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NIR spectrometry
Pavel Matějka
NIR spectrometry
molecular absorption/reflection spectrometry
non-destructive method used in process
analysis, QC/AC
practical method that can replace more
expensive, more time-consuming and more
laboured methods – GC, HPLC, titrimetry
relatively fast method for a routine use in
technological applications
NIR spectrometry
qualitative information – NIR libraries –
identification of pure substances and/or
check of pre-defined mixtures
pharmaceuticals, polymers etc.
quantitative analysis – multivariate
calibration models
multi-component analysis - organic, inorganic
NIR spectrometry
from
14 000 cm-1 714 nm
12 500 cm-1 800 nm
12 000 cm-1 833 nm
to
4 000 cm-1 2 500 nm
from
4 000 cm-1 2 500 nm
to
400 cm-1 25 000 nm
200 cm-1 50 000 nm
NIR spectrometry
relatively broad bands – overtones and
combination bands
NIR spectra
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
Lo
g(1
/R)
500 0 600 0 700 0 800 0 900 0 100 00
Wav en umbers (cm-1)
Combination
1st Overtone
2nd Overtone
3rd Overtone
NIR spectra
1000 2000 4000 6000 8000 10000
3-rd Overtone
1-st Overtone
Fundamental bands
(Mid IR) 1
0.5
Ab
so
rba
nce
Wavenumber, cm-1
NIR Range
Combination
2-nd Overtone
3000
NIR/MIR spectra intensities
Po ly s ty ren NIR
Po ly s ty rene meas ured as a film
0,5
1,0
1,5
2,0
2,5
3,0
3,5
4,0
4,5
Ab
so
rba
nc
e
2000 4000 6000 8000 10000
Wav enumbers (cm-1)
Polystyrene - MIR
Polystyrene – NIR
common scale
the intensities are decreasing with increasing
frequency / wavenumber
NIR spectrometry –
transmission measurement
cells - various types of glass
INFRASIL, SUPRASIL (critical part ~ 4000 cm-1)
NIR spectrometry –
transmission measurement
cells - various types of glass
pathlength 1 – 5 (10) mm
effect of solvent absorption
effect of selected subregion (combination bands, order of overtones)
effect of concentrations of analytes studied
fiber optics probes
fixed pathlength or adjustable pathlength
NIR spectrometry –
transmission measurement
cells – both polar and non-polar samples organic liquids (oils, petroleum)
aqueous solutions (drinks – content of sugars, ethanol) Ac eton_5mmDV
Ac eton_1mmDV
Ac eton_2mmDV
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
Ab
so
rba
nc
e
4500 5000 5500 6000 6500 7000 7500 8000
cm-1
Acetone – various pathlength
• 5 mm
• 2 mm
• 1 mm
Voda_5mmDV
Voda_1mmDV
Voda_2mmDV
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
Ab
so
rba
nc
e
4500 5000 5500 6000 6500 7000 7500 8000
cm-1
NIR spectrometry –
transmission measurement
cells - both polar and non-polar samples organic liquids (oils, petroleum)
aqueous solutions (drinks – content of sugars, ethanol)
Water
• 5 mm
• 2 mm
• 1 mm
NIR spectrometry –
transmission measurement
aqueous solutions calibration model for sugar content in soft drinks
NIR spectrometry –
transmission measurement
aqueous solutions calibration model for alcoholic drinks
NIR spectrometry –
transmission measurement
aqueous solutions calibration for alcoholic drinks - spectra
NIR-805 -02 -MP
NIR-1-01-MP
NIR-1-02-MP
NIR-2-01-MP
NIR-2-02-MP
NIR-3-01-MP
NIR-3-02-MP
NIR-4-01-MP
NIR-4-02-MP
NIR-5-01-MP
NIR-5-02-MP
NIR-6-01-MP
NIR-6-02-MP
NIR-7-01-MP
NIR-7-02-MP
NIR-8-01-MP
NIR-8-02-MP
NIR-9-01-MP
NIR-9-02-MP
NIR-10-01-MP
NIR-10-02-MP
NIR-11-01-MP
NIR-11-02-MP
NIR-12-01-MP
NIR-12-02-MP
NIR-13-01-MP
NIR-13-02-MP
NIR-14-01-MP
NIR-14-02-MP
NIR-15-01-MP
NIR-15-02-MP
NIR-16-01-MP
NIR-16-02-MP
NIR-17-01-MP
NIR-17-02-MP
NIR-18-01-MP
NIR-18-02-MP
NIR-19-01-MP
NIR-19-02-MP
NIR-20-01-MP
NIR-20-02-MP
NIR-21-01-MP
NIR-21-02-MP
NIR-22-01-MP
NIR-22-02-MP
NIR-23-01-MP
NIR-23-02-MP
NIR-24-01-MP
NIR-24-02-MP
NIR-25-01-MP
NIR-25-02-MP
NIR-26-01-MP
NIR-26-02-MP
NIR-27-01-MP
NIR-27-02-MP
NIR-28-01-MP
NIR-28-02-MP
NIR-105 -01 -MP
NIR-105 -02 -MP
NIR-205 -01 -MP
NIR-205 -02 -MP
NIR-205 -01 -MP
NIR-305 -02 -MP
NIR-405 -01 -MP
NIR-405 -02 -MP
NIR-505 -01 -MP
NIR-505 -02 -MP
NIR-605 -01 -MP
NIR-605 -02 -MP
NIR-705 -01 -MP
NIR-705 -02 -MP
NIR-805 -01 -MP
0.85
0.90
0.95
1.00
1.05
1.10
1.15
1.20
1.25
1.30
1.35
Ab
so
rba
nc
e
4300 4320 4340 4360 4380 4400 4420 4440 4460 4480
Wav enumbers (cm-1)
range of combination bands
NIR-805 -02 -MP
NIR-1-01-MP
NIR-1-02-MP
NIR-2-01-MP
NIR-2-02-MP
NIR-3-01-MP
NIR-3-02-MP
NIR-4-01-MP
NIR-4-02-MP
NIR-5-01-MP
NIR-5-02-MP
NIR-6-01-MP
NIR-6-02-MP
NIR-7-01-MP
NIR-7-02-MP
NIR-8-01-MP
NIR-8-02-MP
NIR-9-01-MP
NIR-9-02-MP
NIR-10-01-MP
NIR-10-02-MP
NIR-11-01-MP
NIR-11-02-MP
NIR-12-01-MP
NIR-12-02-MP
NIR-13-01-MP
NIR-13-02-MP
NIR-14-01-MP
NIR-14-02-MP
NIR-15-01-MP
NIR-15-02-MP
NIR-16-01-MP
NIR-16-02-MP
NIR-17-01-MP
NIR-17-02-MP
NIR-18-01-MP
NIR-18-02-MP
NIR-19-01-MP
NIR-19-02-MP
NIR-20-01-MP
NIR-20-02-MP
NIR-21-01-MP
NIR-21-02-MP
NIR-22-01-MP
NIR-22-02-MP
NIR-23-01-MP
NIR-23-02-MP
NIR-24-01-MP
NIR-24-02-MP
NIR-25-01-MP
NIR-25-02-MP
NIR-26-01-MP
NIR-26-02-MP
NIR-27-01-MP
NIR-27-02-MP
NIR-28-01-MP
NIR-28-02-MP
NIR-105 -01 -MP
NIR-105 -02 -MP
NIR-205 -01 -MP
NIR-205 -02 -MP
NIR-205 -01 -MP
NIR-305 -02 -MP
NIR-405 -01 -MP
NIR-405 -02 -MP
NIR-505 -01 -MP
NIR-505 -02 -MP
NIR-605 -01 -MP
NIR-605 -02 -MP
NIR-705 -01 -MP
NIR-705 -02 -MP
NIR-805 -01 -MP
0.30
0.31
0.32
0.33
0.34
0.35
0.36
0.37
0.38
0.39
0.40
Ab
so
rba
nc
e
5500 5600 5700 5800 5900 6000
Wav enumbers (cm-1)
NIR spectrometry –
transmission measurement
aqueous solutions calibration for alcoholic drinks - spectra
range of 1-st ovetones
NIR spectrometry –
transflectance measurement
Petriho miska
Vzorek
ZrcadloDrážka pro odstranění vzduchu
Definovaná optická dráha
Sample
Defined
optical path
Petri dish
Mirror Groove for air removal
transflectance
cells defined
pathlength
transmission/
reflection
viscous liquids,
pastes
transflectance cells
various
pathlengths
transmission/ reflection
viscous liquids, pastes
NIR spectrometry –
transflectance measurement
MIRRORS
transflectance cells fat in the butter
NIR spectrometry –
transflectance measurement
NIR spectrometry –
TABLET Analyzer
(Diffuse)
Transmission
Diffuse
Reflectance
Tablet
NIR spectrometry –
TABLET Analyzer
tablet analyzer determination of active substance in a capsule
UpDRIFT
absorption and reflections on irregular particles reflected
radiation collected
NIR spectrometry – diffuse
reflectance measurement
Sample area
UpDRIFT
background measurement
with Spectralon (ceramics)
direct measurement of
pellets, powders …
measurement in rotational
cell (glass bottom) –
powders, granular
materials, pulps …
NIR spectrometry – diffuse
reflectance measurement
NIR spectrometry – fibre
optics probes
remote
sensing
NIR spectrometry – fibre
optics probes
remote
sensing
Source of radiation Detector
Light beam
Optical fibres Immersion
probe
Optical pathlength
SMA connectors
NIR spectrometry – fibre
optics probes
IMMERSION PROBES
standard type
Light beam
Prism
Window
Light path in sample
NIR spectrometry – fibre
optics probes
IMMERSION PROBES
types for small sampling volumes
Light beam
Prism
Window
Light path in sample
Window
Light beam
Light path in sample
Mirror
NIR spectrometry – fibre
optics probes
IMMERSION PROBES
types for process analysis
Light beam
Prism
Window
Light path in sample
NIR spectrometry – fibre
optics probes
IMMERSION PROBES
ATR probe
Sapphire prism
Light beam
NIR spectrometry – fibre
optics probes
Multiplexer System
NIR spectrometry –
some practical applications
ANALYSIS OF FOODS
MILK, CHEESES, SOFTDRINKS, WINES etc.
ANALYSIS OF MEDICAMENTS
active substances in tablets, plant extracts etc.
ANALYSIS OF POLYMERS
quality control of products, additives etc.
ANALYSIS OF PETROCHEMICAL PRODUCTS
content of aromates, octane number etc.
NIR spectrometry –
instrumentation Nicolet
ANTARIS
NIR spectrometry –
instrumentation Bruker
MPA - multi-purpose analyzer
NIR spectrometry –
instrumentation
various probes for technologies
microPHAZIR Rx
Handheld Pharmaceutical Material Analysis
The microPHAZIRTM Rx is the world’s first handheld analysis
system designed for rapid on-site pharmaceutical material identification
and analysis.
• Diffuse reflectance, optional adapters for liquids
• Tungsten light bulb, safe for operators and sample integrity
• Measurement time – several seconds
• 1600 – 2400 nm ( cca 6250 – 4160 cm-1) including the complete near-infrared combination region and first overtone region) – wolfram bulb – light source
• Resolution – 8 nm per pixel / 12 nm optical
microPHAZIR Rx
microPHAZIR Rx
NIR spectrometry – practical examples
NIR spectrometry – practical examples
NIR spectrometry – practical examples