8/3/2009

NEAR INFRARED TRANSMISSION

SPECTROSCOPY AS APPLIED TO

FATS AND OIL

Phillip J. Clancy, NIR Technology Systems,

56 Kitchener Pde, Bankstown, NSW, Australia.

8/3/2009

Near Infrared Transmission (NIT)

Spectroscopy

Oil Seeds: Soybean, Canola, Corn, Olives Oil,

Moisture, Protein

Vegetable Oils: Iodine Value, Peroxide Value, Free Fatty

Acids, Moisture

Fats: Tallow Free Fatty Acids, Moisture

Foods: Dairy, Meat, Margarine Fat, Moisture,

Protein

Cosmetics and Pharmaceuticals: Creams and Lotions Lanolin, Moisture

8/3/2009

NIR –

Vibrational Spectroscopy

Anharmonic Motions

Exist where large and small atoms are bound together

Overtone and Combination Bonds

8/3/2009

NIR Spectral Region

Chemical Bonds in NIR

Carbon-Hydrogen

Nitrogen-Hydrogen

Oxygen-Hydrogen

Restrictions >1% concentrations

Does the chemical entity contain C-H, O-H or N-H

Can you present the sample to the NIR Analyser

Ideal for: Agricultural products

Food products

Cosmetics

Natural products

8/3/2009

NIR region – 700-2500nm

3 regions of the NIR Spectrum Transflectance Transmission Reflectance

CH

HOH

CH OH NH OHCH

CH

CH2

HOH

CH3

OHNH

Ar-CH

CH2

CH3

HOH

NH

OH OH

NH

Ar-CHCH

CH2 CH3

3rd Overtone 1st & 2nd Overtone Region Combination Region

1000 1250 1500 1750 2000 2250 2400700

8/3/2009

Technology Description

Transmission

Lamp

Sample

Optics –

Diffraction

Grating

Detector

P0 P

The Beer-Lambert Law

P

PbcA olog A=absorbance ε=absorptivity

b=pathlength c=concentration

8/3/2009

Near Infrared Transmission (NIT)

Spectroscopy - Transflectance

Sample = Oil Seeds, Food, Creams, Ointments, Lotions

Light passes through a sample by reflecting off the particles. NIR energy is absorbed by N-H, C-H and O-H bonds

Transflectance 720 to 1100nm, 3rd overtone region

8/3/2009

Near Infrared Transmission (NIT)

Spectroscopy - Transmission

Light passes thru a clear liquid sample with no deflection of the light. Protein, alcohol, fat etc absorb light directly proportional to concentration.

Transmission 720-2500nm, 1st, 2nd, 3rd Overtones and Combination Regions

8/3/2009

Series 2000 Near Infrared

Transmission Analysers

Diode Array Spectrometers

720-1100nm

Multiple Sample Cells

- Solids, Liquids, Powders and Suspensions

Simple to use

Suitable for laboratory and at line applications

8/3/2009

Transflectance Spectra of Oil Seeds

NIT Spectra of Canola

10mm Cell: 720 to 1100nm NIT Spectra of Soybean

28mm Cell: 720 to 1100nm

Soy Bean Spectra

2

2.2

2.4

2.6

2.8

3

3.2

1 3 5 7 9

11

13

15

17

19

21

23

25

27

29

31

33

35

37

Pixel

Ab

so

rb

an

ce

Canola Seeds

0

0.5

1

1.5

2

2.5

3

3.5

4

4.5

5

1 3 5 7 9

11

13

15

17

19

21

23

25

27

29

31

33

35

37

Wavelength(Pixels)

Ab

so

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ce

8/3/2009

Transflectance Spectra of Foods

NIT Spectra of

Milk Powder720 to 1100nm

Minced Beef Spectra

1.5

2

2.5

3

3.5

4

1 3 5 7 9

11

13

15

17

19

21

23

25

27

29

31

33

35

37

Pixels

Ab

so

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NIT Spectra of Minced Beef

720 to 1100nm

Used for analysis of high fat and

high water content samples.

Milk Powder Blend

2

2.5

3

3.5

4

1 4 7

10

13

16

19

22

25

28

31

34

37

Wavelength

Ab

so

rb

an

ce

8/3/2009

Analysis of Oil and Moisture in Olives

Transflectance Spectra: 10mm

Oil SEC = 0.6%, R2 = .95

Moisture SEC 0.9% R2 = .96

8/3/2009

Transmission Spectra of Oils and Fats

NIT Spectra of Tallow

720-1100nm

NIT Spectra of Bio-Diesel

720-1100nm

8/3/2009

Analysis of Total Glycerides in Bio-Deisel

Transmission Spectra: PLS calibration

SEC = 18ppm, R2 = .99

8/3/2009

Analysis of Free Fatty Acids in Tallow

Transflectance Spectra: 10mm Cell

SEP = 0.15%, R2 = .99

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Pharmaceutical Application

Absorbance spectra of

dermatology ointment

Second Derivative spectra of

dermatology ointment

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Ointment Calibration

10 samples from 3 batches scanned 4times each = 40 spectra.

Reference = HPLC method for Active component.

PLS calibration using 2nd Derivative spectral transformation.

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Ointment Calibration

Active A

SEC = 0.7mg/ml

R2 = 0.82

Note the very narrow range =

99 to 104mg/ml

8/3/2009

Ointment Prediction

6 different samples analysed using the PLS calibration model

SEP = 0.4mg/ml

R2 = 0.99

8/3/2009

Conclusion

NIT Spectroscopy proves to be a rapid and simple means of analysing a broad range of materials containing Oils and Fats.

Transflectance provides a means of measuring oils in complex and very dense materials such as dairy, meat, olives etc.

Transmission provides a means of measuring properties of oils and fats such as Iodine Value, Peroxide Value and Free Fatty Acids.