Practical Applications of Infrared Microspectroscopy for Industrial Problem Solving

1. Practical Applications of Infrared Microspectroscopy for Industrial Problem Solving Sample Preparation: Garbage In …You Know the Rest P.T. McKittrick, Ph.D. Nalco Company

2. Instruments Provide Data, Not Answers! 90 88 86 799.1 84 627.2 535.6 82 1260.0 1452.0 1377.1 80 %T 1523.8 78 76 2928.8 74 1652.2 72 3329.2 70 1034.6 68 4000 3500 3000 2500 2000 1500 1000 500 Wavenumbers (cm-1)

4. http://www.jwst.nasa.gov/images/em_spectrum_satellite.jpg http://upload.wikimedia.org/wikipedia/en/6/6f/IR_summary_version_2.gif

5. A. OH stretch B. Aromatic CH stretch C. Methylene CH Stretch D. Overtones E. CC ring stretch F. OH bend G. CO stretch H. OOP CH bend

6. Infrared Micro-what? • Two names in use in the literature • Infrared Microscopy • Infrared Microspectroscopy • Same thing • Microscope with optics for the infrared coupled to an FTIR for obtaining spectra

7. The Three Functions of a Microscope • Focus the radiation onto the sample • Collect the transmitted or reflected energy and image the energy onto a detector • Provide the user a means of observing the sample

8. FTIR coupled to a Light Microscope The first union of an FT-IR with a microscope. Image courtesy of G. Shearer, The McCrone Group

10. Four Things to Keep in Mind • Morphology is important. The sample is part of the optical system. • In general, the path length should be less than 10 microns.

12. Four Things to Keep in Mind • Morphology is important. The sample is part of the optical system. • In general, the path length should be less than 10 microns. • Generally, transmission is preferable to reflection.

13. Sometimes You Get Lucky

14. Sometimes You Don’t…

15. Reflectance with Kramers-Kronig Transform

16. Plastic Spacer in Transmission

17. Fiberglass Fibers

18. Adhesive Between Fibers

19. Micro Extractions

20. 60 Washer Black Residue Micro 40 %T 20 0 Washer Control CH2Cl2 Micro 100 99 %R 98 97 Washer Black Residue Micro CH2Cl2 90 %R 80 Washer Black Residue Micro CH2Cl2 60 50 %R 40 4000 3000 2000 1000 Wavenumbers (cm-1)

21. Spectra of Extractions from Pipe

22. Contamination in Finished Paper

23. Where Did The Fibers Come From? 90 Armor All Wipes 80 %T 70 60 Finished Paper Micro 80 60 %T 40 20 Finished Paper Fuorescent Fibers 80 60 %T 40 20 3500 3000 2500 2000 1500 1000 Wavenumbers (cm-1)

24. http://www.astrochem.org/compare.html

25. Pyrolysis

26. Four Things to Keep in Mind • Morphology is important. The sample is part of the optical system. • In general, the path length should be less than 10 microns. • Generally, transmission is preferable to reflection. • Everything is inhomogeneous

27. Patricia L. Lang, J.E. Katon and Anthony S. Bonano, Applied Spectroscopy, Vol. 42, # 2, 313-317, 1988

31. Diamond Anvil Cell

32. Particle in TPU

33. ATR Objective

36. White Inclusion in Paper

37. ATR Spectrum of Inclusion

38. Blisters in an In-Mold Label

41. EVA Spectrum

42. EVA calibration plot

43. The Latest Developments • First mapping, now imaging • Mapping – moving the sample relative to the detector • Imaging – Linear and focal plane array detectors • Chemometrics • Analysis of large numbers of spectra using data reduction techniques • Better use of optical microscopy • Simpler ways of doing micro-samples • Combined IR and Raman Instruments

44. Thanks to… • Kate Martin and The ACCA – for inviting me to speak • Nalco – for allowing me to speak • Kirk Ashline – for allowing me to speak with him • All of you – for listening