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

from
4 000 cm-1 2 500 nm

to

to

4 000 cm-1 2 500 nm

400 cm-1 25 000 nm

200 cm-1 50 000 nm

NIR spectrometry
relatively broad bands overtones and

combination bands

NIR spectra
Combination
0.9

1st Overtone

0.8

2nd Overtone

0.7

Lo g(1/R )

0.6

0.5

3rd Overtone

0.4

0.3

0.2

0.1

100 00

900 0

800 0
700 0
Wav en umbers (cm-1)

600 0

500 0

NIR spectra
Fundamental
bands
(Mid IR)

Absorbance

NIR Range
0.5

Combination
1-st Overtone
2-nd Overtone

3-rd Overtone
10000

8000

6000

4000

3000

Wavenumber, cm-1

2000

1000

NIR/MIR spectra intensities

the intensities are decreasing with increasing

frequency / wavenumber
4,5

4,0

Po ly s ty r en N IR
Po ly s ty r ene meas ur ed as a film

Polystyrene - MIR
Polystyrene NIR

common scale

3,5

Absorbance

3,0

2,5

2,0

1,5

1,0

0,5

100 00

800 0

600 0
W av enu mber s ( c m- 1)

400 0

200 0

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)
6.0 Ac eton_ 5mmD V
Ac eton_ 1mmD V
5.5 Ac eton_ 2mmD V
5.0

4.5

Absorbance

4.0

3.5

Acetone various pathlength

5 mm
2 mm
1 mm

3.0

2.5

2.0

1.5

1.0

0.5

800 0

750 0

700 0

650 0

600 0
c m- 1

550 0

500 0

450 0

NIR spectrometry
transmission measurement
cells - both polar and non-polar samples
organic liquids (oils, petroleum)
aqueous solutions (drinks content of sugars, ethanol)
6.0 Vo da_ 5mmD V
Vo da_ 1mmD V
5.5 Vo da_ 2mmD V

5.0

4.5

Absorbance

4.0

3.5

Water
5 mm
2 mm
1 mm

3.0

2.5

2.0

1.5

1.0

0.5

800 0

750 0

700 0

650 0

600 0
c m- 1

550 0

500 0

450 0

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

Absorbance

aqueous solutions
calibration for alcoholic drinks - spectra
1.35 N IR - 805 -02 -MP
N IR - 1-0 1- MP
N IR - 1-0 2- MP
1.30
N IR - 2-0 1- MP
N IR - 2-0 2- MP
N IR - 3-0 1- MP
1.25
N IR - 3-0 2- MP
N IR - 4-0 1- MP
1.20 N IR - 4-0 2- MP
N IR - 5-0 1- MP
N IR - 5-0 2- MP
1.15 N IR - 6-0 1- MP
N IR - 6-0 2- MP
N IR - 7-0 1- MP
1.10 N IR - 7-0 2- MP
N IR - 8-0 1- MP
N IR - 8-0 2- MP
1.05 N IR - 9-0 1- MP
N IR - 9-0 2- MP
N IR - 10- 01- MP
1.00
N IR - 10- 02- MP
N IR - 11- 01- MP
N IR - 11- 02- MP
0.95
N IR - 12- 01- MP
N IR - 12- 02- MP
0.90 N IR - 13- 01- MP
N IR - 13- 02- MP
N IR - 14- 01- MP
0.85 N IR - 14- 02- MP
N IR - 15- 01- MP
N IR - 1502-0 MP
448
N IR - 16- 01- MP
N IR - 16- 02- MP

range of combination bands

446 0

444 0

442 0

440 0

438 0

W av enu mber s ( c m- 1)

436 0

434 0

432 0

430 0

NIR spectrometry
transmission measurement

Absorbance

aqueous solutions
calibration for alcoholic drinks - spectra
0.40 N IR - 805 -02 -MP
N IR - 1-0 1- MP
N IR - 1-0 2- MP
0.39 N IR - 2-0 1- MP
N IR - 2-0 2- MP
N IR - 3-0 1- MP
0.38
N IR - 3-0 2- MP
N IR - 4-0 1- MP
N IR - 4-0 2- MP
0.37
N IR - 5-0 1- MP
N IR - 5-0 2- MP
0.36 N IR - 6-0 1- MP
N IR - 6-0 2- MP
N IR - 7-0 1- MP
0.35 N IR - 7-0 2- MP
N IR - 8-0 1- MP
N IR - 8-0 2- MP
0.34
N IR - 9-0 1- MP
N IR - 9-0 2- MP
0.33 N IR - 10- 01- MP
N IR - 10- 02- MP
N IR - 11- 01- MP
0.32 N IR - 11- 02- MP
N IR - 12- 01- MP
N IR - 12- 02- MP
0.31 N IR - 13- 01- MP
N IR - 13- 02- MP
N IR - 14- 01- MP
0.30
N IR - 14- 02- MP
N IR - 15- 01- MP
N IR0- 15- 02- MP
600
N IR - 16- 01- MP
N IR - 16- 02- MP

range of 1-st ovetones

590 0

580 0

570 0
W av enu mber s ( c m- 1)

560 0

550 0

NIR spectrometry
transflectance measurement
transflectance

cells

defined
pathlength

transmission/
reflection

viscous liquids,
pastes

Zrcadlo
Mirror
Petriho
miska
Petri dish

Vzorek
Sample

Drka
Groovepro
forodstrann
vzduchu
air removal

Defined
Definovan
optick
optical
path
drha

NIR spectrometry

transflectance measurement
transflectance

cells

various
pathlengths

transmission/
reflection

viscous liquids,
pastes
MIRRORS

NIR spectrometry

transflectance measurement
transflectance cells
fat in the butter

NIR spectrometry
TABLET Analyzer
(Diffuse)
Transmission

Tablet
Diffuse
Reflectance

NIR spectrometry
TABLET Analyzer

tablet analyzer
determination of active substance in a capsule

NIR spectrometry diffuse

reflectance measurement

UpDRIFT

absorption

and reflections
on irregular
particles

reflected
radiation
collected

Sample area

NIR spectrometry diffuse

reflectance measurement

UpDRIFT

background measurement
with Spectralon (ceramics)
direct measurement of
pellets, powders
measurement in rotational
cell (glass bottom)
powders, granular
materials, pulps

NIR spectrometry fibre

optics probes
remote

sensing

NIR spectrometry fibre

optics probes
remote

sensing
SMA
connectors
Light beam

Source of radiation

Detector

Optical
fibres

Immersion
probe
Optical
pathlength

NIR spectrometry fibre

optics probes
IMMERSION PROBES

standard type
Window

Light path
in sample
Prism

Light beam

NIR spectrometry fibre

optics probes
IMMERSION PROBES

types for small sampling volumes

Window
Light path
in sample
Prism

Window
Light path
in sample
Light beam
Mirror

Light beam

NIR spectrometry fibre

optics probes
IMMERSION PROBES

types for process analysis

Window

Light path
in sample
Prism

Light beam

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