NIR spectrometry

Pavel Matjka
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
L
o
g
(
1
/
R
)
5000 6000 7000 8000 9000 10000
Wavenumbers (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
A
b
s
o
r
b
a
n
c
e

Wavenumber, cm
-1

NIR Range
Combination
2-nd Overtone
3000
NIR/MIR spectra intensities

Poly styr en NIR
Poly styr ene meas ur ed as a film
0,5
1,0
1,5
2,0
2,5
3,0
3,5
4,0
4,5
A
b
s
o
r
b
a
n
c
e
2000 4000 6000 8000 10000
Wav enumber s ( 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
A
b
s
o
r
b
a
n
c
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
A
b
s
o
r
b
a
n
c
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
A
b
s
o
r
b
a
n
c
e
4300 4320 4340 4360 4380 4400 4420 4440 4460 4480
Wav enumber s ( 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
A
b
s
o
r
b
a
n
c
e
5500 5600 5700 5800 5900 6000
Wav enumber s ( 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
Zrcadlo
Drka pro odstrann
vzduchu
Definovan optick
drha
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 worlds 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