1. PRELIMINARY EVALUATIONS of MICRONAIRE MEASUREMENTS by NEAR INFRARED (NIR) SPECTROSCOPY for FIELD APPLICATIONS James Rodgers 1, Sho Yeung Kang, 2 Gayle Davidonis 1, Vikki Martin 3, Michael Watson 3 1 SRRC-ARS-USDA, New Orleans, LA; 2 UNIVERSITY of GEORGIA, Athens, GA; 3 COTTON INCORPORATED, Raleigh, NC 2008 BELTWIDE COTTON CONFERENCE NASHVILLE, TN JANUARY 10, 2008

2. ACKNOWLEDGEMENTS SRRC: Raisa Moiseyev, Students (CSQ)SRRC: Raisa Moiseyev, Students (CSQ) LSU AG CENTER: Ernest Clawson, Gerald MyersLSU AG CENTER: Ernest Clawson, Gerald Myers ARS, Stoneville: Bill PettigrewARS, Stoneville: Bill Pettigrew COTTON INCORPORATED personnelCOTTON INCORPORATED personnel BRIMROSE: Lynda TankersleyBRIMROSE: Lynda Tankersley

3. PROGRAM SPECIFICS OBJECTIVES 1. TO DETERMINE THE CAPABILITIES OF BENCH-TOP AND PORTABLE NIR INSTRUMENTATION TO MONITOR CRITICAL COTTON FIBER PROPERTIES (MICRONAIRE, MATURITY RATIO, FINENESS, etc.). 2. TO DETERMINE THE ABILITY OF PORTABLE INSTRUMENTATION TO MONITOR CRITICAL COTTON FIBER PROPERTIES OF BREEDER SAMPLES BOTH AT-LINE AND IN THE FIELD. 3 COMPONENTS 3 COMPONENTS Comparative Program, Portable & Bench-Top NIR AnalyzersComparative Program, Portable & Bench-Top NIR Analyzers Laboratory TrialsLaboratory Trials Initial Field/At-Line TrailsInitial Field/At-Line Trails

4. SAMPLES COMPARATIVE EVALUATIONS: Selected ginned cotton samples with wide property ranges for Micronaire, Maturity Ratio (MR), and Fineness. The same sets of samples were measured on each NIR analyzer.COMPARATIVE EVALUATIONS: Selected ginned cotton samples with wide property ranges for Micronaire, Maturity Ratio (MR), and Fineness. The same sets of samples were measured on each NIR analyzer. PORTABLE UNIT, LABORATORY EVALUATIONS: Selected ginned cotton samples (191 cottons) with wide range of Micronaire values. PORTABLE UNIT, FIELD EVALUATIONS: Selected seed cottons from several varieties, with the measurement performed directly on the cotton boll.PORTABLE UNIT, FIELD EVALUATIONS: Selected seed cottons from several varieties, with the measurement performed directly on the cotton boll.

5. NIR ANALYSES PRIMARILY 1100-2500nm SPECTRAL REGIONPRIMARILY 1100-2500nm SPECTRAL REGION (BETWEEN VISIBLE & IR) PRIMARILY COMBINATION & OVERTONE BANDSPRIMARILY COMBINATION & OVERTONE BANDS PRIMARILY CH n, NH n, & OH GROUPS, WITH STRONGPRIMARILY CH n, NH n, & OH GROUPS, WITH STRONG ABSORBENCIES FOR C=O & AMIDE GROUPS MEASURES ABSORBANCE (ABS) vs. WAVELENGTH (nm) CALIBRATED TO A REFERENCE/STANDARD METHOD

6. NIR ANALYSES ADVANTAGES FASTFAST ACCURATEACCURATE PRECISEPRECISE EASY TO MAINTAINEASY TO MAINTAIN EASY TO OPERATEEASY TO OPERATE NON-DESTRUCTIVENON-DESTRUCTIVE RUGGEDRUGGED MULTIPLE, SIMULTANEOUS ANALYSESMULTIPLE, SIMULTANEOUS ANALYSES QUALITATIVE & QUANTITATIVE ANALYSESQUALITATIVE & QUANTITATIVE ANALYSES DISADVANTAGES REQUIRES LARGE NUMBER OF SAMPLESREQUIRES LARGE NUMBER OF SAMPLES CHEMOMETRIC CALIBRATIONSCHEMOMETRIC CALIBRATIONS MODERATE COSTMODERATE COST

7. COMPARATIVE PROGRAM

8. MIC COMPARATIVE ANALYSES

9. SUMMARY OF RESULTS 1. GOOD SPECTRAL AGREEMENT WAS OBSERVED BETWEEN THE BENCH- TOP AND PORTABLE NIR ANALYZERS FOR THE COTTON FIBERS IN THIS PRELIMINARY STUDY. 2. FOR WELL-DEFINED SAMPLES, THE RAPID MEASUREMENT OF KEY FIBER MATURITY AND FINENESS PROPERTIES BY MULTIPLE BENCH-TOP AND PORTABLE NIR ANALYZERS WAS SHOWN TO BE FEASIBLE. 3. NO SAMPLE PREPARATION REQUIRED (measure directly on the fiber). 4. ANALYSIS TIME OF <5 MINUTES PER SAMPLE. 5. THE “UNIVERSAL” NATURE OF NIR MEASUREMENTS OF MICRONAIRE AND ITS COMPONENTS WAS VERIFIED.

10. PORTABLE NIR ANALYZER, LABORATORY ANALYSES

11. PORTABLE ANALYSES PROGRAM END-STATE CRITERIA: INTER-INSTRUMENT/METHOD AGREEMENT OF ± 0.30INTER-INSTRUMENT/METHOD AGREEMENT OF ± 0.30 MIC FOR ≥ 70% OF THE SAMPLES ANALYZED.  HVI Micronaire – NIR Micronaire FAST  < 5 MINUTES ANALYSIS PER SAMPLE EASY TO USE AND MAINTAINEASY TO USE AND MAINTAIN

12. BRIMROSE 5030 PORTABLE NIR ANALYZER Measuring Head Base Unit/Electronics

13. INSTRUMENTAL CONDITIONS VARIABLECONDITION 1CONDITION 2CONDITION 3CONDITION 4 MEASURING HEAD WithOut/No GLASS (NG) With GLASS (G) With GLASS (G) NO. SCANS300400300400 INSTRUMENT GAINX 1X 2X 1X 2

14. INSTRUMENTAL CONDITIONS WATER BAND

15. INSTRUMENTAL CONDITIONS ITEMCALIBRATION, MICRONAIRE (MIC), 191 SAMPLES HVINIR 300/NG 1 300/G 2 400/NG 3 400/G 4 AVG4.22 R2R2 NA0.870.88 0.91 SECNA0.210.20 0.17 CVSEPNA0.22 0.210.19 No. >± 0.3 (%)NA15.719.814.710.8 NOTES: 1. Brimrose 5030 NIR, No Glass, 300 Scans, Gain = 1 2. Brimrose 5030 NIR, Glass, 300 Scans, Gain = 1 3. Brimrose 5030 NIR, No Glass, 400 Scans, Gain = 2 4. Brimrose 5030 NIR, Glass, 400 Scans, Gain = 2

16. INSTRUMENTAL CONDITIONS

17. ITEM PREDICTION, MICRONAIRE (MIC), 50 SAMPLES HVINIR 300/NG 1 300/G 2 400/NG 3 400/G 4 AVG4.204.214.174.22 R2R2 NA0.810.790.740.87 SDDNA0.260.270.300.22 No. >± 0.3 (%)NA18.024.020.010.0 NOTES: 1. Brimrose 5030 NIR, No Glass, 300 Scans, Gain = 1 2. Brimrose 5030 NIR, Glass, 300 Scans, Gain = 1 3. Brimrose 5030 NIR, No Glass, 400 Scans, Gain = 2 4. Brimrose 5030 NIR, Glass, 400 Scans, Gain = 2

18. INSTRUMENTAL CONDITIONS

19. PORTABLE NIR ANALYZER, FIELD ANALYSES

20. NIR FIELD ANALYSES 2006: LSU EXTENSION CENTER, ST. JOSEPH, LA (4) 2007: LSU EXTENSION CENTER, ST. JOSEPH, LA (3) LSU EXTENSION CENTER, WINNSBORO, LA (3) ARS, STONEVILLE, MS (6)

21. NIR FIELD ANALYSES Plant Measurements

22. NIR FIELD ANALYSES Vehicle Measurements

23. NIR FIELD ANALYSES

24. PORTABLE NIR ANALYSES, RESULTS 1. COMPARATIVE STUDIES ON OPTIMUM INSTRUMENTAL CONDITIONS/SETTINGS WERE COMPLETED AND IMPLEMENTED. **400 Scans/Gain=2 results were overall superior to those of 300 Scans/Gain =1. **400 Scans/Gain=2 results were overall superior to those of 300 Scans/Gain =1. **For lab measurements, the 400 Scans/Gain = 2/Glass condition was shown **For lab measurements, the 400 Scans/Gain = 2/Glass condition was shown to be the best overall portable NIR method for fiber micronaire. 2. VERY GOOD & ENCOURAGING LABORATORY RESULTS WERE OBTAINED WITH THE PORTABLE NIR UNITS FOR MICRONAIRE. **Method Agreement of ± 0.30 MIC was achieved for >85% of the samples. **Method Agreement of ± 0.30 MIC was achieved for >85% of the samples. **Fast analysis (< 5 minutes per sample). **Fast analysis (< 5 minutes per sample). **Easy to use technique. **Easy to use technique. 3. EXPANDED FIELD TRIALS FOR MICRONAIRE ON COTTON BOLLS WERE PERFORMED. **4 fields/14 varieties (LA and MS) **4 fields/14 varieties (LA and MS) **Macro developed and installed for remote field operation (battery power). **Macro developed and installed for remote field operation (battery power). **Field sampling systems developed—Plant Analyses and Vehicle Analyses. **Field sampling systems developed—Plant Analyses and Vehicle Analyses. **Distinct micronaire differences observed (tactile, different cotton varieties). **Distinct micronaire differences observed (tactile, different cotton varieties).

25. PORTABLE NIR ANALYSES, NEXT STEPS COMPLETE ANALYSES OF FIELD SAMPLESCOMPLETE ANALYSES OF FIELD SAMPLES  Field/Seed Cotton → Lab/Seed Cotton → Lab/Lint → HVI → NIR/HVI Lint  Bench-Top and Portable NIR NEW FIELD ANALYSES FOR 2008NEW FIELD ANALYSES FOR 2008 ADVANCED CHEMOMETRIC STATISTICAL MODELINGADVANCED CHEMOMETRIC STATISTICAL MODELING EVALUATION OF NEW PORTABLE ANALYZERSEVALUATION OF NEW PORTABLE ANALYZERS  Polychromix PHAZIR EXPAND PROGRAM TO OTHER PROPERTIESEXPAND PROGRAM TO OTHER PROPERTIES  Maturity/Maturity Ratio (MR)  Moisture