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

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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