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BRUINS INSTRUMENTS

BRUINS INSTRUMENTS. Training Near Infrared Transmission Whole Grain Analyzer. Targets:. History and Basics of NIR Calibration development Toubleshooting & Maintainance. History of NIR. First detected by William Herschel beginning of 19th century

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BRUINS INSTRUMENTS

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  1. BRUINS INSTRUMENTS Training Near Infrared Transmission Whole Grain Analyzer BRUINS INSTRUMENTS

  2. Targets: • History and Basics of NIR • Calibration development • Toubleshooting & Maintainance BRUINS INSTRUMENTS

  3. History of NIR • First detected by William Herschel beginning of 19th century • First instrument built by W.W. Coblentz about 1900 • First practical use in the 1930s • First agriculture usage by Karl Norris 1968 • First commercial scanning instruments 1978 • First BRUINS NIR spectrophotometer 1979 • First BRUINS NIT spectrophotometer 1982 BRUINS INSTRUMENTS

  4. Basics of NIR NIR = Near InfraRed Spectroscopy Wavelength of Light UV > VIS > NIR >(M)IR nm 380 750 / 1100 2500 (NIT / NIR) Energy of Light BRUINS INSTRUMENTS

  5. 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. BRUINS INSTRUMENTS

  6. Basics of NIR • NIR active groups O-H Water, Alcohol C-H Carbohydrates (Starch, Sugar, Cellulose) Fat / Oil N-H Protein BRUINS INSTRUMENTS

  7. Basics of NIR Molekular Vibrations O H H BRUINS INSTRUMENTS

  8. Basics of NIR Molekular Vibrations BRUINS INSTRUMENTS

  9. Basics of NIR Molekular Vibrations BRUINS INSTRUMENTS

  10. Calibration • Reference Analysis • Sample selection • Sampling • Sample Preparation / Homogenisation • Sample Presentation BRUINS INSTRUMENTS

  11. Calibration: Reference Analysis • NIR calibration will be dependend from reference analysis, so • Select best possible method • Investigate „real“ method error • Make sure that the same sample material will be analysed • Use at least double analysis • Comment all specialities of actual sample BRUINS INSTRUMENTS

  12. Calibration: Lab Error Influence BRUINS INSTRUMENTS

  13. Calibration: Lab Error Influence BRUINS INSTRUMENTS

  14. Calibration: Sample Selection • The complete interesting concentration range must be covered by calibration samples. • The calibration set must also include samples with changes from other constituents, eg. low protein with high moisture, low protein with low moisture etc. • Further samples must be included which are representing influences from climate, soil, cultivars etc. • Due to the effect of temperature to NIR also cold and warm samples should be added. BRUINS INSTRUMENTS

  15. Calibration: Sampling • The sample must be representative for the total amount. • Take subsamples from different locations. • Thoroughly mix these to get a homogene sample. BRUINS INSTRUMENTS

  16. Calibration: Sample Preparation • No extra preparation needed for most grain and oil seeds. • Samples with thick shell must be ground (e.g. sunflower seeds). • The same 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. BRUINS INSTRUMENTS

  17. Calibration: Sample Presentation • OmegAnalyzer and AgriCheck uses the NIR transmission, so for such meal the MultiCheck will be the better choice • As an alternative, but less efficient, a micro sample cup for meal or powders can be used BRUINS INSTRUMENTS

  18. Calibration: Sample Presentation In all cases, if fine powder or ground sample: • Thoroughly mix the sample before filling • In cases of components with different density make sure, that no material separate If a micro sample cup is used: • Make sure that the sample is filled without wholes • Knock a bit, that the sample will slide together, but not to often because different components may separate BRUINS INSTRUMENTS

  19. 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. BRUINS INSTRUMENTS

  20. 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 how good the predicted values fit to the reference analysis. BRUINS INSTRUMENTS

  21. Calibration: Bias BRUINS INSTRUMENTS

  22. Calibration: Bias BRUINS INSTRUMENTS

  23. Calibration: Bias BRUINS INSTRUMENTS

  24. Calibration: Bias, 0.43 added BRUINS INSTRUMENTS

  25. Calibration: Bias BRUINS INSTRUMENTS

  26. 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. BRUINS INSTRUMENTS

  27. Calibration: Slope BRUINS INSTRUMENTS

  28. Calibration: Slope BRUINS INSTRUMENTS

  29. Calibration: corrected Slope BRUINS INSTRUMENTS

  30. Calibration: corrected Slope BRUINS INSTRUMENTS

  31. Calibration: Slope BRUINS INSTRUMENTS

  32. Calibration: Slope BRUINS INSTRUMENTS

  33. Calibration: Slope BRUINS INSTRUMENTS

  34. Calibration: corrected Slope? BRUINS INSTRUMENTS

  35. Calibration: corrected Slope? BRUINS INSTRUMENTS

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