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IDRC Practical Experiences with a Variety of Instrumentation for Diffuse Reflectance Measurments
- 1. Practical Experiences with a Variety of Instrumentation for Diffuse Reflectance Measurements Arnold Eilert Unity Scientific
- 2. Overview • “Real World” Deviations from the “Ideal” • Diffuse Reflectance (I/Io) Measurement Approaches – Sample & Reference • Sample Measurement Considerations, Challenges, Obstacles, and Strategies • Various Examples to Illustrate Diffuse Reflectance NIR Measurements
- 3. Diffuse Reflectance NIR Specular Diffuse Reflectance Modes
- 4. Diffuse Reflectance Theory Ideal versus Reality Diffuse Reflectance NIR
- 5. Impinging Radiation Detectors Sample Sample Incident Radiation Return Radiation Sample Integrating Sphere Close Proximity Detectors Fiber Optic Bundle Diffusely Reflected Radiation Collection Schemes Remote Non-Contact Diffuse Reflectance NIR
- 6. Diffuse Reflectance NIR “Absorbance” = -Log(R); R = I/Io Various Referencing Schemes for Io
- 7. Particle Size Effects Density Effects Practical Diffuse Refl. NIR
- 8. Distance Effects Residual Sample (Contaminant) Effects “Practical” Diffuse Refl. NIR
- 9. • Flour – Compression/Compaction • Tissue Paper - Compression • Tissue Paper – “Infinite Thickness” Diffuse Reflectance NIR Experiments (“Academic” Tests using Model 2600XT) “Practical” Diffuse Refl. NIR
- 10. Variable Compaction Pressure Study InfraAlyzer 400 & InfraAlyzer 500 w/ Edapt Probe
- 11. “Practical” Diffuse Refl. NIR • Wheat flour placed in rotating cup on SpectraStar XT unit • Uniform weights incrementally added to top of plunger
- 12. “Practical” Diffuse Refl. NIR Flour Compaction Pressure Measurement Levels 0.034 PSI 0.689 PSI
- 13. Wheat Flour; Variable Compaction Pressure Absorbance Spectra; 680-2600 nm
- 14. ͛ Wheat Flour; Variable Compaction Pressure Absorbance + SNV + 1st Derivative Spectra; 680-2600 nm
- 15. 균ж Variable Compaction – Wheat Flour Protein
- 16. Variable Compaction – Wheat Flour Moisture
- 17. Variable Compaction – Wheat Flour Ash
- 18. A. Tissue Paper Compression “Academic” Diffuse Refl. NIR • 15 Layers of Paper Placed on Window • Increasing Pressure Applied B. “Infinite Thickness” Demonstration • Consistent Pressure Applied • Layers Peeled Off One-by-One • Influence of Backing Evaluated
- 19. 1 2 3 4
- 20. Tissue Paper (15 Thick) & Styrofoam Plate Backing Absorbance Spectra Styrofoam Plate (Backing) Tissue Paper (15 Thick) 15 Layers Thick (Moderate Compression) = Approx. 0.25 inch Thick
- 21. ͔丠 Increasing Compaction Pressure (PSI) 0.05 0.10 0.16 0.21 0.26 0.31 0.37 0.42 0.47 0.52 0.58 Total Paper Thickness ~ 0.25 inch Tissue Paper (15 Layers Thick) Absorbance Spectra; 680-2600 nm Increasing Weight (Lbs)
- 22. ͔丠 Tissue Paper (15 Layers Thick) Absorbance Spectra; 680-1900 nm 680-1100 nm
- 23. Tissue Paper (15 Layers Thick) Absorbance + 1st Derivative Spectra; 680-1900 nm
- 24. 斐С Tissue Paper (15 Layers Thick) Absorbance + SNV + 1st Derivative Spectra; 680-1900 nm
- 25. 窠С Tissue Paper (15 Layers Thick) Predicted “Pulp Viscosity” versus Compression Pressure
- 26. “Academic” Diffuse Refl. NIR “Infinite Thickness” Demonstration ~ 0.6 PSI 15 Layers (0.25”) 1 Layer
- 27. Tissue Paper (Varying # of Layers) Absorbance Spectra Polystyrene “Contaminant”
- 28. 析С Tissue Paper (Varying # of Layers) Absorbance Spectra
- 29. 窠С Tissue Paper (Varying # of Layers) Absorbance Spectra; 1600-1900 nm
- 30. 析С Tissue Paper (Varying # of Layers, 1 - 15) Absorbance Spectra; 680-1750 nm
- 31. 窠С Tissue Paper (Varying # of Layers, 1 - 15) Absorbance Spectra; 680-1400 nm
- 32. 析С Tissue Paper (Varying # of Layers, 1 - 15) Absorbance + SNV + 1st Derivative Spectra
- 33. 窠С Tissue Paper (Varying # of Layers, 1 - 15) Absorbance + SNV + 1st Derivative Spectra
- 34. 挠Т Tissue Paper (Varying # of Layers, 1 - 15) Absorbance + SNV + 1st Derivative Spectra; 680-1400 nm
- 35. ︀Х To Grind, or Not to Grind??? Practical Diffuse Refl. NIR
- 36. Particle Size / Compaction • To homogenize composition of a larger sample (i.e. representative subsampling) • To get best results with for some properties with complex/layered products (seeds, coated products, . . .) • To minimize variable particle size effects • To minimize “macro” particle size effects • Simply to make the sample presentable to the instrument Why Choose the Grinding Option?
- 37. Rotating Transport Linear Transport Diffuse Reflectance NIR Particle Heterogeneity/Orientation Effects
- 38. Unground “Crystal” Ground “Crystal” Unground “High Impact” Polystyrene Pellets – Ground & Unground
- 39. “Crystal” Pellets “High Impact” Pellets Gnd “Crystal” Pellets Clear Layer / Transfl. Polystyrene Pellets – Comparisons Absorbance Spectra
- 40. ︀Х .4 .6 .8 1 1.2 1.4 1.6 1000 1200 1400 1600 1800 2000 2200 High Impact Polystyrene, “Full Range” Spectra SpectraStar 2200 RTW 512 Element InGaAs Diode Array Analyzer
- 41. 湰Ь Diode Array Unit (512 Element): Ethylene Copolymer Pellets; 920-1700 nm Absorbance Spectra All Samples Varying % Vinyl Acetate
- 42. Т Absorbance Spectra Select Samples Varying % Vinyl Acetate Diode Array Unit (512 Element): Ethylene Copolymer Pellets; 920-1700 nm
- 43. ︀Х 1.6% 3.8% 8.8% 9.5% 15.2% 18.3% 27.4% 32.2% Absorbance + 2nd Derivative Spectra Select Samples Varying % Vinyl Acetate Diode Array Unit (512 Element): Ethylene Copolymer Pellets; 1300-1360 nm
- 44. ︀Х 1.6% 3.8% 8.8% 9.5% 15.2% 18.3% 27.4% 32.2% Absorbance + 2nd Derivative Spectra Select Samples Varying % Vinyl Acetate Diode Array Unit (512 Element): Ethylene Copolymer Pellets; 1580-1650 nm
- 45. ︀Х Absorbance Spectra 2 Wavelength MLR Calibration: # Samples = 10 + 1 Val Sample R-Squared = 0.99940 S.E.C. = 0.306 Absorbance + 1st Derivative Spectra 2 Wavelength MLR Calibration: # Samples = 10 + 1 Val Sample R-Squared = 0.99993 S.E.C. = 0.103 512 Element Diode Array Unit: Ethylene Copolymer Pellets Absorbance Spectra All Samples Varying % Vinyl Acetate
- 46. Т Smokeless Gunpowder Graphite Coated Uncoated
- 48. 湰Ь Soy White Flakes Ground Unground
- 49. White Flake - Unground Absorbance Spectra Measured on SpectraStar 2600 XT 12 Individual Cup Orientations
- 50. White Flake - Unground Absorbance Spectra Measured on SpectraStar 2500 XL-R 12 Individual Cup Orientations
- 51. White Flake - Unground Absorbance + SNV + 1st Derivative Spectra Measured on SpectraStar 2600 XT 12 Individual Cup Orientations
- 52. 湰Ь White Flake - Unground Absorbance + SNV + 1st Derivative Spectra Measured on SpectraStar 2500 XL-R 12 Individual Cup Orientations
- 53. 湰Ь White Flake - Unground Absorbance Spectra Measured on SpectraStar 2500 XL-R 12 Repeated Measurements - Step Rotation
- 54. 湰Ь Soy White Flake - Unground Absorbance + SNV + 1st Derivative Spectra Measured on SpectraStar 2500 XL-R 12 Repeated Measurements - Step Rotation
- 55. 析С White Flake - Unground Absorbance Spectra Measured on SpectraStar 2500 XL-R 12 Repeated Measurements - Continuous Rotation 90 deg/s
- 56. 析С White Flake - Unground Absorbance + SNV + 1st Derivative Spectra Measured on SpectraStar 2500 XL-R 12 Repeated Measurements - Continuous Rotation 90 deg/s
- 57. 湰Ь Grind & Rotation Comparison 1. Measurements at 12 Different Orientations 2. Step Rotation; 12 Measurements 3. Continuous Rotation 90 deg/s; 12 Measurements 4. Continuous Rotation 30 deg/s; 12 Measurements A. Unground White Flake 1. Measurements at 12 Different Orientations 2. Step Rotation; 12 Measurements 3. Continuous Rotation 90 deg/s; 12 Measurements 4. Continuous Rotation 30 deg/s; 12 Measurements B. Ground White Flake
- 58. Unground White Flake Sample Absorbance Standard Deviation
- 59. Ground White Flake Sample Absorbance Standard Deviation
- 60. Ground White Flake Sample Absorbance Standard Deviation (Expanded Y-Axis)
- 61. Unground White Flake Sample Practical Implications using Spectra to Predict Percent Oil
- 62. Grinding – The Only Way to Go???
- 63. White, Yellow, Pink (w/ TiO2) Red, Green, Blue, Violet (w/o TiO2) Black (w/ Carbon Black) Polypropylene Plastic Container Parts; Various Colors Ground Product Spectra; I/A 500 w/ Rotating Cup Drawer
- 64. 뫀л Polypropylene Plastic Container Parts; Various Colors Ground Product Spectra; I/A 500 w/ Rotating Cup Drawer 3 Wavelength MLR Calibration for % Slip Red, Green, & Blue Parts Corr. Coef. = 0.993 S.E.C. = 0.080
- 65. @ې 3 Wavelength MLR Calibration for % Slip Skew & Bias Adjusted for White Parts S.E.P. = 0.144 Polypropylene Plastic Container Parts; Various Colors Ground Product Spectra; I/A 500 w/ Rotating Cup Drawer
- 66. 뫀л 3 Wavelength MLR Calibration for % Slip Skew & Bias Adjusted for White Parts S.E.P. = 0.144 Polypropylene Plastic Container Parts; Various Colors Ground Product Spectra; I/A 500 w/ Rotating Cup Drawer Excluded
- 67. ܠ@ Particle Size / Compaction • Calibrations estimating particle size • Wheat hardness estimation (using MLR equation) • Avoid heating / moisture loss caused by grinding • Avoid grinding step – practical trade-off Q: When might you NOT want to minimize variance due to particle size variation (using preprocessing, grinding, . . .)???
- 68. Diffuse Reflectance NIR Diffuse Transflectance Mode
- 69. Q: Which sampling mode is most appropriate for the application? A: Determined by the optical and physical characteristics of the product being analyzed: • Powders / Granulates - Reflectance • Formed Solids - Reflectance / Transmission • Liquids / Films / Gels Clear - Transmission / Transflectance Semi-Opaque - Transflectance Opaque - Reflectance / Transflectance Diffuse Reflectance NIR
- 70. 1 2 3 4 Liquid Cup + Transflectance Insert
- 71. Egg Yoke – SpectraStar 2400 RTW 0.1 mm Insert 0.2 mm Insert 0.3 mm Insert 0.4 mm Insert Transflectance Mode; Absorbance Spectra
- 72. 뫀л0.1 mm Insert 0.2 mm Insert 0.3 mm Insert Egg Yoke – SpectraStar 2400 RTW Transflectance Mode; Absorbance Spectra
- 73. 뫀л 0.1 mm Insert 0.2 mm Insert 0.3 mm Insert 0.4 mm Insert Egg Yoke – SpectraStar 2400 RTW Absorbance + 1st Derivative Spectra
- 74. 뫀л Egg Yoke – SpectraStar 2400 RTW Absorbance + SNV + 1st Derivative Spectra
- 75. 뫀л 1 2 3 “Special Purpose” Compression Transflectance Cup
- 76. Caramel Sample Placed in SpectraStar Drawer
- 77. Final Tightening Step – Change with Position 1 2 3 4 5
- 78. 1 2 3 4 5 Absorbance Spectra Final Tightening Step – Change with Position
- 79. Final Tightening – Change with Position Absorbance + SNV + 1st Derivative Spectra
- 80. Different Caramel Products Absorbance Spectra
- 81. Absorbance + SNV + 1st Derivative Spectra Different Caramel Products
- 82. Intact Measurement – The Only Way to Go???
- 83. Filled Sample Cup Placed for Measurement
- 84. Smear of an Individual Capsule Liquid on Transflectance-Mode Reflector Surface
- 85. Transflectance Reflector placed in Liquid Cup Against Glass for Measurement (0.3 mm Path Length)
- 86. Bulk Capsules in Rotating Open Cup Reflectance Mode Exctracted Liquid from Single Capsule Transflectance Mode Nutraceutical Capsules – SpectraStar 2500X RTW Reflectance versus Transflectance Mode; Absorbance Spectra
- 87. 뫀л Nutraceutical Capsules – SpectraStar 2500X RTW Reflectance versus Transflectance Mode; Absorbance Spectra Bulk Capsules in Rotating Open Cup Reflectance Mode Exctracted Liquid from Single Capsule Transflectance Mode
- 88. 뫀л Individual Pack (Black) vs Average of 4 Packs (Red) Nutraceutical Capsules – SpectraStar 2500X RTW Bulk Capsules in Rotating Open Cup; Absorbance Spectra
- 89. 뫀л Nutraceutical Capsules – SpectraStar 2500X RTW Bulk Capsules in Rotating Open Cup; Absorbance + SNV + 1st Deriv Spectra Individual Pack (Black) vs Average of 4 Packs (Red) 800-2200 nm Range
- 90. 뫀л Regions of Highest Degree of Undesirable Variance “Blotted Out” Nutraceutical Capsules – SpectraStar 2500X RTW Bulk Capsules in Rotating Open Cup; Absorbance + SNV + 1st Deriv Spectra Individual Pack (Black) vs Average of 4 Packs (Red) 800-2200 nm Range
- 91. 뫀л Confirmed misidentified (bad) sample in test set A-Type Capsules Quantitative Feasibility Evaluation
- 92. 뫀л A E A E A E A E Bad Bad Regions of Highest Degree of Undesirable Variance “Blotted Out” Nutraceutical Capsules – SpectraStar 2500X RTW Bulk Capsules in Rotating Open Cup; Absorbance + SNV + 1st Deriv Spectra Discriminant Analysis Potential Evaluation
- 93. Nutraceutical Capsules – SpectraStar 2500X RTW Bulk Capsules in Rotating Open Cup; Absorbance + SNV + 1st Derivative Cluster Model Discriminant Analysis
- 94. 嵐У Corn Syrup Types: DE28 DE63 DE99 42FCS 55FCS HMCS Corn Syrup Grades – SpectraStar 2400D Transflectance Mode; 0.3 mm PL; Absorbance Spectra
- 95. я Corn Syrup Grades – SpectraStar 2400D Transflectance Mode; 0.3 mm PL; Absorbance + SNV + 1st Deriv Spectra All Calibration Spectra Corn Syrup Types: DE28 DE63 DE99 42FCS 55FCS HMCS
- 96. Average Spectra for Each Type Corn Syrup Grades – SpectraStar 2400D Transflectance Mode; 0.3 mm PL; Absorbance + SNV + 1st Deriv Spectra Corn Syrup Types: DE28 DE63 DE99 42FCS 55FCS HMCS
- 97. 뫀л Average Spectra for Each Type 1450-1820 nm Corn Syrup Grades – SpectraStar 2400D Transflectance Mode; 0.3 mm PL; Absorbance + SNV + 1st Deriv Spectra
- 98. 뫀л Corn Syrup Grades – SpectraStar 2400D Transflectance Mode; 0.3 mm PL; Absorbance + SNV + 1st Deriv Spectra Average Spectra for Each Type 2050-2350 nm
- 99. 뫀лDE99 42FCS DE28 HMCS 55FCS (HFCS) DE63 Cluster Model for Corn Syrup Qualification; Scores Plot of Factor 3 vs Factor 2 (Circles represent Factor Space Occupied by Corresponding Type) Cluster Model Discriminant Analysis
- 100. 뫀л 10o C - 86o C Range T Temperature can influence band shape and peak position
- 101. 뫀л T
- 102. 뫀л Diffuse Reflectance NIR • Sample presentation consistency (minimize controllable variables) • Optimize optics, general performance of instrument, sampling mode • Utilize the optimal spectral region • Optimize the calibration (# factors / wavelengths, mathematical pretreatment, proper exclusion of outliers . . .) Getting Optimal Results
- 103. • Keep an open mind . . . - but keep in mind the fundamentals • Diffuse reflectance NIR doesn’t do it all - but it does a lot! Summary Diffuse Reflectance NIR