Several rubies heated with lead rich glass in Chantaburi (photo 1) and in Bangkok (photos 2 to 6)
PART 3: Identification and analysis of the “repaired rubies”:
Identification of the lead glass “repaired rubies” is very easy for any laboratory that owns an EDXRF
(Energy Dispersive X-Ray Fluorescence), but microscopic observation is in most cases enough for a
gemologist that has experience with these stones. Using EDXRF the AIGS laboratory was able to find
lead in all the stones studied. It is the ideal instrument to provide a rapid diagnostic result.
|
EDXRF: This instrument’s main use is to provide some quantitative and qualitative information on the chemical composition of a given stone.
EDXRF: can detect any element heavier than fluorine and it is especially efficient for heavy elements such as lead.
This instrument provides a very fast and reliable diagnostic analysis. The AIGS laboratory is using this instrument on all rubies presented for identification.
On the EDXRF spectrum on the right you can clearly see the peaks related to various elements. Ruby is composed of aluminum, oxygen and some trace elements such as chromium and iron that give the stone its color.
The presence of lead (PbL on the photo) is diagnostic that the stone has been treated with the lead glass technology because lead is never found in natural corundum.
Lead was found in every stone that was tested and copper was also found in 2 stones with very large filled cavities.
This cavity on a “repaired” ruby was carefully placed to be checked using EDXRF, as the cavity luster is very close to the ruby luster showing that the glass has a refractive index very close to the ruby.
The cavity surface is visibly damaged, as the glass is very soft. Such damages could have occurred during the cutting or polishing process.
Copper was detected while studying this large cavity along with lead but it
could be the result of pollution from polishing powder residue filling damaged areas. (The detection of copper was not successful under other conditions)
|
|
Because lead is a very heavy element, we are here in the exact opposite situation compared to the
Beryllium issue. Beryllium is a very light element. Its detection is not possible using EDXRF, which
makes the detection of the stones, treated using beryllium a complicated matter. This relatively new
type of treatment involving lead is very easy to detect.
Ultra Violet: Examination of the stones using a standard SW and LW (short wave and long wave)
fluorescent box did not give any diagnostic result.
Microscopic observation: An experienced gemologist using a microscope and dark field illumination will be able to identify correctly the “repaired” rubies without any difficulty:
Using dark field illumination, most lead-rich glass filled fissures will display blue/orange flashes as seen
on the following photos. This observation can be easier using fiber optic illumination looking near
parallel to the fissure. This is a very typical diagnostic feature that is quite similar to “opticon flash
effect” in emeralds or in lead glass filled diamonds.
Note: Depending upon the company performing the treatment, the composition of the glass and the
parameters used, the “blue/orange flashes” may vary from very obvious to very difficult to observe:
With careful close-up examination of the fissures an observer may also find gas bubbles or “platelets”.
Gas bubbles were found in many rubies filled with the simple lead glass:
Some “platelets” are present in all the “repaired” rubies that were treated using the so called “popular”
formula in Chantaburi and in most stones from Bangkok, these platelets could be remnants of former
“iron stains” formerly present in many rough stones from alluvial mining areas.
(“Platelets” found in Chantaburi rubies: They are transparent or act as mirrors depending the light orientation.)
(“Platelets” found in Chantaburi rubies: They are transparent or act as mirrors depending the light orientation.)
Mr. Mahiton Thondisuk told first AIGS gemologists about “copper platelets”. It was in fact a language
misunderstanding as he was in fact speaking about “iron stain” present in the stone before the
treatment: “Iron stain” is present in many stone from alluvial mines like Andilamena. Orange or
yellowish before heat treatment, it turns to whitish or blackish after treatment:
Orange “Iron stain” is very visible in these unheated Andilamena rubies fissures (photo under immersion)
(“Iron stain” remains in Pailin blue sapphire heated using traditional heating methods)
The “platelets” present in many stones does not present the typical shape of flattened glass bubbles
but could be in fact the result of the mixing of the glass with some iron rich natural powders. “The
number of such platelets can be reduced with careful temperature control” said master burner Mahiton
Thondisuk. Careful observation of these platelets shows that they were transparent when observed
from most directions, but they can also act as small mirrors inside the gem. In this case they are often
seen reddish. Color concentrations in the fissures were not found in any stone from Chantaburi using
the immersion technique, but some platelets did seem to have subtle coloration. In rubies enhanced in
Bangkok by Orange Sapphire company, some yellow to orange color concentration appears is large
fissures and in cavities. The fact that lead glass used in most Chantaburi treatment is pink explains why it is most of the time not visible inside the gem:
(Photo 1 and 2: Bangkok heated rubies presenting some orange color concentration in fissure and cavities
Photo 3: Yellow lead rich glass sticking together two rubies after heat treatment using lead rich glass)
(A wide fissure filled with lead glass from a “Bangkok repaired” ruby present a noticeable orange color:
Left to right: overhead, transmitted and dark field illumination)
(A cavity filled with orange lead glass in a “Bangkok repaired” ruby:
Photo 1: overheard light, photo 2: transmitted light, photo 3: dark field light)
(Other cavities filled with orange lead rich glass in “Bangkok repaired” rubies. Photos: Transmitted light)
An attempt to explain the reason why the stones repaired using the “popular” formula present a
stronger coloration than the stones using the “lead only” formula could be in the fact that the
transparent platelets could act as mirrors inside the gem. They are normally present in a random
orientation inside the gem, following the former fissures planes. They don’t block the light path as
orientated rutile silk can do. The light passes through some of them and is reflected by others. These
reflections could increase the length of the travel of the light inside the gem. As we know, the longer
the length of the light passing inside the gem, the more saturated the stone color will be. But this
attempt to explain the improvement of the color should be confirmed by more in-depth studies.
Some observers could be disturbed by the fact that the heat treatment temperature is not high
compared with the temperature at which many stones are heated nowadays using gas furnaces.
Many inclusions may still appear as “unheated” which could disturb an inexperienced observer:
Heat treatment temperature can vary from as low as possibly 800 degrees Celsius to more than 1300
degrees Celsius. As rutile needles begin to resorbe over 1000 degrees Celsius, it is possible to find
perfectly shaped needles in lead glass repaired rubies. Burmese star rubies are also known to have
been repaired by burners in Mae Sot. As the glass composition, the treatment parameters and the ruby
material used are not the same in Chantaburi, Bangkok, Mae Sot and in the other places this treatment is or will be performed, different features are possible.
Inclusions in Andilamena rubies repaired in Chantaburi at low temperature (Under 1000 degrees):
(Intact rutile needles, euhedral crystals found in many lead glass
treated stones giving them an “unburned” aspect)
Inclusions in Andilamena rubies repaired in Chantaburi over 1000 degrees:
(Melted crystals surrounded by glassy discoids,
typical of heated corundum are also found in many “repaired” rubies)
(Melted crystals, glassy discoids, resorbed needles
typical of heated gems are also found in many “repaired” rubies)
(High luster rutile crystals reaching the surface
should not be mistaken with lower luster lead glass filed areas)
“FUNNY” IDENTIFICATION STORY: A funny identification story happened during this lead glass
ruby study: One of AIGS good friends that have provided us some stones did not warn us that the
parcel was not only rubies: One stone with a similar aspect as the others was not ruby… Inclusions in
this stone were slightly different from the typical ruby heated with lead glass but not that much as you
can discover on the following photos: If “blue/orange flashes” were absent numerous “platelet” looking inclusions were present along with needles. When the stone was drop for immersion study in heavy liquid something was really wrong for corundum as the stone was floating! Refractive Index and EDXRF study confirmed its true nature: Pezzottaite…
(The pezzottaite cabochon submitted to AIGS lab and some of its “red platelet” looking inclusions)
“What about the durability of these gems? Should we buy it?”
Here are several questions dealers in Bangkok, and from outside Thailand asked AIGS gemologists
recently. In order to help them to find the answers, the AIGS laboratory has performed some tests to
evaluate the durability of these gems:
What is the origin of the color in these stones? The gemstone color improvement seems
to result from the fact that the fissures that were formerly filled with air or liquid are then filled
with a transparent glass. As lead glass and ruby refractive index are very close, the light can
then travel more easily inside the gem, and as a result, the overall color looks dramatically
improved. The same phenomenon is encountered with emeralds before and after oiling them.
Some questions were raised about the fact that some pink colored glass is used in Chantaburi, and a
more yellow one in Bangkok:
Can we describe these stones as dyed? Regarding the stones we have seen up to now: No.
We have observed some light color in some wide fissures and cavities in rubies from Bangkok
ovens but it was never enough to honestly say that the stone was dyed. Color concentration in
fissures was not detected in Chantaburi stones.
Some red or orange color can be seen in some stones using “day light” tubes like those in common use
in Chantaburi’s buying offices. But these red looking inclusions described as “copper platelets” by
treatment master Mahiton Thondisuk, present similarities with the glassy areas showing similar red
coloration found in many Mong Shu rubies heated with flux under the same illumination:
(Glassy inclusions showing some red reflected color visible in Mong Shu rubies heated with flux)
The glass lead glass present in this new treatment or the “flux residue glass” present in Mong Shu act
in fact as a mirror, reflecting the color of the stone to finally give the illusion that the glass is colored.
The same phenomenon can also be observed when twinning is present: Twinning planes can appear
colored under some orientations. Twinning plane cannot be described as colored:
(Twinning planes seen in Mong Shu rubies heated with borax presenting some pinkish to reddish “coloration”)
Dyed rubies present on the other hand some very clear color concentration in fissures which is in
strong contrast with the light colored to colorless body color whatever is the direction we observe
them. The presence of a light pink or yellowish glass visible in wide fissures or cavities in “repaired
rubies” is very different in intensity compared to dyed rubies in which fissures are filled with intensely
colored red dying agent. In fact this light colored glass found in some important fissures can be more
compared to “iron stain” in natural stones: The coloration of the glass is not the origin of the color, but
massively filling important fissures, it can modify the stone color if the stone color is weak.
(Typical dyed rubies presenting strong red colored fissures and a very lightly colored body color)
Are these stones durable? If handled with care: Yes, probably…
As this study was performed over a 2 month period, and regarding to the fact that none of the studied
treated stones were more than one year old, we cannot be 100% sure about the durability of the glass
inside the gem. Now if we compare this glass filling method to the glass filling used in diamonds, the
treatment looks to be suitable for “normal wear”.
Compared to emerald oiling or impregnation using resins, this current ruby treatment is probably more
durable. Glass is more stable than resin and its presence in a fissure will probably lower the probability
that the fissure will expand. The fact that the fissures are closed with a lead rich glass is also probably
improving the durability of the “repaired” gemstone, but not as much as those fissures filled by flux
additives. It is reasonable to assume that these stones are possibly more durable than an impregnated
emerald, but less than a ruby heated with flux.
Now we have also to consider that many companies are now trying to perform this treatment and if
some will succeed, some other may encounter technical problems. As the “glass” composition might
vary a lot in the future, some surprises are probably still to come.
Note: If this treatment technique is currently performed mostly on Andilamena Madagascar rubies, it is
likely to spread on other fractures corundum like star rubies, sapphires and even other gemstones
which can support temperatures around 1000 degrees and present fissures.
Are only large rubies affected? No
The stones are heated together in large amounts. The most suitable material is corundum presenting
multiple fissures. But small stones and clean material are submitted to the treatment in large parcels
along with fissured stones. These stones after cutting will not present filled fissures, so it will not be
possible to find diagnostic “blue/orange” flashes. Lead detection using EDXRF can also become a
problem: When dealing with small stones, it is more difficult to get diagnostic results as we have less
material to investigate. Small stones testing present some identification challenges and several EDXRF tests on different parts of a given stone are recommended: AIGS laboratory has studied several stones under 1 carat presenting lead reaction using EDXRF only when studied on the pavilion as no filled fissures were reaching the stone surface on the crown.
What should be avoided with these stones? AIGS laboratory has performed several
durability tests:
o One of these stones to a jeweler’s torch for a few seconds, and we observed some glass
leaving the fissure and some glassy bubbles created on the stone’s surface. This stone
would then need to be polished again at a minimum to enhance its aspect.
o Some stones were also boiled for several hours, immersed in detergents and exposed for
short periods to ultrasonic cleaning without any apparent damage.
o Several stones were submitted to “light and heat” fade test in order to study the color
stability after long exposition to light. No color modification was observed.
o Recutting or repolishing should be performed with care as the glass used is very soft and
could be damaged during the process. Many stones studied presented damaged or
incomplete fillings.
o The most important threat to the stone’s durability and beauty is contact with powerful
acids, such as hydrofluoric acid (also known as HF). AIGS exposed several stones to
hydrofluoric acid for 12 hours and 48 hours. In all cases the acid dissolved the glass and
the fissures in the stones were much more visible. The color and the clarity of the
gemstones were then seriously damaged in 3 cases out of 4. The attractive transparent
purplish red stones had lost some saturation after immersion in HF and were then
presenting unpleasant shiny whitish fissures.
Conclusions:
It is likely than in a close future different types of lead glass filled rubies will be present in
the market as several companies and individuals are investing in the process.
The detection of these repaired rubies should not be a problem for any experienced
gemologist with dark field illumination microscope or using EDXRF technology. But the
fact that the treatment can be performed at low temperature and let many inclusions in
their “unheated aspect” we recommend all ruby buyers to check their purchases with care.
Experienced gemological laboratories can provide them rapid identification if needed.
As long as these stones are properly disclosed and priced AIGS feels that these stones
should find their place in the gem trade where large size and low prices are of prime
importance.
The stone durability under “normal wear” should not be a problem, but it is important to
notify that these stones have to be kept away from excess of heat or powerful acids. If
some repairs are required special attention similar to that used for glass filled diamonds
and epoxy filled emeralds, should be observed. Jewelers wishing to use these stones in
jewelry should be cautious, but if handle correctly this product can be used in jewelry
without problem.
AIGS Laboratory Reports Comments:
In order to properly disclose these stones to its customers, AIGS Gem testing Laboratory currently
describe them as follows:
• On full reports:
Result: Found to be a Natural Ruby
Comments: This stone has been clarity enhanced.
(Color if noticeable) lead rich foreign substance found in fissures and cavities.
• On mini reports:
Identification: Natural Ruby.
This stone has been clarity enhanced. Lead rich foreign substance found in
fissures and cavities.
Learn more about “lead glass filled/repaired” rubies
Acknowledgments: A special thanks is extended by AIGS laboratory to Mr Mahiton Thondisuk and Mr
Somkuan Plairahan for their open and forthright disclosure of processes used in their fracture filling/
repair treatment. Special thanks also to orange sapphire people to have received and provide some
samples for study to AIGS laboratory.