'NAIL-HEAD SPICULE' INCLUSIONS IN NATURAL GEMSTONES

Authors: Gagan Choudhary and Chaman Golecha

(This article was first appeared in Gems & Gemology, Vol. 43, No. 3, pp 228 - 235)

Although the identification of any gem material requires testing with a variety of
i st u e ts, i ost ases the sto e s atu al o s theti o igi a e dete i ed
conclusively by the features seen with magnification. For example, curved lines or bands
fla e fusio , hou ds tooth patte s h d othe al , a d isp eil i lusio s flu
are all classically associated with synthetics.
Nail-head spicules are associated with synthetic hydrothermal (and occasionally
flux-grown) emerald (figure 1) and synthetic quartz (figure 2). However, such inclusions
have been reported in a number of natural and other synthetic gem materials (table 1),
including natural emerald (DelRe, 1992; Rockwell, 2003). Similar-appearing features have
been observed in photomicrographs of natural sapphires from Madagascar (Kiefert et al.
1996; Milisenda and Henn, 1996) though they have not been described in detail. This
article documents nail-head spicules and similar-appearing features in a variety of natural
gem materials, which could potentially lead to their misidentification as synthetics.

Figure 1: At left is a classic nail-head spicule in a hydrothermally grown synthetic emerald. On the
right is a spicule breaking on the surface of a flux-grown synthetic emerald. Note the black
material at the surface break. Photomicrographs by John I. Koivula (left, magnified 80x) ©GIA and
G. Choudhary (right, magnified 60x)

1 'Nail-Head' Spicule Inclusions in Natural Gemstones www.gem-passion.com

NAIL-HEAD SPICULES AND THEIR FORMATION
Nail-head spicules are wedge-shaped two-phase (liquid and gas) inclusions capped by
crystals that act as growth obstacles. In synthetic materials, they may occur in numerous
places throughout the sample, but mainly they appear near the seed plate. According to
Gübelin and Koivula (1986), fluid component is in direct contact with the crystal cap, an
inclusion of this kind is technically a three-phase inclusion.
Relatively disturbed growth is the primary cause of nail-head spicules. During
growth of the host crystal, a small crystal or platelet is deposited on its surface. As the
crystal continues to grow past the inclusion, a tapered void is created, which traps the
hydrothermal growth medium such that, upon cooling, it becomes two-phases consisting
of liquid and a gas bubble. In flux-grown emeralds, the crystals cap is usually phenakite,
beryl, or chrysoberyl and may even be gold from the crucible (again, see table 1). These
flat platelets/ crystals are not always easily resolved with a standard gemmological
microscope.
In synthetic emeralds, nail-head spicules develop most readily when growth
occurs on a seed plate inclined at an angle to the crystallographic axes, as in the case of
Biron synthetic emeralds (Kane and Liddicoat, 1985). To the best of the authors'
knowledge, no detailed research has been performed on the formation of nail-head
spicules in synthetic gem materials, and further correlation with the growth conditions is
beyond the scope of this article.

Figure 2: Nail-head spicules

are also seen in synthetic
quartz, where they are
commonly situated along the
seed plate, as in this
synthetic citrine.
Photomicrograph by C.
Golecha, magnified 30x

2 'Nail-Head' Spicule Inclusions in Natural Gemstones www.gem-passion.com

 TABLE 1: Selected reports of nail-head spicules and similar inclusions in natural and
synthetic stones.
Gem Material Inclusions References
Natural
Emerald Tapered voids with flat platelets, filled with two-phase Rockwell, 2003
inclusions
Spicule like inclusion capped by a yellowish crystal (calcite) DelRe, 1992
Diamond Hexagonal columnar indented natural Smith, 1991
Etched out - Needle like crystals Chapman, 1992
Sapphire Rounded apatite crystals accompanied by growth tubes Kiefert et al. 1996
Apatite crystals at the ends of hollow tubes Milisenda and
Henn, 1996
Pezzottaite Fine growth tubes emanating from crystals of tourmaline Laurs et al. 2003
Synthetic
Hydrothermal “ho t eedle e a ati g f o a ti luster of euhedral Sechos, 1997
emerald (Biron) phenakite crystal
Cone shaped void filled with a fluid and a gas bubble and a Kane and
phenakite crystal at base; nail head spicules at the edge of Liddicoat, 1985
gold inclusions
Hydrothermal Needle like tubes with one or two phase associated with Schmetzer et.al.,
emerald (Chinese) beryl or chrysoberyl crystals at broader ends 1997
Hydrothermal Phenakite crystals with wedge shaped voids extending from Liddicoat, 1993
emerald (Linde) them
Hydrothermal Growth tubes filled with liquid or two-phase associated with Schmetzer, 1988
emerald (Russian) double refractive crystals
Hydrothermal Reddish brown crystals with pointed growth tubes containing Gubelin and
emerald (Regency) liquid and gas. Koivula, 1997
Flux emerald Elongated cone shaped spicules associated with tiny Schmetzer et
(Chatham) i ef i ge t phe akite stals a d filled ith colourless or al.,1999
yellowish molybdenum.
Flux emerald Cone shaped cavities with tiny crystals (beryl) and partially Schmetzer et
(Nacken) filled with multicomponent inclusions: V-bearing al.,1999
polymerized molybdate, non-polymerised molybdate,
isolated aluminous silicates
Wedge shaped nail-like i lusio s ith phe akite stal at Nassau, 1980
wider end and filled with flux; rarely, large dark brown
tapered inclusions with a polycrystalline appearance
Hydrothermal red Hollow or two phase (liquid and gas) capped by a colourless Shigley et al.,
beryl or coloured solid inclusion of unknown nature 2001
Hydrothermal B ead u i lusio s asso iated ith t o-phase spicule Gubelin and
quartz (Citrine) Koivula, 1997

3 'Nail-Head' Spicule Inclusions in Natural Gemstones www.gem-passion.com

 MATERIALS AND METHODS
Six stones are documented in this report: two sapphires, an emerald, a spinel, a diamond,
and a sample of rock crystal quartz. All were faceted except the spinel (a pebble), and all
were submitted for testing at the Gem Testing Laboratory, Jaipur, India. The emerald was
brought in by a gemmologist who had purchased it as a natural specimen of Sandawana
(Zimbabwe) origin but was concerned about its identity due to the presence of nail-head
spicules along some planes. The remaining stones were submitted for routine
identification reports.
Standard gemmological tests were conducted on all six stones; however, we could
not determine the refractive index of spinel as it was a water-worn. We examined the
internal features of the samples with both a binocular gemmological microscope, with
fibre -optic and other forms of lighting, and a horizontal microscope. Infrared spectra (in
the 6000-400 cm-1 range for all stones, with particular attention in the 3800-3000cm-1 for
the quartz) were recorded using a Nicolet Avatar 360 FTIR spectrophotometer at room
temperature with a transmission accessory. The stones were oriented in the direction of
best transmission. In the case of the rock crystal quartz, spectra were taken according to
the optic axis direction as well (both parallel and perpendicular to the c- axis).

RESULTS AND DISCUSSION

The gemmological properties of the six stones are summarized in table 2. In all cases,
these were consistent with those reported in the gemmological literature for natural
samples of each material.
TABLE 2: Gemmological properties of six natural stones with nail-head spicule or similar inclusions.

Property Sapphire Emerald Spinel Diamond Rock crystal

Specimen 1 Specimen 2
Colour Blue Yellow Green Blue Light yellow Colourless
Weight (ct) 3.09 5.00 12.56 13.84 0.61 5.00
Cut style Cushion mixed Oval mixed Octagonal step Rough Round brilliant Oval mixed
RI 1.762-1.770 1.762-1.770 1.584-1.591 nd OTL 1.542-1.551
SG 3.99 3.99 2.73 3.61 3.52 2.64
Abs. Spectrum nd nd Typical chromium Iron band at nd nd
spectrum 460 nm
UV Fluorescence Apricot (LW); Apricot (LW); Inert in LW& SW Inert in Blue (LW); Inert in LW &
weaker in SW weaker in SW LW& SW weaker in SW SW

4 'Nail-Head' Spicule Inclusions in Natural Gemstones www.gem-passion.com

Sapphire (Specimen 1)
Viewed with magnification, the stone exhibited many crystalline inclusions and some
elongate inclusions, mainly concentrated along the wider girdle end. Also observed were
elongated, somewhat conical or rectangular inclusions terminated by crystals; these
appeared to be nail-head spicules.
When the specimen was immersed in methylene iodide, the nature of the
inclusions became clearer. All the nail-head spicules were oriented in a single direction
parallel to the optic axis (figure 3). Each typically consisted of a cluster of crystal-like
terminations connected to an elongated conical cavity; several also exhibited two-phase
inclusions within the cones. Those spicules with a rectangular tube-like projection were
somewhat similar to inclusion pattern illustrated by Kiefert et al. (1996) and Milisenda
and Henn (1996). Most of the spicules were situated among a group of birefringent
transparent colourless crystals, many of which had highly reflective faces (figure 4). Also
observed were conical apatite crystals which are commonly associated with Sri Lankan
origin (Hughes, 1997). Viewed with diffused illumination (while still in immersion), the
sapphire showed strong hexagonal growth zoning with uneven patches of colour.

Figure 3: Nail-head spicules are

oriented parallel to optic axis in
this natural blue sapphire, seen
here immersed in methylene
iodide. Each consists of a cluster of
crystal terminations connected to a
cone. Some of the cones are two-
phase inclusions. Photomicrograph
by C. Golecha, magnified 40x

5 'Nail-Head' Spicule Inclusions in Natural Gemstones www.gem-passion.com

 A weak undulating chevron pattern, which indicated rapid growth necessary for
formation of nail-head spicules, was seen mainly where the spicules were concentrated.
(Unfortunately, these features could not be resolved clearly for photography.) This
undulating pattern somewhat followed the hexagonal colour zoning. A literature search
turned up no reports of nail-head spicules in synthetic sapphires, so this stone was
particularly unusual, as this chevron pattern is often seen in hydrothermal synthetics.
The natural origin of this sapphire was easily confirmed with standard
instruments and the presence of other features such as zoning and fluorescence.
However, another similar spicule (figure 5) was present near the pavilion, which could
lead to misidentification had the stone been cut with that inclusion alone.

Figure 4: Viewed with crossed polarizers, the Figure 5: A single spicule was present near the
crystal clusters proved to be birefringent. Also pavilion of the sapphire. Identification by
note the conical elongated apatite crystals, which standard techniques could be difficult if the stone
are commonly observed in Sri Lankan sapphires. was cut with this inclusion alone.
Photomicrograph by C. Golecha, magnified 25x Photomicrograph by C. Golecha, magnified 30x.

Sapphire (Specimen 2)
This yellow sapphire contained numerous etch channels, and one of them reached a
crystalline inclusion, giving the general appearance of a nail-head spicule (figure 6). The
identification of the stone and its natural origin was easily established; however the
inclusion could create confusion for a novice gemmologist.

6 'Nail-Head' Spicule Inclusions in Natural Gemstones www.gem-passion.com

 Figure 6: This etch channel in a
yellow sapphire is in contact with
an included crystal, resulting in a
nail-head spicule –like appearance.
Photomicrograph by G. Choudhary,
magnified 30x

Natural Emerald
The stone contained abundant curved, tremolite–like fibrous inclusions (figure 7), which
proved its natural origin and indicated its source as Sandawana (Gübelin and Koivula,
1986). When it was viewed from various angles, however, numerous nail-head spicules
were observed in a single direction originating from parallel planes (figures 7 and 8) that
were oriented perpendicular to the optic axis. The effect was very similar to that seen in
synthetic emeralds. In this case, the crystals at the base of the spicules appeared to
originate from the plane itself.

Figure 7: In this emerald,

small dark conical
inclusions can be seen
projecting from the parallel
planes in the background,
similar to nail-head spicules
projecting from the seed
plate in a synthetic
emerald. However, the
presence of abundant
curved, fibrous tremolite-
like inclusions indicates a
natural origin: Sandawana,
Zimbabwe.
Photomicrograph by G.
Choudhary; magnified 20x

7 'Nail-Head' Spicule Inclusions in Natural Gemstones www.gem-passion.com

 Figure 8: At higher
magnification, the
parallel growth planes in
figure 7 showed
abundant nail-head
spicules; also note the
two-phase inclusions at
the broader end.
Photomicrograph by G.
Choudhary, magnified
35x.

Also p ese t e e li uid fi ge p i ts, flat efle ti e fil s o ie ted along the
basal plane, and angular zoning. Further confirmation came from FTIR spectra taken in
various directions, which showed the strong peak at 5270 cm-1 that is characteristic of
natural emerald (e.g., Choudhary, 2005). Nail-head spicules have been previously
encountered in natural emeralds (DelRe, 1992; Rockwell, 2003), so this sample served as
a further reminder of the need for careful and complete examination.

Natural Spinel
Magnification revealed numerous surface reaching conical inclusions (figure 9) pointing
toward the interior of the pebble from various directions. Some also exhibited a sharp
angular bend (figure 10). Careful examination revealed that the inclusions broke the
surface with rhomboid or sub- hexagonal/ rounded cross sections (figure 11) that varied
with the direction of entrance into the stone, which suggested that the shapes were
determined by the growth orientation. Some of these inclusions were filled with a
brownish epigenetic impurity (figure 11, right)
At certain angles, these inclusions were highly reflective, with flat surfaces
intersecting each other in a pyramidal arrangement. Although, their overall

8 'Nail-Head' Spicule Inclusions in Natural Gemstones www.gem-passion.com

 characteristics were indicative of etch channels, the possibility of these being elongated
needles cannot be ruled out (Chapman, 1992). The authors have observed similar
inclusions in a few flux-grown emeralds, where the spicules broke the surface and
appeared to be filled with a black material (again figure 1, right).
Although etch channels are common in a number of natural gems, in this
specimen they closely resembled nail-head spicules. Due to the absence of any other
visible inclusions, this specimen could have easily confused a novice gemmologist.

Figure 9: Near the surface of this spinel pebble, a Figure 10: Spicule-like inclusions, some displaying
number of long, conical etch features resemble a sharp bend, were observed in various directions
oriented spicule inclusions. Photomicrograph by pointing toward the interior of the spinel pebble.
C. Golecha, magnified 30x Photomicrograph by C. Golecha, magnified 30x

Figure 11: These spicule-like inclusions in spinel appear to be etch channels. Their cross-sections varied from
rhomboid (left) to hexagonal (right). Also note the brownish epigenetic filling material (right).
Photomicrographs by G. Choudhary; magnified 30x (left) and 45x (right).

9 'Nail-Head' Spicule Inclusions in Natural Gemstones www.gem-passion.com

Natural Diamond
Because diamonds form at conditions of very high temperature and pressure, they do not
contain fluid inclusions that are resolvable with a gemmological microscope. However,
this diamond possessed several crystal inclusions with stress cracks (figure 12) that at
certain angles appeared to be short needles associated with a crystal. The combination
gave a strong resemblance to nail-head spicules. These features were mainly
o e t ated ea the o i a do di e tio s. The dia o d s atu al o igi was
ascertained by the presence of naturals on the girdle.

Figure 12: This diamond contains

some nail-head spicule-like
inclusions that are actually crystals
with stress cracks at one end. Given
the formation conditions of
diamond, true nail-head inclusions
are not possible. Photomicrograph
by C. Golecha; magnified 30x

Rock Crystal Quartz

Scattered inclusions consisting of whitish aggregates were concentrated along two
parallel planes in this stone (figure 13). The scene resembled the 'breadcrumb' inclusions
often present along the seed plate in synthetic quartz. In certain orientations, some of
these whitish clusters closely resembled nail-head spicules (figure 14) and seemed to be
formed by the orientation of crystal inclusions almost perpendicular to each other. At
higher magnification, the clusters proved to be aggregates of a whitish mineral (figure
15). The morphology of the clusters resembled muscovite flakes (Gübelin and Koivula,
2005), but we could not conclusively identify them due to lack of access to Raman
spectroscopy.

10 'Nail-Head' Spicule Inclusions in Natural Gemstones www.gem-passion.com

Figure 13: Inclusions are concentrated along two Figure 14: The aggregation patterns of these
parallel planes in this faceted quartz. The pattern inclusions in quartz strongly resemble nail-head
resembles a common inclusion scene in synthetic spicules at certain orientations. Photomicrograph
quartz: "breadcrumbs" along a seed plate. by C. Golecha, magnified 35x
Photomicrograph by C. Golecha , magnified 15x

Figure 15: At higher magnification,

the inclusions in figure 14 proved to
be aggregates of natural mineral,
possibly muscovite.
Photomicrograph by C. Golecha,
magnified 45x

Further analysis with FTIR spectroscopy showed absorptions in the 3600-3000 cm-
1
region, along with a strong peak at 3483 cm-1 that is characteristic for natural crystalline
quartz. Similar spectra were recorded parallel and perpendicular to the optic axis, with
only minor differences in the intensity of the peaks.
Although the pattern of the whitish crystal aggregates indicated a natural
specimen, the presence of spicule-like inclusions and the concentration of the inclusions
11 'Nail-Head' Spicule Inclusions in Natural Gemstones www.gem-passion.com
along a defined plane could have lead to the stone's misidentification as synthetic
without careful examination.

CONCLUSIONS
Nail-head spicule inclusions have long been associated with hydrothermally grown
synthetic gem materials. Such inclusions indicate a rapid, disturbed growth, which is the
case for most synthetics but also for some natural gems. Similar appearing inclusions may
be produced by a combination of other features. Much like the spiral 'fingerprint'
inclusions that were once considered characteristic of Biron synthetic emerald (Gübelin
and Koivula, 1986), the mere appearance of nail-head spicules should not be considered
conclusive proof of synthetic origin. When such inclusions or similar structures are
present, a more detailed examination is necessary to determine the nature of the
sample. Such instances serve us reminders of the importance of not relying on any one
feature for the identification of a gem material.

REFERENCES
Chapman. J. (1992) Letters: Hollow Hexagonal Columns in diamond Not Etch Pits. Gems &
Gemology, Vol. 28, No.1, pp 73
Choudhary G. (2005) Gem News International: An unusual emerald with conical growth
features. Gems & Gemology, Vol. 41, No. 3, pp. 265–266.
DelRe N. (1992) Gem Trade Lab Notes: Emerald. Gems & Gemology, Vol. 28, No. 1, pp.
54–55.
Gubelin .E J. & Koivula. J.I. (1974). Internal World of Gemstones, ABC Verlag, Zurich
Gubelin .E J. & Koivula. J.I. (1986). Photoatlas of Inclusions in Gemstones, ABC Edition,
Zurich.
Gubelin .E J. & Koivula. J.I. (2005). Photoatlas of Inclusions in Gemstones, Volume 2,
Opinio Publishers, Basel, Switzerland
Hughes. R.W. (1997) Ruby & Sapphire, RWH Publishing, Boulder, USA
Kane.R.E. & Liddicoat R.T., (1985) The Biron Hydrothermal Synthetic Emerald, Gems &
Gemology, Vol. 21, No.3 pp 156- 170

12 'Nail-Head' Spicule Inclusions in Natural Gemstones www.gem-passion.com

Kiefert.L., Schmetzer.K., Krzemnicki. M. S., Bernhardt. H. J., Hanni. H.A., (1996) Sapphires
from Andranondambo area, Madagascar, Journal of Gemmology, Vol. 25, No. 3
Laurs.B.M., simmons.W.B., Rossman.G.R., Quinn. E.P., Mcclure.s.F., Peretti.A.,
Armbuster.T., Howthorne.F.C., Falster. A.V., Gunther. D., Cooper.M.A.,
Geobety.B., (2003) Pezzottaite from Ambatovita, Madagascar: a New Gem
Mineral, Gems & Gemology, Vol. 39, No. 4, pp 284- 301.
Liddicoat. R. T. (1993) Handbook of Gem Identification, Gemological Institute of America,
Santa Monica, California
Milisenda.C.C & Henn.U. (1996), Compositional characteristics of sapphires from a new
find in Madagascar, Journal of Gemmology, Vol 25, No. 3, pg 177- 184.
Nassau. K. (1980). Gems made by man. Gemological Institute of America, Santa Monica,
California
Rockwell K. (2003) Lab Notes: Natural emerald with abundant nail-head spicules. Gems &
Gemology, Vol. 39, No. 4, pp.316–317.
Schmetzer. K.(1988) Characterization of Russian hydrothermally- grown synthetic
emeralds, Journal of Gemmology, Vol 21, No.3, pp 162
Schmetzer.K., Kiefert.L., Bernhardt.H., Beili. Z., (1997) Characterization of Chinese
Hydrothermal Synthetic Emerald, Gems & Gemology, Vol. 33, No. 4, pp 276-291
Schmetzer.K., Kiefert.L., Bernhardt.H.J., Multicomponent inclusions in nacken synthetic
emeralds (1999), Journal of Gemmology, Vol 26, No. 8, pg 487-500.
Sechos. B., Identifying Characteristics of Hydrothermal Synthetics (1997) The Australian
Gemmologist, Vol 19, No. 9, pp 383-388.
Shigley.J.E., McClure.S.F., Cole.J.E., Koivula.J.I., Lu. Taijin., Elen.S., Demianets.L.N., (2001)
Hydrothermal Synthetic Red Beryl from the Institute of Crystallography, Moscow,
Gems & Gemology, Vol. 37, No. 1, pp 42- 55
Sinkankas. J (1981) Emerald and Other Beryls, Chilton Book Company, Radnor, USA
Smith C.P. (1991) Gem Trade Lab Notes: Diamond with Hexagonal Indented Natural.
Gems & Gemology, Vol. 27, No. 3, pp 174

13 'Nail-Head' Spicule Inclusions in Natural Gemstones www.gem-passion.com