NIR Spectrometry

8/11/2019 NIR Spectrometry

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NIR spectrometry

Pavel Matjka


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NIR spectrometrymolecular absorption/reflection spectrometrynon-destructive method used in process

analysis , QC/ACpractical method that can replace moreexpensive, more time-consuming and more

laboured methods GC, HPLC, titrimetryrelatively fast method for a routine use intechnological applications


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NIR spectrometryqualitative information NIR libraries identification of pure substances and/or

check of pre-defined mixturespharmaceuticals, polymers etc.

quantitative analysis multivariatecalibration models

multi-component analysis - organic, inorganic


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NIR spectrometry

from14 000 cm -1 714 nm

12 500 cm-1

800 nm

12 000 cm -1 833 nm

to4 000 cm -1 2 500 nm

from4 000 cm -1 2 500 nm

to400 cm -1 25 000 nm 200 cm -1 50 000 nm


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NIR spectrometryrelatively broad bands overtones and

combination bands


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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 )

5000600070008000900010000Wavenumbers (cm-1)

Combination

1st Overtone

2nd Overtone

3rd Overtone


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NIR spectra

1000200040006000800010000

3-rd Overtone

1-st Overtone

Fundamentalbands

(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


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NIR/MIR spectra intensities

Poly styren N IRPoly styrene measur 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

200040006000800010000

Wavenumbers (cm-1)

Polystyrene - MIRPolystyrene NIRcommon scale

the intensities are decreasing with increasing

frequency / wavenumber


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NIR spectrometry transmission measurement

cells - various types of glassINFRASIL, SUPRASIL (critical part ~ 4000 cm -1)


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NIR spectrometry transmission measurement

cells - various types of glasspathlength 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 probesfixed pathlength or adjustable pathlength


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NIR spectrometry transmission measurementcells both polar and non-polar samples

organic liquids ( oils, petroleum )aqueous solutions ( drinks content of sugars, ethanol )

Ac eton _5 mmD V Ac eton _1 mmD V Ac eton _2 mmD V

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

45005000550060006500700075008000

cm-1

Acetone various pathlength 5 mm 2 mm 1 mm


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Voda_5mmDVVoda_1mmDVVoda_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

45005000550060006500700075008000

cm-1

NIR spectrometry transmission measurementcells - both polar and non-polar samples

organic liquids ( oils, petroleum )aqueous solutions ( drinks content of sugars, ethanol )

Water 5 mm 2 mm 1 mm


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NIR spectrometry transmission measurementaqueous solutions

calibration model for sugar content in soft drinks


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calibration model for alcoholic drinks


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calibration for alcoholic drinks - spectraNIR-805-02-MPNIR-1-01-MPNIR-1-02-MPNIR-2-01-MPNIR-2-02-MP

NIR-3-01-MPNIR-3-02-MPNIR-4-01-MPNIR-4-02-MPNIR-5-01-MPNIR-5-02-MPNIR-6-01-MPNIR-6-02-MPNIR-7-01-MPNIR-7-02-MPNIR-8-01-MPNIR-8-02-MP

NIR-9-01-MPNIR-9-02-MPNIR-10-01-MPNIR-10-02-MPNIR-11-01-MPNIR-11-02-MPNIR-12-01-MPNIR-12-02-MPNIR-13-01-MPNIR-13-02-MPNIR-14-01-MPNIR-14-02-MPNIR-15-01-MPNIR-15-02-MPNIR-16-01-MPNIR-16-02-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

4300432043404360438044004420444044604480

Wavenumbers (cm-1)

range of combination bands


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NIR-805-02-MPNIR-1-01-MPNIR-1-02-MPNIR-2-01-MPNIR-2-02-MPNIR-3-01-MPNIR-3-02-MPNIR-4-01-MPNIR-4-02-MPNIR-5-01-MPNIR-5-02-MPNIR-6-01-MPNIR-6-02-MPNIR-7-01-MPNIR-7-02-MPNIR-8-01-MPNIR-8-02-MPNIR-9-01-MPNIR-9-02-MPNIR-10-01-MPNIR-10-02-MPNIR-11-01-MPNIR-11-02-MPNIR-12-01-MPNIR-12-02-MPNIR-13-01-MPNIR-13-02-MPNIR-14-01-MPNIR-14-02-MPNIR-15-01-MPNIR-15-02-MPNIR-16-01-MPNIR-16-02-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

550056005700580059006000

Wavenumbers (cm-1)


calibration for alcoholic drinks - spectra

range of 1-st ovetones


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NIR spectrometry transflectance measurement

Petriho miska

Vzorek

ZrcadloDrka pro odstrann vzduchu

Definovan optickdrha

Sample

Definedoptical path

Petri dishMirror

Groove forair removal

transflectancecells

defined

pathlength

transmission/reflection

viscous liquids,pastes


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transflectancecells

variouspathlengths

transmission/reflection

viscous liquids,pastes


MIRRORS


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transflectance cellsfat in the butter



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NIR spectrometry TABLET Analyzer

(Diffuse)Transmission

DiffuseReflectance

Tablet


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NIR spectrometry TABLET Analyzer

tablet analyzerdetermination of active substance in a capsule


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UpDRIFT

absorptionand reflectionson irregularparticles

reflectedradiationcollected

NIR spectrometry diffusereflectance measurement

Sample area


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UpDRIFT

background measurementwith Spectralon (ceramics)direct measurement ofpellets, powders measurement in rotational

cell (glass bottom) powders, granularmaterials, pulps

NIR spectrometry diffusereflectance measurement


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NIR spectrometry fibreoptics probes

remotesensing


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remotesensing

Source of radiationDetector

Light beam

Opticalfibres Immersion

probeOptical

pathlength

SMAconnectors


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IMMERSION PROBESstandard type

Light beam

Prism

Window

Light pathin sample

NIR f


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IMMERSION PROBEStypes for small sampling volumes

Light beam

Prism

Window

Light pathin sample

Window

Light beam

Light pathin sample

Mirror

NIR f b


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IMMERSION PROBEStypes for process analysis

Light beam

Prism

Window

Light pathin sample

NIR f b


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IMMERSION PROBES ATR probe

Sapphireprism

Light beam

NIR fib


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Multiplexer System


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NIR spectrometry some practical applications

ANALYSIS OF FOODSMILK, CHEESES, SOFTDRINKS, WINES etc.

ANALYSIS OF MEDICAMENTSactive 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


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NIR spectrometry instrumentation Nicolet

ANTARIS

NIR


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NIR spectrometry instrumentation Bruker

MPA - multi-purpose analyzer


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i PH ZIR R


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microPH ZIR Rx Handheld Pharmaceutical Material Analysis

The microPHAZIRTM Rx is the worlds first handheld analysis

system designed for rapid on-site pharmaceutical material identificationand analysis.

Diffuse reflectance, optional adapters for liquids

Tungsten light bulb, safe for operators and sampleintegrity

Measurement time several seconds 1600 2400 nm ( cca 6250 4160 cm -1) including the

complete near-infrared combination region and firstovertone region) wolfram bulb light source

Resolution 8 nm per pixel / 12 nm optical

i PH ZIR R


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microPH ZIR Rx

i PH ZIR R


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microPH ZIR Rx

NIR spectrometry practical examples


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http://www.ft-nir.com/


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NIR Spectrometry