from Nepal; view almost perpendicular to the c-axis;               part of a natural ruby from Nepal; view almost perpen-
        growth structure parallel to the hexagonal prism a                 dicular to the c-axis. Transmitted light using methylene
        (1120) visible as boundary between colourless edge and             iodide as immersion liquid. 25x. (Photo by K.
        dark red central part, spindle-like growth structures in           Schmetzer.)
        the central part, parallel to the basal face c (0001).
        Transmitted light using methylene iodide as immersion
        liquid. 30x. (Photo byK. Schmetzer.)

ambiguous, i.e. if they could be found in both                     which had not been observed previously in
natural and synthetic stones and are not typical of                Nepalese rubies. So the stone was examined in
either. This happened recently during the inves-                   detail using spectroscope, microprobe and further
tigation of a faceted red stone, whereby the ques-                 microscopic investigations.
tion was raised whether it was a natural or a
synthetic stone, and whether it originated from the                Investigation
Kingdom of Nepal.                                                     The faceted ruby weighs 1.288 ct and is cut as an
   Ruby, as well as pink, violet and purplish sap-                 almost equilateral octagon (6.00 x 6.00 x 4.15
phires, from Nepal were recently described by                      mm). The physical properties of the sample are
Harding and Scarratt (1986) and Kiefert and                        within the range known for both natural and
Schmetzer (1986, 1987). Most of the material                       synthetic ruby, i.e. n 0 = 1.770, n e = 1.762, An =
available until now has been of cabochon quality                   0.008, D = 3.98 g/cm3, and with the hand spectro-
and any faceted samples of notable transparency                    scope the normal chromium spectrum of ruby was
have been few. Thus, the authors were surprised to                 detected.
receive a faceted sample of more than one carat,                      The absorption spectrum of the sample in the
with excellent purity, a good 'Burmese red' colour,                visible and ultraviolet regions, as examined with
and which was said to originate from Nepal. Under                  the aid of a UV/VIS spectrophotometer, is similar
the microscope the ruby revealed characteristics                   to the spectra already published for ruby and
which closely resembled some of the properties                     sapphire from Nepal by Harding and Scarratt
seen in Ramaura and Kashan synthetic rubies and                    (1986) and Kiefert and Schmetzer (1986, 1987),
224                                                                                              J. Gemm., 1988,21,4

but does not
but        not contain    significant Fe 2 ++ /Ti
               contain a significant              4+
                                              ITi4+  charge   observed
                                                              observed previously
                                                                          previously byby the authors
                                                                                                authors in Ramaura
transfer
transfer absorption
          absorptlon in the red
                              red region of  of the visible   synthetic rubies. However, in such
                                                              synthetic                             such stones the
spectrum. Due Due to the absence of     of ironiron and/or    growth
                                                              growth zones forming
                                                                                forming angles ofof 86° are made
                                                                                                               made by
titanium
titanium inin distinct
              distinct amounts, the sample reveals a                different rhombohedral
                                                              two different   rhombohedral faces rrand
                                                                                                     and rr'' (lOTI).
                                                                                                              (lOTl).
good
good ruby
       ruby colour
              colour without
                       without any purplish
                                     purplish hue, i.e.           Many
                                                                  Many ofof the microscopic
                                                                                 microscopic observations
                                                                                              observations disclosed
without
without anan additional
             additional sapphire
                         sapphire component.                   ambiguous features
                                                              ambiguous      features which
                                                                                       which could
                                                                                              could neither
                                                                                                     neither be attri-
                                     immersion liquid,
   Using methylene iodide as an immersion                      buted clearly to a natural
                                                              buted                   natural nor a synthetic ruby.
a microscopic examination of    of the ruby, in a direc-       Amongst the most confusing
                                                              Amongst               confusing characteristics
                                                                                                characteristics of
                                                                                                                 of this
tion normal to the table facet, revealed a dark    dark red    1.288 ct ruby are the spindle-like growth struc-
                                                               1.288
                    well-defined and near-colourless
central area, two well-defined                                tures in the darkdark red central part
                                                                                                  part of
                                                                                                        of the stone.
       situated close to the girdle and on opposite
areas situated                                                These are parallel to the basal pinacoid
                                                                                                   pinacoid c (0001)
       and another
sides and   another area, also bounded
                                 bounded at one edge                                             connected with the
                                                              (Figures 1 and 4), and are connected
by the girdle, in which there was strong colour               colour zoning. These structural
                                                                                        structural characteristics
                                                                                                   characteristics re-
zoning (Figures 1, 2 and 3). In the latter area the           semble features
                                                                        features often
                                                                                  often observed
                                                                                         observed in synthetic flux-
              broad colourless and red zones (Fig-
alternating broad                                             grown rubies.
ures 1 and 2) are parallel to the basal pinacoid                  Both at the girdle and near the culet ofof the stone
c (0001), and the two near-colourless areas form              several small, solid inclusions are exposed at the
        of 90° and 85° respectively, with the growth
angles of                                                     surface. Examination
                                                                         Examination by electron
                                                                                           electron microprobe both
structures
structures connected
            connected with this colour zoning. Con-           in London
                                                                   London and Heidelberg
                                                                                   Heidelberg indicated
                                                                                                indicated that these
sequently, these colour zones are confined    confined to     inclusions are phlogopite (Figure 5), a mica which
growth structures parallel to the hexagonal prism             has already been identified
                                                                                   identified in the paragenesis of   of
a (1l20)
   (1120) and parallel to the hexagonal dipyramid             ruby and rose and violet sapphire from Nepal.
v (4481). Similar almost rectangular growth struc-                Further
                                                                  Further microscopic examination
                                                                                          examination revealed the
tures connected
        connected with colour zoning have been                presence ofof dark 'feathers' consisting of
                                                                                                       of small more

                       A/IV.., SiK,;..

                   Mgl
J. Gemm., 1988,21,4                                                                                                             225

Fig. 6. 'Feather' consisting of irregular cavities and negative     Fig. 7. 'Feather' consisting of liquid, two- and most probably
        crystals with liquid and two-phase filling. Transmitted             three-phase inclusions in natural ruby from Nepal.
        light using methylene iodide as immersion liquid. 75x.              The solid components (probably margarite) show in-
        (Photo by U. Henn.)                                                 terference colours. Transmitted light using methylene
                                                                            iodide as immersion liquid, crossed polarizers. 80x.
                                                                            (Photo by K. Schmelzer.)

Fig. 8. 'Feather' consisting of small irregularly shaped cavities   Fig. 9. 'Feather' consisting of small irregularly shaped cavities
        and negative crystals with multi-phase filling in natural           and negative crystals with multi-phase filling (lower
        ruby from Nepal. Darkfield illumination. 40x. (Photo                left part) and ultra-thin liquid and two-phase inclu-
        byK. Scarratt.)                                                     sions showing interference colours under suitable illu-
                                                                            mination (central and upper right part). Transmitted
                                                                            light using methylene iodide as immersion liquid,
                                                                            crossed polarizers. lOOx. (Photo by K. Schmelzer.)

Fig. 10. Ultra-fine liquid films, partly also two-phase (liquid/    Fig. 11. Fine and bright dust-like 'fog' particles in natural
         gaseous) in natural ruby from Nepal; these fluid                    ruby from Nepal. Reflected light. 60x. (Photo by K.
         inclusions reveal interference colours under suitable               Scarratt.)
         illumination. Darkfield illumination. 50x. (Photo by
         E. Giibelin.)
226                                                                                                             1988, 21 , 4
                                                                                                      J. Gemm., 1988,21,4

          irregularly shaped cavities as well as small
or less irregularly                                             ultra-fme fluid
                                                            as ultra-fine   fluid inclusions in this high quality,
crystals (Figures 6 to 9). TheThe filling
                                   filling of
                                            of the small    1.288 ct ruby, on the one hand, proves the sample
                                                            1.288
                                (solid/liquid or liquid/
cavities is liquid, two-phase (solid/liquid                        of natural origin, and, on the other, confirms
                                                            to be of
gaseous) and, most probably, also three-phase               its locality as Nepal. Until now the exceptional
(solid/liquid/gaseous). The solid parts of  of the inclu-   growth structures
                                                            growth    structures of of this ruby
                                                                                             ruby had not
                                                                                                        not been
        displayed interference
sions displayed    interference colours under
                                          under crossed     observed in natural rubies either
                                                            observed                       either from
                                                                                                  from this or any
polarizers (Figure 4). Such feathers, which have            other locality.
                                                            other
       observed previously in Nepalese rubies of
been observed                                        of a
much lower quality, closely resemble residual flux          Acknowledgement
                                                            Acknowledgement
in flux-grown synthetic rubies. In addition, ultra-                             thank Ms FF. Wall, Department
                                                               We would like to thank
fine liquid films, sometimes also as two-phase              of Mineralogy, BM(NH), for Microscan
                                                            of                           Microscan IX micro-
              (liquid/gaseous) were observed in the
inclusions (liquid/gaseous)                                 probe analyses ofof the ruby
                                                                                     ruby and its phlogopite
natural ruby fromfrom Nepal (Figures 9, 10). Under          inclusions.
suitable illumination, these filmy inclusions glow
        interference colours. The ultra-fine
with interference                       ultra-fine films    References
testify
testify - together with the phlogopite inclusions           Harding, R.R.,
                                                            Harding,    R.R., Scarran,
                                                                               Scarratt, K., 1986. A description
                                                                                                        description of
                                                                                                                     of ruby
                                                                                                                        ruby from
                                                                                                                              from
examined by electron microprobe - to the natural                         J ournal of Gemmology, 20, 3-10.
                                                                Nepal. Journal
                                                            Kiefert, L. , Schmetzer,
                                                            Kiefert, L.,    Schmetzer,    K.,  1986.   Rosafarbene
                                                                                                       Rosafarbene    und  violette
origin of of the ruby. Howeyer,
                          However, another type of     of       Sapphireaus  ausNepal.
                                                                                 Nepal.   Zeitschrift  der Deutschen   Gemmologi-
                                                                Sapphire               Zeitschrift der Deutschen  Gemmologischen
inclusion was quite ambiguous at first sight; these             schen Gesellschaft,
                                                                       Gesellschaft, 35, 113-25.
are dust-like 'fog' striations (Figure 11), which are       Kiefert,L.,L.Schmetzer,
                                                            Kiefert,      , Schmetzer,    K., 1987.
                                                                                     K., 1987.         Pink
                                                                                                Pink and     andsapphires
                                                                                                          violet  violet sapphires
reminiscent
reminiscent of of Kashan synthetic rubies.                      from Nepal. Australian
                                                                from            Australian Gemmologist, 16, 225-30.

Conclusion
  In summary, the presence of of phlogopite, two-
and, most probably, three-phase inclusions, as well         [Manuscript
                                                            [Manuscript received
                                                                        received 28 April,
                                                                                    April, /988.]
                                                                                            1988.]

      ·:~~!h:l' ,.~. NEW GEMMOLOGY COURSE
      ~...;:~:.::~~- ~ '- The Gemmological Association of Great Britain is proud to
  r   /r'                - announce that it has introduced a new home study course in
                                                                        examinations
                           gemmology. This prepares students for the examinations
                           leading to the award of the Association's Fellowship
                           Diploma.
                           The new course is radically different
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                           gemmological courses, and presents a new, friendly, step-
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                           For          details, contact
                                                 contact the
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                                                                       Department,
                           Gemmological Association of Great Britain,
                           Saint Dunstan's House, Carey Lane, London EC2V 8AB.
                           Tel: 01-7264374. Cables:
                           Tel:             Cables: GEMINST.
                                                    GEMINST.
J. Gemm., 1988,21,4
          1988,21,4                                                                                                               227

                                          2
            ESR
            ESR and
                and optical
                    optical spectra
                            spectra of Mn2++ sapphire
                                    of Mn    sapphire
                              R. Liebach, Jill
                              R. Liebach, Jill Dobbie,      Hutton and G.].
                                                       D.R. Hutton
                                               Dobbie, D.R.            G.J. Troup

                       Physics Department, Monash University, Clayton 3168, Victoria, Australia

Introduction                                                          Synthesis of   Mn 2 + sapphire
                                                                                  of Mn2+
   In our studies of the Electron Spin Resonance                         Crystals of Mn sapphire were grown in PbO-Pb
(ESR) spectra of natural sapphires (Troup and                         Fz
                                                                      F 2 flux (Chase and Osmer, 1970). Analytical re-
Hutton, 1983) we observed in many cases, a large                      agent grade chemical compounds were used, and
number of small lines covering a large magnetic                       the composition was: 17 mol % of A1   A1 z200 33,, 30 mol %
field range: an example is given in Figure 1. The                     of PbFz,
                                                                          PbF 2 , 53 mol % of PbO and 0.05 mol % of             of
hypotheses we put forward to explain these lines                      MnOz.
                                                                      Mn0 2 . These amounts of the compounds were
                                             Cr 3+ or
were: (a) that they could be due to pairs of Cr3+                     mechanically mixed in an alumina container by
   3+
Fe + ions; (b) that they could be due to radiation                    shaking with a mixing pulsator for two hours.
                                            Mn 2 + .
damage; and (c) that they could be due to Mnz+.                          Subsequently the mixture was placed in a 60ml
   Although the Spin-Hamiltonian
                   Spin-Hamiltonian (ESR spectral                     platinum crucible which was then closed with a
                                     2+
parameters and behaviour) of Mn  Mn2+    in sapphire                  platinum plug. The filled crucible was placed in a
have been published previously (Low and Suss,                         closed-end alumina tube and covered with alumina
1960; Folen, 1962), no illustrations of spectra were                  bubbles. A ceramic cap was used to close the open
given. It would have been possible to calculate the                   end of the tube. (Figure 2).
appearance of the spectra, but this involves                             The alumina tube containing the Pt crucible was
assumptions about line-shapes. Accordingly, it was                    placed in the furnace and heated to 1270°C, held
decided to synthesize some Mn2+ Mn 2 + sapphire, in                   for 4 hours and cooled at 4°C/h to 900°C.
order to record the ESR spectra, and compare the                         The crucible was then cooled with the furnace.
appearance and line positions with the extended,                      The crystals which grew on the melt surface were
small line spectra mentioned above.                                   removed from the solidified
                                                                                           solidified flux by leaching in hot

                              1 3 5
                                                     t Fe (Z )

                                                                                                           f
                         t Fe ( 2" ) 1 t Fe ( "2 ) 3

       _(a)
         _ _ _. .       ~         ••__ tcr(z)         ~____ _ _ _ _ _{'.AtCr(i)
                                                                          _ _ _ _ _--,                         _ _B_l_ue
                                                                                                                     Sapphire

       _(b)               A__________~                 ~~ _________. ~ow
                        V'                      - \j     ---                                             V -sapphire
       I                             I                            I                           I                            I
       o                           Q2                           Q4                          Q6                            0.8
                                         Magnetic Field l Tesla )

Fig. I.
Fig. 1. ESR spectra of blue and yellow sapphire at -~ 33 cm
                                                         cm wavelength
                                                            wavelength with
                                                                       with the
                                                                             the steady
                                                                                 steady magnetic
                                                                                        magnetic field
                                                                                                  field perpendicular
                                                                                                        perpendicular to
                                                                                                                       tothe
                                                                                                                          the trigonal
                                                                                                                               trigonal
        axis.
        axis.

©
© Copyright the Gemmological Association
                             Association                                                                           ISSN: 0022-1252
228                                                                                                            J. Gemm., 1988,21,4

25% H N 0 3 . They were in the form of pink
pseudo-hexagonal or irregular platelets, which
proved to have the large faces perpendicular to the
c-axis. Most crystals had flux inclusions, and a
somewhat irregular distribution of the pink colora-
tion. Some of them are shown in Figure 3.                                                           ^ c e r a m i c cap
                                                                                            A
                                                                                             f 51
                                                                                                11
Optical spectrum                                                                                    m   ^ c e r a m i c tube
   The optical (visible) spectra to be presented and
discussed below were taken with a Varian DMS100
UV-Visible spectrophotometer. Because the Mn 2 +                                  Alumina
                                                                                  bubbles
                                                                                                                          tube
sapphire crystals were thin basal pinacoids, only                                                                  ^ ^    furnace
the ordinary ray spectrum, shown in Figure 4,
could be obtained. A comparison spectrum of Cr 3+
sapphire ('pink ruby') is shown in Figure 5. Be-
cause the spectrophotometer has an unpolarized
light source, and because of the cut of the synthetic
Cr 3+ sapphire sample available to us, its spectrum
                                                                                             1      L-" crucible

is a 'mixture' of ordinary and extraordinary ray
spectra.
   However, the familiar absorption bands in the
blue and green are clearly displayed, as is the                                                 1
ultraviolet absorption edge. The feature labelled                                               1
'D', in the red, results from the usually fluorescent
'ruby doublet'; in this case, because the dispersive
element in the spectrophotometer comes im-
mediately after the source, so that monochrome light                  Fig. 2. Details of the arrangement used in the furnace in order
falls on the sample, the lines are in absorption.                             to synthesize Mn 2 + sapphire.

Fig. 3. Some crystals of Mn 2 + sapphire. The largest crystal is ~ 1 cm across.
':-'
                                                                                                                                                                              ~
                                                                                                                                                                              oC')
                                                                                                                                                                              "8o
                                                                                                                                                                              ~f
                                                                                                                                                                               I:J
                                                                                                                                                                              '~
                                                                                                                                                                              00
                                                                                                                                                                              00
                                                                                                                                                                              -
                                                                                                                                                                              !?"
                                                                                                                                                                              ~
                                                                                                                                                                              N
                                                                                                                                                                              N
                                                                                                                                                                               .....
                                                                                                                                                                               j>.
                                                                                                                                                                              .~
                                                                                                                                                                              -
            3.200
            3200

            2.560
            2.560                                                                               2.400

    -V
     V)I
                    r
   ......
   .....
N
                                                                                                                                                                                              W
                                                                                                                                                                                              o
                                                                                         F

                        (a)

                        ( b)
                                      F

                                                                                                                                                                                              ~
                                  0.2                                          0.3                                           0.4                                            0.5               o
                                                                                                                                                                                              (b

                                                                           Magnetic Field ( Tesla)                                                                                            3
                                                                                                                                                                                              P
                                                                                                                                                                                              I-"
                                                                                                                                                                                              \0
                                                                                                                                                                                              00
                                                                                                                                                                                              .YJ
                                                                                                                                                                                              N
Fig. 6. ESR spectrum of Mn 2 + sapphire at --- 3 ern wavelength. Curve (a): static magnetic field parallel to the trigonal axis. Curve (b): static magnetic field perpendicular to trigonal   I-"

        axis.                                                                                                                                                                                 ~
J. Gemm.,
   Gemm., 1988,21,4
          1988,21,4                                                                                                             231
                                                                                                                                231

         Mn 2 + sapphire shows little absorption in
   The Mn2+                                                 Thus the lines arising in many natural sapphires sapphires
the visible:
     visible: what there is,is, occurs in a region not      must be due to some other impurity ion, to               to
occupied by the ruby absorption bands. bands. Further,
                                               Further,     radiation damage centres, to close pairs of Fe3+      Fe 3 +
the ultraviolet (UV) absorption edge is shifted,shifted,    ions, or a combination of these three.
                                                                                                three.
                                          considerably.
towards longer wavelengths, quite considerably.                However, there may be a good case for the
Because of the reduction process used to synthe-            natural yellow sapphire of Figure lea)   1(a) containing
                                                                                                            containing
                                                 Mn 2 + ,
size this material, it will contain not only Mn2+,          Mn 2 + , since the small lines appear approximately
                                                            Mn2+,                                      approximately
but charge compensation centres as well, and also           at equal strength on either side of the g == 2 Fe3+   Fe 3 +
some Mn H  3+
              . Any or all of these may be the cause of     line, for the appropriate field spread. The Fe H         3+

the shift of the UV absorption edge.                        lines are very broad in this particular specimen,
   The Mn sapphire fluoresces under UV light,               and magnetic interaction (known as 'anisotropic
                                                                                                          'anisotropic
appearing pink to the eye. eye. A gemmological hand-        exchange interaction') is possible between the Fe3+   Fe 3 +
held spectroscope showed a broad fluorescent line           and Mn22 +  +
                                                                           ions.
                                                                           ions. This would broaden the Mn2+     Mn 2 +
                                    spectrum.
on the yellow-green edge of the spectrum.                   lines, thus including the small lines (labelled F in
                                                            Figure 6) under the broadened large lines.     lines. The
                                                                                                                   The
ESR spectrum                                                        Mn 2 + field lines of Figure 6(b) would simply
                                                            lower Mn2+
   The ESR spectrum of Mn 22 +     +
                                     sapphire is shown      be smeared out by this broadening, and thus would
                                                   field
in Figure 6: curve (a) for the static magnetic field        not be easily detected. However, the breadth of the
parallel to the c-axis, curve (b) for the field perpen-     Fe H
                                                               3+
                                                                   lines could indicate a high Fe3+ Fe 3 + concentra-
dicular to the c-axis. The spectrum is complicated,         tion, in which case the small lines in the yellow
and spread over quite a large region of     of magnetic     sapphire could be due to close Fe 33++ pairs. More
field, in comparison to the Fe 33++-and          CR 3+ -
                                           -and CRH-        work, including quantitative analysis, is necessary
sapphire spectra (static magnetic field perpendicu-         to resolve this question.
lar to the c-axis) shown in Figures lea)  1(a) and (b).        It is clear that either optical or ESR spectra will
This spread comes about because the nucleus of        of    discriminate easily between (synthetic) Mn2+    Mn 2 + and
Mn has a spin of 5/2, and this interacts with the            Fe 3+ or Cr33++ sapphire. While Mn22 +
                                                            Fe3+                                     +
                                                                                                        sapphire is a
total electron spin of 5/2. The phenomenon is               pleasing pink colour, different
                                                                                      different from the colour of
                         splitting,. The small lines in
             'hyperfine splitting;
known as 'hyperfine                                                 (Cr 3+ ) sapphire~
                                                            'pink (Cr3+)     sapphire', it is unlikely to become a
Figure 6, labelled F, in between the large lines, are       competitor on the synthetic sapphire market, be-
         'forbidden transitions;
due to 'forbidden     transitions'. So is the group of      cause it is much more difficult
                                                                                      difficult to make.
lines, at comparatively low field, labelled T     'L' in
Figure 6(b).
        6(b ).                                              References
Discussion                                                  Chase,A.B.,
                                                            Chase,   A.B.,Osmer,
                                                                             Osmer,   Judith
                                                                                   Judith       A., 1970.
                                                                                          A., 1970.  Habit Habit
                                                                                                             changeschanges    of sap-
                                                                                                                      of sapphire
                                                                phire grown
                                                                         grown from
                                                                                  from PbO-PbF
                                                                                         PbO-PbF,2 and  and MoOMoO,-PbF,
                                                                                                                     3 -PbF 2 fluxes.
   To our knowledge, pure Mn 2     2+
                                    + sapphire does not         AmericanCeramic
                                                                American      CeramicSociety
                                                                                        Society  Journal,
                                                                                               Journal, 53,53,  343-5.
                                                                                                             343-5.
                                                                                                                                fluxes.
occur naturally. Our hypothesis, that the ESR lines         Folen, V.J.,
                                                            Folen,   V.J.,'Forbidden'
                                                                            'Forbidden'   transitions
                                                                                      transitions in theinparamagnetic
                                                                                                            the paramagnetic
                                                                                                                         resonancereso-
in the g = 2 region (near 0.3 Tesla) might be due to        of Mn 2+
                                                                nance   of Mn'·
                                                                     in A1         in Al,O,.
                                                                            2O3. Physical      Physical
                                                                                          Review,   125, Review,
                                                                                                          1581-3. 125, 1581-3.
                      2                                     Low, W.,
                                                                   W, Suss,
                                                                        Suss, J.T.,
                                                                               J.T., 1960. Paramagnetic
                                                                                            Paramagnetic Resonance
                                                                                                              Resonance Spectrum
the presence of of Mn
                   Mn2+ ^ in natural sapphire is, for the   Low,
                                                                of Manganese in Corundum. Physical Review, 119, 132-3.
                                                                of
most part, not supported, because the spread of    of the   Troup, G.J.,
                                                                     G.}., Hutton,      D.R. 1983. The
                                                                             Hulton, D.R.              The useuse of
                                                                                                                   of electron
                                                                                                                        electron spin
                                                            Troup,
Mn 22 ++ lines about this region is almost symmetric-           resonancespectroscopy
                                                                resonance     spectroscopy to to distinguish
                                                                                              distinguish      synthetic
                                                                                                           synthetic fromfrom    natu-
                                                                                                                            natural
al. For reasons of of space, we do not reproduce the            ral sapphires.
                                                            sapphires. Journal ofJournal   of Gemmology
                                                                                    Gemmology,    XVIII, 5,, XVIII,
                                                                                                              421-31.5, 421-31.
spectra given in Troup and Hutton, 1983 here:
                                            2+
these spectra, we believe, show that Mn Mn2+ is absent.
                                                  absent.   [Manuscript received
                                                            [Manuscript          23 December
                                                                        received23  December1987.J
                                                                                             1987.]
232                                                                                                     J. Gemm., 1988,21,4

        The gemmological characteristics of Inamori
         synthetic cat's-eye alexandrite chrysoberyl

                      John    Koivula*,*, Dr
                      John I. Koivula                 Fritsch * and
                                             Emmanuel Fritsch*
                                          Dr Emmanuel           and Chuck
                                                                    Chuck Fryer **
                                                                           Fryer**

 *Gemological Institute of America, Research Department, 1660 Stewart Street, Santa Monica, California 90404,
                                                   USA
                **GIA Gem Trade Laboratory Inc., Santa Monica, Los Angeles and New York

Abstract
   Kyocera
   Kyocera Corporation
               Corporation of   of Kyoto,
                                   Kyoto, Japan,
                                           Japan, has successfully
                                                         success- to sophisticated
                                                                      sophisticatedtesting
                                                                                     testing equipment,
                                                                                           equipment,  the the internal
                                                                                                           internal     charac-
                                                                                                                    characteristics
fully  synthesized,
   synthesized,     andand    is currently
                         is currently       marketing,
                                        marketing,         a cha-
                                                    a chatoyant   teristics are the only universally available means of
toyant colour change material that gemmologically                 identifying  thisnew
                                                                  identifying this   newsynthetic
                                                                                          synthetic  product.
                                                                                                  product.
tests as cat's-eye alexandrite chrysoberyl. With the
exception of microscopic
exception        microscopic characteristics,
                                  characteristics, all
                                                   all the gemmological
                                                            gem-  Introduction
mological
   properties properties
                 shown by   shown   by this material
                              this material            are essen-
                                             are essentially          Since late 1986 Kyocera America Corporation's
tially
   the the
        same same  as those
               as those        encountered
                           encountered       in natural
                                         in natural       alexan-
                                                     alexandrite   'Inamori' gemstone and jewellery division has been
drite  cat's-eyes.
   cat's-eyes.   ForFor   those
                       those     gemmologistswithout
                              gemmologists       withoutaccess
                                                           access
                                                                  marketing, as *'Inamori~
                                                                                       Inamori', aa new
                                                                                                      new chatoyant
                                                                                                             chatoyant colour
                                                                                                                          colour
                                                                  change material that gemmologically tests as alex-
                                                                  andrite cat's-eye chrysoberyl. This new synthetic is
                                                                  manufactured
                                                                  manufactured by their parent company, Kyocera
                                                                  Corporation, which has headquarters in Kyoto,
                                                                  Japan.
                                                                      In an effort
                                                                             effort to provide the gemmological com-
                                                                  munity with information
                                                                                    information on their new product,
                                                                   Kyocera recently loaned the Gemological Institute
                                                                  of America, in Santa Monica, California, some
                                                                  samples of these new colour change cat's-eyes for
                                                                  gemmological examination. The results of this
                                                                  detailed examination comprise the body of this
                                                                  report.
                                                                   Description
                                                                      The two largest stones supplied by Kyocera
                                                                   (Figure 1) were semi-transparent, well polished,
                                                                   oval double cabochons that weighed 3.27 and 3.31         3.31
                                                                   carats respectively, with corresponding measure-
                                                                   mentsof9.00
                                                                   ments of 9.00 x 7.01 x 5.55 mmand   mm and 8.92 x 7.11   7.11
                                                                    x 5.61 mm. The remaining bulk of the test sample
                                                                   consisted of ten smaller uniform-cut
                                                                                                   uniform-cut 6 xX 55 mm
                                                                   double cabochons with a total weight of 10.86
                                                                   carats.
                                                                      With the aid of a single overhead incandescent
                                                                   light source all the stones displayed a relatively
                                                                   sharp, moderately intense, bluish-white chatoyant
                                                                   band running across their length (Figure 1).
                                                                      The stones showed a moderate change of colour
                                                                   that complemented their near transparency. The
      1. The two largest synthetic Kyocera alexandrite chry-
Fig. I.
                                                                   body-colour in incandescent light (Figure 1) was a
         soberyl
         so beryl cat's-eyes described in this report. Incandes-   vivid, slightly-dark, purplish-red. Under the sun,
         cent fibre-optic illumination.                            or in fluorescent light, the colour changed to a very

©
© Copyright the Gemmological Association
                             Association                                                                      ISSN: 0022-1252
J. Gemm., 1988,21,4                                                                                       233

slightly brownish purple-green. In addition to' the     stones were no exception. They showed brownish
colour change, under all lighting conditions, the       green, brownish yellow and slightly brownish red.
stones possessed a somewhat greyish milky over-
tone which is also shown in Figure 1.                   Reaction to ultravioletradiation
   In transmitted incandescent light these cat's-          When exposed to long-wave ultraviolet radiation
eyes showed a columnar cone of milky pink light         the cat's-eyes fluoresced a uniform dull, chalky red
(Figure 2). Its diameter was controlled by the size     colour of moderate intensity. The short -wave reac-
of the aperture placed between the light source and     tion appeared to be a slightly stronger, very chalky,
the stone.                                              brownish-orange. Phosphorescence was not
                                                        observed in any of the stones.
Gemmological properties
   The properties listed by Kyocera in the prom-        Specific gravity
otional brochure for their new 'Inamori Created'           Using the hydrostatic method the specific grav-
alexandrite cat's-eye are provided, for reasons of      ity of the two largest stones was determined. The
comparison, in the table below.                         average value for six tests was calculated as 3.74.

                                                        Colourfilter reaction
                                                          As expected, the colour of these synthetic colour
Classification             Chrysoberyl
                                                        change cabochons appeared red when viewed
Chemical composition       BeAlz0 4
                                                        through the Chelsea colour filter.
X-ray diffraction          Same as natural
                           alexandrite cat's-eye
                                                        Spectroscopy
Spectograph                Same as natural
                                                           The visible light spectrum, obtained by trans-
                           alexandrite cat's-eye
                                                        mitting white light through the domes of the
Crystal system             Orthorhombic
                                                        cabochons, was typical of those recorded previous-
Hardness (Mohs)            81/ 2
                                                        ly for alexandrite (Liddicoat, 1981). The observed
Specific gravity           3.72
                                                        lines were located at 680, 650, 625, 616 and 471
Melting point              1,870°C
                                                        nanometres. In addition there was a smudged band
Transparency               Transparent/ semi
                                                        between 590 and 535 nanometres, and a cut-off in
                           transparent
                                                        the blue at 445 nanometres. It was also noticed that
Refractive index           1.743-1..752
                                                        the largest of the stones showed a weak cat's-eye in
Double refraction          0.008
                                                        transmitted light.
Change of colour           Distinct
Averagedispersion          0.015
Pleochroism                                             Microscopy
  Daylight                 Strong green/yellowish          When microscopically examining these synthe-
                           green/dark red               tic cat's-eyes the first thing noticed is the transmit-
  Incandescent light       Reddish purple               ted light appearance of a multitude of apparently
Chelsea colour                                          parallel colour zones (Figure 3) that run perpen-
  filter reaction          Red                          dicular to the chatoyant band (Figure 1). At first
Inclusion                  Solidus                      these zones appear to be perfectly straight, but
                                                        close scrutiny, in combination with shadowing,
                                                        shows that they are very slightly undulating. This
The results of the laboratory testing done by the       suggests that these cat's-eyes are crystallized from
authors on Inamori's alexandrite cat's-eyes are re-     a high temperature melt rather than grown as
ported as follows:                                      euhedral crystals by a flux or hydrothermal pro-
                                                        cess.
                                                           When incident illumination is used, numerous
Refractive index                                        thin, purplish blue-white, milky zoned bands
  Using the largest possible 'spot' contact area on     appear where the colour zones are (Figure 4). The
the refractometer, and sodium light, the refractive     precise directional relationship between these mil-
index of these cat's-eyes was read as 1.747 to 1.753.   ky bands and the colour zones is revealed when the
Because the stones' surfaces were curved, more          stones are examined, directly through the
precise readings and accurate birefringence deter-      cabochon's dome, using both fibre optic and sha-
mination were not possible.                             dowed transmitted light in combination (Figure 5).
                                                           These zoned bands are composed of tiny white
Pleochroism                                             particles which are far too small to be individually
  Alexandrite chrysoberyls are trichroic and these      resolved microscopically. They are the cause of the
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