Synthetic Diamonds: Rough And Treated, Faceted

(via ICA Early Warning Flash, No.74, August 13, 1993) GIA GTL writes:

Background
Recently a 0.74 carat yellow rough crystal was submitted to the GIA Gem Trade Laboratory in New York for routine identification. Shortly thereafter, a 0.55 carat dark brownish orangy red round brilliant was submitted to GIA GTL for an origin of color determination. Examination of both specimens revealed that they were synthetic diamonds. It was further determined that the rough specimen had been annealed and that the faceted one had been irradiated and subsequently annealed.

Appearance
The habit of the rough crystal was predominantly cubic, with some octahedral and dodecahedral faces. Smooth cube, and to a lesser extent, dodecahedral, faces are seen only on synthetic diamonds.

Magnification/magnetism
Both the rough and faceted pieces contained fairly large inclusions with a metallic luster. When suspended at the end of a thread, both were attached to a magnet, actually attaching to it. This reaction has been noted to date only with synthetic diamonds containing large, magnetic inclusions derived from the metallic flux in which they are produced.

The two showed similar patterns of ultraviolet luminescence and color zoning, forming essentially a square; the faceted piece also revealed this in the form of graining. This growth pattern was centered roughly in the middle of the base of the crystal and on the table of the round brilliant. Octagonal to square patterns are commonly seen in synthetic diamonds, but not in natural diamonds.

Ultraviolet luminescence
The ultraviolet luminescence of both pieces was stronger in short wave than long wave radiation. They both emitted a moderate to strong green fluorescence along the pattern described above in short wave UV radiation, with a weaker green reaction in long wave. The round brilliant also emitted a moderate orange fluorescence in short wave. Gem quality yellow synthetic diamonds previously examined by GIA Research and GIA GTL personnel have shown luminescence in short wave exclusively. The reactions noted in the two specimens under discussion would therefore appear to be from a source other than those we have previously documented in the gemological literature.

UV/Visible/IR spectroscopy
Spectroscopy helped to further characterize the specimens. Infrared spectroscopy showed them both to be essentially type Ib, as are most yellow synthetic diamonds. However, they both also showed a IaA character. This has not previously been observed in gem quality synthetic diamonds.

In the visible range, the round brilliant showed a number of sharp lines between 500 and 700bn at liquid nitrogen temperature. These features were noted both in the hand held spectroscope and on the chart of the spectrometer. Some of these lines have never been observed in natural diamond but have been reported in synthetic diamonds.

Finally, the presence of the features typical of treated pink diamonds in the spectrum of the red brilliant (in addition to other lines mentioned above) and a small HIb peak in the infrared prove that it had been irradiated and subsequently annealed. The yellow crystal also shows a line at about 637nm, which suggests that it, too, had been subjected to annealing.

Conclusion
The above characteristics clearly identify both the crystal and round brilliant as synthetic diamonds. However, some of their properties are slightly different from what we have observed before in yellow gem quality synthetic diamonds. Interestingly, virtually all the features noted are consistent with those of a group of Russian yellow synthetic diamonds currently being studied by GIA Research and the GIA GTL.

Polymer-impregnated Jadeite

(via ICA Early Warning Flash, No.75, November 23, 1993) GIA GTL writes:

Background
Over the last several years polymer-impregnated jadeite has become prevalent in the jade market. This has given rise to some colors of jadeite being routinely tested for the presence of this treatment.

Recently, the GIA GTL in Santa Monica received for identification a 15 carat purple oval cabochon that we identified as jadeite. Subsequent testing determined the stone to be polymer impregnated. To the best of our knowledge, this is the first report of a jadeite of this color that is polymer-impregnated.

Polymer-impregnated ‘lavender’ jadeite
Gemological properties: Gemological testing revealed an index of refraction and visible absorption spectrum consistent with jadeite jade. Specific gravity was measured by the hydrostatic method and determined to be 3.32, which is slightly lower than the norm for jadeite. This is consistent with previous findings of polymer-impregnated jadeite. The stone was inert to longwave ultraviolet radiation. Magnification did not reveal any evidence of treatment. As is often the case with purple jadeite, the origin of the color could be be determined.

Infrared spectroscopy
The spectrum of this stone reveals intense absorptions around 2900cm¯¹ which are not found in natural jadeite. These additional features are due to the presence of an ‘opticon-like’ polymer. This is not surprising, since this type of polymer is the most commonly employed for jadeite impregnation, according to many reports and our own experience.

Discussion
This finding is particularly significant since none of the polymer-impregnated jadeite (or B jade) we have seen so far was purple in color. They have all been green or mottled green and white, some with applied spots of brown. This means that we will now have to expand our routine testing for polymer impregnation to include purple jadeites as well.

New polymers for jadeite impregnation
We have recently encountered two new types of polymer used for the treatment of jadeite, in addition to the three previously described which are wax, an ‘opticon-like’ polymer, and phthalate-like polymer. Since we do not know yet their exact nature, we will refer to them as polymer 4 and polymer 5.

Polymer 4
The infrared spectrum of polymer 4 is very similar—but not identical—to that of wax. In particular, the major absorption is slightly shifted and of different width than that for wax. Jadeites treated with this product do not ‘sweat’ when tested with the thermal reaction tester, as opposed to those impregnated with wax which do. We measured the SG of one stone showing this kind of impregnation at 3.33.

Polymer 5
The infrared spectrum of polymer 5 shows similar absorption features as polymer 4, plus five more in the range of 2950-3150 cm¯¹. The three jadeites impregnated with this material that we studied are inert in ultraviolet radiation. We could measure the SG on only one of them, and the stone floated in the 3.32 SG liquid (methylene iodide). It is interesting to note that two of these stones displayed ‘sweating’ when tested with T.R.T.

Conclusion
These two new polymers have been seen on a few jadeites submitted for identification, and laboratories involved in B-jade detection should be aware of them. They demonstrate the growing variety of polymers that are being used for jade treatment. One reason for this could be the increasing number of companies involved in this treatment.

Yellow And Orange Sapphires

(via ICA Lab Alert, No.1, June 2, 1987) AIGS writes:

Background
In 1981, we at AIGS were asked to identify what was undoubtedly among the first heat treated Sri Lankan yellows to come out of ovens of Bangkok. We were told that the stone was treated by an unknown process (which was later found to be heat), and were asked to determine the color stability. This we proceeded to do by performing our usual fade test. This consisted of exposing the stone to heat and light at 1cm distance of a 150 watt spotlight for up to one hour. We were truly surprised when, after a few minutes exposure, the color had become much darker and more brownish (stones treated with irradiation would fade; some untreated Sri Lankan yellows will fade, but in most the color will not change). This change was temporary only; as the stone cooled to room temperature the color returned to normal.

Since this time we have tested over a thousand Sri Lankan yellow/orange sapphires and have found that all of the heat treated yellow to orange stones react in this way. Thus, a simple test for detection of heat treatment in Sri Lankan yellow/orange sapphires is possible.

The test
Place the stone in close proximetry to a source of mild source of heat, such as an incandescent bulb.

Results
Heat treated Sri Lankan yellow/orange sapphire —The color darkens temporarily, becoming more brownish. The deeper the original color, the greater the change. As the stone cools, the color returns to its original state. Control stones should be used so as to detect even slight changes in color.

Irradiated Sri Lankan yellow/orange sapphire —The color will fade, usually within one hour.
Untreated Sri Lankan yellow/orange sapphire —Generally no change, however some stones may show some fading.
Thai/Australian yellow/orange sapphire, heat treated or untreated—no change has been observed in the color of these stones.

(To: Mr N Horiuchi; Subject: Response to comment on Lab Alert No.1) AIGS writes:

Discussion
Mr N Horiuchi has commented on the test we previously described in Lab Alert No.1 to detect heat treatment in Sri Lankan yellow/orange sapphires. Mr Horiuchi stated that this color also did not fade under the same condition as reported on (by) AIGS.

From the above statement it appears that Mr Horiuchi has not understood the text of Lab Alert No.1. As others may also have misunderstood the text, we will describe the test again below.

Heat treatment in Sri Lankan yellow to orange sapphires may be detected by applying a simple fade test. (Caution: This test only works for Sri Lankan stones). Once a yellow/orange sapphire has been identified as definitely originating from Sri Lanka, its color is tested by applying a simple fade test. The stone in question should be placed on a glass (or other nonflammable) platform within ½ cm of a hot 150 watt (or more) spotlight. The idea is to expose the stone to lots of light and heat. After about 15 minutes exposure (as the stone heats up), the color of a heat treated yellow/orange sapphire will have been found to have become slightly darker and more brownish (the deeper the starting color before the test, the deeper and more brownish the color after heating up). This change is temporary only. As the stone cools its color will fade back to the color before the test was started, not, we repeat, not back to the color before the stone was heat treated (by someone else presumably). We believe that is where Mr Horiuchi misunderstood the original Lab Alert.

Other possible reactions
If the stone has been irradiated (either by nature or by man) the color will fade, usually within one hour’s exposure. In most natural Sri Lankan sapphires, however, the color will show no change. Natural yellow/orange sapphires from other sources and synthetic yellow/orange sapphires also show no change.

To make this test more accurate, control stones of similar color to the stone being tested should be used. Then after the stone in question heats up it can be compared to the color of the control stone. In the case of heat treated yellow/orange Sri Lankan sapphires, the change is not subtle in deeply colored stones, and anyone with normal vision should easily detect it, but the comparison must be made quickly before the stone tested cools down.

Dr Kurt Nassau has informed us that under certain conditions, yellow/orange sapphires may get darker upon exposure to some kinds of visible light. We have absolutely no information on exactly what kinds of stones do this or under what conditions. However he has promised us that the subject will be described in detail soon in an article he has written for Gems & Gemology. We have also written an article on the subjects covered in Lab Alerts Nos. 1 and 2 and submitted it to Gems & Gemology. We don’t know when it will appear (or if it will appear). We have had no reply of any kind, even though we sent it 8 weeks ago.

The subject of color in yellow sapphires is extremely complex. We have no illusions that the above information is the last word on the subject. However, over the past ten years we have tested thousands of pieces of yellow/orange sapphire from all sources and this is what we have found. If anyone else could she additional light on the subject, we would love to hear from them.

Dr K Schmetzer replies:
A. Fe³+ or by Fe³+ and Ti³+: Type 1, originating from Nigeria, Thailand, Australia or
B. By a yellow color center: Type 2, originating from Sri Lanka.

By heat or irradiation heat treatment, yellow stones with similar color centers, i.e with absorption spectrum similar to the spectrum of Type 2, but with different stabilities to light or heat are produced.

C. Irradiation treatment, color center: Type 3
D. Heat treatment, color center: Type 4

According to my experience and knowledge, AIGS describes a test for Type 4 stones, and N Horiuchi is dealing with Type 3 stones. Dr Nassau describes Type 2 stones in Alert No.9, and this type of yellow color center may be connected with natural irradiation. The reason for the higher stability of this naturally irradiated yellow compared to artificially irradiated yellow is an unknown but similar results were found by myself with natural irradiated yellow quartz (citrine) and artificially irradiated yellow quartz.

Unusual Composite Ruby

(via ICA Lab Alert, No.2, June 1987) AIGS writes:

During June of 1987, a very unusual composite ruby/synthetic ruby was brought in to the lab of AIGS for testing. It consisted of a piece of Verneuil synthetic ruby to which had been joined at the edge a smaller chunk of natural Burmese ruby. The whole stone was then faceted, concealing the join.

Two features are unusual about this stone. First of all, what appears to be glass has been used to join the two together. Gas bubbles were found in the glass area. Secondly, the edges of both the natural and synthetic areas were irregular. The use of glass to join the two together made this possible, as the glass-filled in the irregular surfaces. The entire stone showed signs of heat treatment, with induced fingerprints present in the synthetic section.

Detection
With the loupe or naked eye this stone could fool many people as the join looks like a crack and the natural area contained a large cloud of silk. However, immersion or overhead lighting will reveal the different luster of the glass join in the microscope. In addition, the synthetic portion displays curved striae and gas bubbles, as well as the induced fingerprints. The stone was purposely cut ‘native’ to imitate the appearance of a ruby just brought out from Burma.

Plastic Coating Of Gemstones

(via ICA Lab Alert, No.3, 1987) AIGS writes:

Details
In the past 3 years, gemologists at AIGS in Bangkok have encountered an unusual type of assembled stone in which an inferior specimen is coated with colored plastic. All of the stones treated in this manner have been of Burmese origin and so it is believed that the treatment is probably done in Burma.

One type consists of a poor color jadeite cabochon coated with a thin layer of rich green plastic. The coating covers all surfaces of the cabochon except the bottom. After coating, the stone appears to be of very high quality.

Another type is a light color faceted ruby coated with red plastic and then repolished. This gives the appearance of a fine ruby.

The third type seen is a white star sapphire cabochon entirely coated with red plastic. The gem then appears like a beautiful star ruby.

Detection
Although extremely deceptive to the naked eye, these plastic coated stones are readily identified under magnification. They may be dangerous to the trade, though, because their appearance is so natural that unsuspecting dealer might not even check them with the loupe. One unaided clue is provided by the slightly warm and plastic-like feel of the stones. This, however, is very subtle.

Identification of plastic coating is made with the microscope. In the case of the jadeite, as the plastic does not cover the stone entirely, it may be seen to peel away from the stone in places along the girdle. In all types, gas bubbles may be visible in the plastic coating, particularly in the star ruby type, where the coating was thicker. Color swirls could also be seen in the star ruby type. Judicious use of the hot point will, of course, also reveal this fraud.

Glass Infilling Of Cracks In Ruby

(via ICA Lab Alert, No. 4, June, 1987) AIGS writes:

Details
During the ICA Congress held recently in Bangkok, Dr Henri Hanni of Switzerland described to us a new ruby treatment. This consisted of poor quality African ruby cabochons whose cracks had been filled with glass. At the time of the Congress we had not yet seen these stones in Bangkok. In late June of 1987 we saw the first stone. It was a heavily included ruby cabochon, with many cracks that passed deep into the stone. These were filled with glass-like substance. This treatment differs from ordinary surface repaired rubies as the glass dos not just fill in surface pits, but instead appears to penetrate deep into the cracks.

Detection
This treatment is easily detected in the same manner as ordinary surface repaired rubies. Using overhead lighting, or immersion in methylene iodide, will reveal the glass filling due to its different luster or relief. If the opening of the crack is very narrow, however, the glass filling may be difficult to see. Gas bubbles may be found in some of the glass areas.

Dr K Schmetzer writes:
Kenyan rubies are also treated with plastics in order to improve the quality of the stones. In the treatment, cracks or fissures were filled with plastics which is sometimes deeply penetrating into the stones.

Natural And Synthetic Yellow/Orange Sapphires

(via ICA Lab Alert, No. 5, December 1987) AIGS writes:

Subject
The detection of color banding/growth zoning in natural and synthetic yellow/orange sapphires.

Method
Color banding, either straight or curved, can be detected much more easily by using a technique developed at AIGS in 1981. This involves the use of a frosted (diffused) blue filter over the microscope’s light source.

When looking for color zoning in yellow sapphires, the usual practice is to immerse the stone in methylene iodide. However, with a yellow stone in a yellow liquid over a yellow (incandescent) light, there is little chance of finding yellow bands of color. Using a white (fluorescent) light helps a bit, but not enough. AIGS have found that by using a frosted blue filter it becomes a much more easier to locate color bands, either straight or curved, as blue is the color being absorbed the most in yellow stones. Sometimes we stack two or three blue filters on top of one another. Although this does not cut down on the light intensity, it still makes it much easier to locate the color zoning. Using the frosted blue filter plus immersion, it is possible to locate straight or curved color banding in about 95% or more of all natural and synthetic yellow/orange sapphires. Furthermore, a green filter can be used for rubies—the color of the should approximate the absorption maxima of the stone.

E Gubelin writes:
To use a frosted blue filter and examine the gem in immersion is an excellent suggestion (though known to experienced gemologist for many years already). The effect may be enhanced if one close the diaphragm to about half or about a quarter of its diameter below the immersion cell.

Plastic Treated Emeralds

(via ICA Lab Alert No. 6, August 13, 1987) Nubio Horiuchi writes:

Source
I have personally seen this treatment for the past three years in Japan (Central Gem Laboratory).

Status
Details of this have not been announced yet, but it is summarized as follows:
The fractures are first cleaned and then impregnated with some kind of liquid plastic. It is presumed that the liquid plastic is hardened by irradiation of light or ultraviolet rays.

Merit of this treatment
In normal oil treatment the oil will seep out during cleaning or over a period of normal wearing and there is a gradual loss of color and the fractures become noticeable. However, with the impregnation of liquid plastic the treatment is durable.It would appear from the durability standpoint that the liquid plastic treatment is better than oiling.

Identification
It is difficult to distinguish between oil and plastic treatments.

Question
In which category of enhancement and treatment should the plastic treated emeralds be classified?

E. Gubelin writes:
Though more durable the result of this new plastic treatment should become to known to all members immediately, because many members of the trade use an ultrasonic cleaning machine which causes the oil to be washed out. If no oil is being washed out, people might not become aware of the fact that the fractures are filled with plastic films. Despite the greater durability the stimulus for easier fraudulent practices does by no ways raise the ethical standard of this plastic treatment.

Dr K Schmetzer writes:
The stones should be classified as plastic-impregnated emeralds.