near infrared transmission spectroscopy as applied to fats and oil
TRANSCRIPT
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
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NIR –
Vibrational Spectroscopy
Anharmonic Motions
Exist where large and small atoms are bound together
Overtone and Combination Bonds
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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
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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
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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
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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
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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
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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
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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
rb
an
ce
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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
rb
an
ce
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
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Analysis of Oil and Moisture in Olives
Transflectance Spectra: 10mm
Oil SEC = 0.6%, R2 = .95
Moisture SEC 0.9% R2 = .96
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Transmission Spectra of Oils and Fats
NIT Spectra of Tallow
720-1100nm
NIT Spectra of Bio-Diesel
720-1100nm
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Analysis of Total Glycerides in Bio-Deisel
Transmission Spectra: PLS calibration
SEC = 18ppm, R2 = .99
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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
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Ointment Prediction
6 different samples analysed using the PLS calibration model
SEP = 0.4mg/ml
R2 = 0.99
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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.