NEAR INFRARED TRANSMISSION SPECTROSCOPY AS APPLIED TO FATS AND OIL
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1 NEAR INFRARED TRANSMISSION SPECTROSCOPY AS APPLIED TO FATS AND OIL Phillip J. Clancy, NIR Technology Systems, 56 Kitchener Pde, Bankstown, NSW, Australia.
2 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
3 NIR Vibrational Spectroscopy Anharmonic Motions Exist where large and small atoms are bound together Overtone and Combination Bonds
4 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
5 NIR region nm 3 regions of the NIR Spectrum Transflectance Transmission Reflectance 3 rd Overtone 1 st & 2 nd Overtone Region Combination Region CH 2 CH 3 HOH OH OH Ar-CH CH CH 3 NH NH Ar-CH HOH HOH OH NH CH CH 2 CH CH OH NH OH CH CH 2 CH
6 Technology Description Transmission P0 P Lamp The Beer-Lambert Law Sample Optics Diffraction Grating Detector Po A bc log A=absorbance ε=absorptivity P b=pathlength c=concentration
7 Near Infrared Transmission (NIT) Spectroscopy - Transflectance Transflectance 720 to 1100nm, 3 rd overtone region 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
8 Near Infrared Transmission (NIT) Spectroscopy - Transmission Transmission nm, 1 st, 2 nd, 3 rd Overtones and Combination Regions Light passes thru a clear liquid sample with no deflection of the light. Protein, alcohol, fat etc absorb light directly proportional to concentration.
9 Series 2000 Near Infrared Transmission Analysers Diode Array Spectrometers nm Multiple Sample Cells - Solids, Liquids, Powders and Suspensions Simple to use Suitable for laboratory and at line applications
10 Absorbance Absorbance Transflectance Spectra of Oil Seeds Canola Seeds Wavelength(Pixels) Soy Bean Spectra Pixel NIT Spectra of Canola 10mm Cell: 720 to 1100nm NIT Spectra of Soybean 28mm Cell: 720 to 1100nm
11 Absorbance Absorbance Transflectance Spectra of Foods 4 Milk Powder Blend Used for analysis of high fat and high water content samples Minced Beef Spectra Wavelength NIT Spectra of Milk Powder720 to 1100nm Pixels NIT Spectra of Minced Beef 720 to 1100nm
12 Analysis of Oil and Moisture in Olives Transflectance Spectra: 10mm Oil SEC = 0.6%, R2 =.95 Moisture SEC 0.9% R2 =.96
13 Transmission Spectra of Oils and Fats NIT Spectra of Tallow nm NIT Spectra of Bio-Diesel nm
14 Analysis of Total Glycerides in Bio-Deisel Transmission Spectra: PLS calibration SEC = 18ppm, R2 =.99
15 Analysis of Free Fatty Acids in Tallow Transflectance Spectra: 10mm Cell SEP = 0.15%, R2 =.99
16 Pharmaceutical Application Second Derivative spectra of dermatology ointment Absorbance spectra of dermatology ointment
17 Ointment Calibration 10 samples from 3 batches scanned 4times each = 40 spectra. Reference = HPLC method for Active component. PLS calibration using 2 nd Derivative spectral transformation.
18 Ointment Calibration Active A SEC = 0.7mg/ml R 2 = 0.82 Note the very narrow range = 99 to 104mg/ml
19 Ointment Prediction 6 different samples analysed using the PLS calibration model SEP = 0.4mg/ml R 2 = 0.99
20 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.
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