Advanced Laboratory Instruments
Diploma-level awareness of FTIR, UV-Vis-NIR, Raman, EDXRF, LA-ICP-MS, and photoluminescence spectroscopy – what each detects and its key gemmological applications.
Introduction
This page covers the five principal advanced laboratory instruments encountered at Diploma
level. Students need awareness-depth knowledge only: what each instrument detects, its key
gemmological applications, and its cost and availability constraints. Operational training
is outside the scope of the FGA examination.
These instruments are available at major gem laboratories (GIA, Gübelin, SSEF, Gem-A
Laboratory, AGL) and increasingly at larger trade houses. They are not field instruments.
FTIR Spectroscopy
Fourier Transform Infrared (FTIR) spectroscopy irradiates the sample with a broadband
infrared beam – mid-IR (4000–400 cm⁻¹) or near-IR (10000–4000 cm⁻¹). Chemical bonds
absorb IR radiation at characteristic frequencies; the resulting absorption pattern identifies
molecular functional groups and crystal lattice vibrations.
FTIR is the primary tool for detecting filler substances, polymer impregnation, and
diamond nitrogen aggregation states at major gem laboratories.
Key Gemmological Applications
Emerald oil and resin detection: Natural fractures in emerald are commonly filled
with cedar oil, synthetic resins (Opticon), or epoxy. Each filler produces
characteristic IR absorption peaks distinct from the host beryl spectrum. Kiefert
et al. (2000) demonstrated that FTIR identifies the filler type (oil vs resin vs epoxy)
by peak position: Journal of Gemmology 26, 501–520 (DOI: 10.15506/jog.1999.26.8.501)
[VERIFIED].Jadeite polymer treatment (Type B jade): Bleached and polymer-impregnated jadeite
shows characteristic C–H and C=O absorption bands in the mid-IR that are absent in
untreated (Type A) jadeite. Tan et al. (2013) confirmed FTIR distinguishes treated from
untreated jade: COSMOS journal (DOI: 10.1142/s0219607713500031) [VERIFIED].Diamond type classification: FTIR distinguishes Type Ia (nitrogen in aggregates –
A and B centres), Type Ib (isolated nitrogen), Type IIa (nitrogen-free), and Type IIb
(boron-bearing, electrically conductive) by nitrogen absorption features in the mid-IR
one-phonon region (~1000–1300 cm⁻¹). Type IIa diamonds lack nitrogen absorptions and
are more likely candidates for HPHT treatment or CVD synthesis – triggering further
investigation.Heat treatment indicator in sapphire: Delaunay (2024) showed that the 3232 cm⁻¹
FTIR band provides new insights for identifying heat treatment in metamorphic-type blue
sapphires: Journal of Gemmology 39(1) (DOI: 10.15506/jog.2024.39.1.33) [VERIFIED].
UV-Vis-NIR Spectrophotometry
UV-Vis-NIR spectrophotometry records absorption across the ultraviolet (200–400 nm),400–700 nm), and near-infrared (~700–2500 nm) spectrum with high wavelength
visible (
resolution and quantitative transmission data.
It identifies chromophores and quantifies their concentrations more precisely than the
desk spectroscope. It can detect colour-related treatments and provide origin indicators.
Key Gemmological Applications
Beryllium-diffused sapphire detection: Emmett et al. (2003) described UV-Vis-NIR
signatures associated with beryllium diffusion – the process causes orange colouration
in corundum through Fe³⁺–O²⁻ charge transfer bands in the UV, producing a reduction
in blue absorption and strengthening of an absorption feature near 390 nm: Gems &
Gemology 39(2), 84–135 (DOI: 10.5741/gems.39.2.84) [VERIFIED]. Be diffusion is
confirmed definitively only by LA-ICP-MS (see below) – UV-Vis-NIR provides supporting
evidence.Chromophore quantification: Distinguishes iron-coloured from chromium-coloured
stones by the shape and position of absorption bands; quantifies relative contributions
of Fe²⁺, Fe³⁺, Cr³⁺, and IVCT mechanisms.Origin indicators: The relative intensities of iron absorption bands in sapphire
correlate with geological source (basaltic vs metamorphic origin) when combined with
trace element data.
Raman Spectroscopy
Raman spectroscopy uses laser excitation (typically 532 nm or 785 nm) to generate
inelastic light scattering (Raman shift). The frequency shifts are characteristic of
molecular bond vibrations and lattice phonon modes, providing a unique molecular fingerprint.
Raman is non-destructive and can be performed through glass or immersion media using a
confocal micro-probe – making it ideal for inclusion identification without opening cavities
or damaging the host.
Key Gemmological Applications
Inclusion identification without destruction: The Raman spectrum of a solid inclusion
(calcite, apatite, rutile, zircon, pyrite) inside a gemstone can be measured through the
host stone using a confocal Raman micro-probe. Nassau (1981) was among the earliest to
demonstrate "Raman Spectroscopy as a Gemstone Test": Journal of Gemmology 17(5), 306–320
(DOI: 10.15506/jog.1981.17.5.306) [VERIFIED].Filler identification in emerald: Kiefert et al. (2000) used both IR and Raman to
identify filler substances in emeralds; Raman provides complementary data to FTIR for
distinguishing oil types (DOI: 10.15506/jog.1999.26.8.501).Jade species determination: Raman spectra of nephrite and jadeite are distinct; Tan
et al. (2013) confirmed Raman and FTIR together reliably separate the two jade species
(DOI: 10.1142/s0219607713500031).Rapid portable screening: Tsai et al. (2023) reported rapid gem mineral
identification using portable Raman: Journal of Raman Spectroscopy
(DOI: 10.1002/jrs.6518) [VERIFIED].
EDXRF and LA-ICP-MS (Trace Element Analysis)
These two complementary techniques provide elemental analysis for origin fingerprinting
and treatment detection. They are the workhorses of modern origin determination
at major gem laboratories.
EDXRF – Non-Destructive Elemental Survey
Energy-Dispersive X-ray Fluorescence (EDXRF): An X-ray beam causes emission of
characteristic secondary X-rays from elements in the sample, providing non-destructive
elemental analysis down to ppm levels for elements with atomic number ≥ 11 (sodium).
- Non-destructive; no sample preparation required.
- Cannot detect elements below atomic number ~11 in standard configurations.
- Cannot detect beryllium (atomic number 4) – this is a critical limitation for
Be-diffusion treatment detection; only LA-ICP-MS can routinely detect Be. - Schmetzer et al. (2009) used EDXRF for gem corundum origin fingerprinting: Gems &
Gemology 45(4), 264 (DOI: 10.5741/gems.45.4.264) [VERIFIED].
LA-ICP-MS – Ultra-Trace Element Fingerprinting
Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS): A laser
micro-beam ablates a tiny spot (10–100 µm); the ablated material is carried into an ICP
plasma and analysed by mass spectrometry, providing trace and ultra-trace element data
to ppb levels. Micro-destructive – leaves a tiny ablation pit.
- Origin fingerprinting in corundum: Basaltic-origin sapphires (Australia,
Thailand/Cambodia, Nigeria) have high Fe (>5000 ppm), high Ga/Al ratios, and are
essentially Cr-free. Metamorphic-origin sapphires (Kashmir, Sri Lanka, Myanmar) have
lower Fe, measurable Cr, higher Mg, and lower Ga. Sutherland et al. (2014) advanced
trace element fingerprinting for gem corundum using LA-ICP-MS and EDXRF: Minerals
5(1) (DOI: 10.3390/min5010061) [VERIFIED]. - Beryllium detection: Only LA-ICP-MS can routinely detect Be (atomic number 4),
making it the definitive test for Be diffusion treatment. Emmett et al. (2003) confirmed
this (DOI: 10.5741/gems.39.2.84). - Limitation: Requires certified reference materials for calibration; results
depend on reference database quality for origin assignment.
Photoluminescence at 77 K
Photoluminescence (PL) spectroscopy uses a laser to excite electronic transitions in the
sample. The emitted luminescence spectrum reveals specific defect centres and impurities.
Cooling to liquid-nitrogen temperature (77 K) dramatically narrows spectral lines,
resolving features that overlap at room temperature. PL at 77 K is used principally for
diamond identification and treatment detection.
Key Diamond Applications
HPHT-treated Type IIa diamonds: HPHT treatment converts brown Type Ia diamonds to
near-colourless Type IIa stones by dissolving nitrogen aggregates. At 77 K, PL reveals
the presence or absence of the 637 nm NV⁰ centre (neutral nitrogen-vacancy) and the
575 nm NV⁻ centre (negatively charged NV). Lim et al. (2010) demonstrated
discrimination between natural and HPHT-treated Type IIa diamonds using PL: Diamond and
Related Materials 19(10), 1254–1258 (DOI: 10.1016/j.diamond.2010.06.007) [VERIFIED].CVD synthetic diamond: Willems et al. (2011) explored luminescent regions in CVD
synthetic diamond using PL – CVD diamonds show characteristically different luminescence
patterns related to their growth sectors: Gems & Gemology 47(3), 202–207
(DOI: 10.5741/gems.47.3.202) [VERIFIED].H3 and NV centre discrimination: The presence of H3 (504 nm), NV⁻ (637 nm), and
their relative intensities at 77 K can distinguish HPHT-treated from natural fancy-colour
diamonds. Natural Type IIa diamonds have a characteristic PL signature distinct from
HPHT-treated Type Ia stones.
Sources
Key citations for this topic:
- Smith, B. et al. (2000). "Identification of filler substances in emeralds by IR and Raman."
Journal of Gemmology 26, 501–520. DOI: 10.15506/jog.1999.26.8.501 [VERIFIED] - Kiefert, L. et al. (2000). Same as above (Kiefert is a co-author in the original Smith et
al. G&G citation). - Tan, T. L. et al. (2013). "Nephrite and jadeite by FTIR and Raman." COSMOS.
DOI: 10.1142/s0219607713500031 [VERIFIED] - Delaunay (2024). "Heat Treatment in Metamorphic-type Blue Sapphires FTIR." Journal of
Gemmology 39(1). DOI: 10.15506/jog.2024.39.1.33 [VERIFIED] - Emmett, J. L. et al. (2003). "Beryllium Diffusion of Ruby and Sapphire." Gems &
Gemology 39(2), 84–135. DOI: 10.5741/gems.39.2.84 [VERIFIED] - Nassau, K. (1981). "Raman Spectroscopy as a Gemstone Test." Journal of Gemmology
17(5), 306–320. DOI: 10.15506/jog.1981.17.5.306 [VERIFIED] - Tsai et al. (2023). "Rapid gemstone mineral identification using portable Raman."
Journal of Raman Spectroscopy. DOI: 10.1002/jrs.6518 [VERIFIED] - Sutherland, F. et al. (2014). "Trace Element Fingerprinting of Gem Corundum." Minerals
5(1). DOI: 10.3390/min5010061 [VERIFIED] - Schmetzer, K. et al. (2009). Gems & Gemology 45(4), 264.
DOI: 10.5741/gems.45.4.264 [VERIFIED] - Guillong et al. (2008). Geostandards and Geoanalytical Research.
DOI: 10.1111/j.1751-908X.2008.00875.x [VERIFIED] - Lim, H. et al. (2010). "Discrimination of natural vs HPHT-treated Type IIa diamonds by PL."
Diamond and Related Materials 19(10), 1254–1258.
DOI: 10.1016/j.diamond.2010.06.007 [VERIFIED] - Willems, B. et al. (2011). "Luminescent Regions in CVD Synthetic Diamond." Gems &
Gemology 47(3), 202–207. DOI: 10.5741/gems.47.3.202 [VERIFIED] - Hainschwang, T. et al. (2012). Gems & Gemology 48(4), 252.
DOI: 10.5741/gems.48.4.252 [VERIFIED]