BRUINS INSTRUMENTS Training Near Infrared Transmission Whole Grain
BRUINS INSTRUMENTS Training Near Infrared Transmission Whole Grain Analyzer 10 / 07 BRUINS INSTRUMENTS 1
Targets: l History and Basics of NIR l Calibration development l Toubleshooting & Maintainance 10 / 07 BRUINS INSTRUMENTS 2
History of NIR l l l l First detected by William Herschel beginning of 19 th century First instrument built by W. W. Coblentz about 1900 First practical use in the 1930 s First agriculture usage by Karl Norris 1968 First commercial scanning instruments 1978 First BRUINS NIR spectrophotometer 1979 First BRUINS NIT spectrophotometer 1982 10 / 07 BRUINS INSTRUMENTS 3
Basics of NIR = Near Infra. Red Spectroscopy Wavelength of Light UV > VIS nm 380 > NIR >(M)IR 750 / 1100 2500 (NIT / NIR) Energy of Light 10 / 07 BRUINS INSTRUMENTS 4
Basics of NIR Typical properties analysed by NIR are organic compounds like Oil Protein Starch And Water Useful concentration are in % range, ppm or ppb level are normally impossible. 10 / 07 BRUINS INSTRUMENTS 5
Basics of NIR l NIR active groups O-H Water, Alcohol C-H Carbohydrates (Starch, Sugar, Cellulose) Fat / Oil N-H 10 / 07 Protein BRUINS INSTRUMENTS 6
Basics of NIR Molekular Vibrations O H 10 / 07 H BRUINS INSTRUMENTS 7
Basics of NIR Molekular Vibrations 10 / 07 BRUINS INSTRUMENTS 8
Basics of NIR Molekular Vibrations 10 / 07 BRUINS INSTRUMENTS 9
Calibration l l l Reference Analysis Sample selection Sampling Sample Preparation / Homogenisation Sample Presentation 10 / 07 BRUINS INSTRUMENTS 10
Calibration: Reference Analysis l l l NIR calibration will be dependend from reference analysis, so Select best possible method Investigate „real“ method error Make sure that the sample material will be analysed Use at least double analysis Comment all specialities of actual sample 10 / 07 BRUINS INSTRUMENTS 11
Calibration: Lab Error Influence 10 / 07 BRUINS INSTRUMENTS 12
Calibration: Lab Error Influence 10 / 07 BRUINS INSTRUMENTS 13
Calibration: Sample Selection The complete interesting concentration range must be covered by calibration samples. l The calibration set must also include samples with changes from other constituents, eg. low protein with high moisture, low protein with low moisture etc. l Further samples must be included which are representing influences from climate, soil, cultivars etc. l Due to the effect of temperature to NIR also cold and warm samples should be added. l 10 / 07 BRUINS INSTRUMENTS 14
Calibration: Sampling The sample must be representative for the total amount. l Take subsamples from different locations. l Thoroughly mix these to get a homogene sample. l 10 / 07 BRUINS INSTRUMENTS 15
Calibration: Sample Preparation l l l No extra preparation needed for most grain and oil seeds. Samples with thick shell must be ground (e. g. sunflower seeds). The sample preparation must be used for calibration and routine analysis. By grinding a sample the moisture content will decrease. Select the best grinder to reduce this moisture loss. If a grinder with a sieve will be used, control the size of the mesh. 10 / 07 BRUINS INSTRUMENTS 16
Calibration: Sample Presentation Omeg. Analyzer and Agri. Check uses the NIR transmission, so for such meal the Multi. Check will be the better choice l As an alternative, but less efficient, a micro sample cup for meal or powders can be used l 10 / 07 BRUINS INSTRUMENTS 17
Calibration: Sample Presentation In all cases, if fine powder or ground sample: l Thoroughly mix the sample before filling l In cases of components with different density make sure, that no material separate If a micro sample cup is used: l Make sure that the sample is filled without wholes l Knock a bit, that the sample will slide together, but not to often because different components may separate 10 / 07 BRUINS INSTRUMENTS 18
Calibration: Standardisation Before using the instrument in routine, it must be compared against the reference method with a set of samples. These samples should cover the range of concentrations and normal variations in moisture, area and genotypes. In order to get a good adjustment, the sample must be well mixed that the same material will be analysed with both methods. The data for the reference analysis need to be well controlled, at least a double analysis must be performed. 10 / 07 BRUINS INSTRUMENTS 19
Calibration: Standardisation The easiest comparison of accuracy and necessary adjustment can be made with Excel. Just two columns need to filled , one with reference analysis the second with predicted NIR data. Using the Excel functions for mean, standard error xy and correlation will calculate all necessary information. Additional the Excel graph can be used to show good the predicted values fit to the reference analysis. 10 / 07 BRUINS INSTRUMENTS 20
Calibration: Bias 10 / 07 Actual Predicted 8 9 10 11 12 13 14 15 16 17 18 7. 5 8. 5 9. 7 10. 6 11. 7 12. 4 13. 7 14. 4 15. 5 16. 6 17. 7 BRUINS INSTRUMENTS 21
Calibration: Bias Actual Predicted 8 9 10 11 12 13 14 15 16 17 18 7. 5 8. 5 9. 7 10. 6 11. 7 12. 4 13. 7 14. 4 15. 5 16. 6 17. 7 10 / 07 Actual Mean 13. 00 SEP 0. 121 R² 0. 999 Bias - 0. 43 Slope 1. 001 BRUINS INSTRUMENTS Predicted 12. 57 22
Calibration: Bias 10 / 07 BRUINS INSTRUMENTS 23
Calibration: Bias, 0. 43 added 10 / 07 Actual Predicted 8 9 10 11 12 13 14 15 16 17 18 7. 93 8. 93 10. 13 11. 03 12. 13 12. 83 14. 13 14. 83 15. 93 17. 03 18. 08 BRUINS INSTRUMENTS 24
Calibration: Bias 10 / 07 BRUINS INSTRUMENTS 25
Calibration: Slope While the bias will move all data parallel, the slope will change the extreme values more than the values around the middle. So adjusting the slope will much more influence the predicted result. For the slope adjustment the sample set must really cover the full calibration range. Normally this adjustment should not be used. If it seems to be necessary, look for the reason. It might be better to select or built another calibration. 10 / 07 BRUINS INSTRUMENTS 26
Calibration: Slope 10 / 07 Actual Predicted 8 9 10 11 12 13 14 15 16 17 18 7. 5 8. 3 9. 8 10. 5 12. 1 12. 9 14. 5 15. 0 16. 6 17. 2 18. 5 BRUINS INSTRUMENTS 27
Calibration: Slope 10 / 07 BRUINS INSTRUMENTS 28
Calibration: corrected Slope 10 / 07 Actual Predicted 8 9 10 11 12 13 14 15 16 17 18 8. 14 8. 86 10. 21 10. 83 12. 27 12. 99 14. 43 14. 88 16. 31 16. 85 18. 02 BRUINS INSTRUMENTS 29
Calibration: corrected Slope 10 / 07 BRUINS INSTRUMENTS 30
Calibration: Slope 10 / 07 Actual Predicted 11 12 13 14 10. 5 12. 1 12. 9 14. 5 BRUINS INSTRUMENTS 31
Calibration: Slope 10 / 07 BRUINS INSTRUMENTS 32
Calibration: Slope 10 / 07 BRUINS INSTRUMENTS 33
Calibration: corrected Slope? 10 / 07 Actual Predicted 8 9 10 11 12 13 14 15 16 17 18 8. 59 9. 21 10. 39 10. 93 12. 18 12. 81 14. 06 14. 45 15. 70 16. 17 17. 18 BRUINS INSTRUMENTS 34
Calibration: corrected Slope? 10 / 07 BRUINS INSTRUMENTS 35
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