안동 대학교 UV/VIS/NIR SPECTROPHOTOMETER 2002년 3월 27일

1. 안동 대학교 UV/VIS/NIR SPECTROPHOTOMETER 2002년 3월 27일

2. OSI Technical Support • About me 심 보 성 Service and Technical Support Engineer bs.sim@varianinc.com Sim bo sung @hotmail.com

3. Agenda • UV/VIS/NIR 기 본 이 론 • SOURCE LAMPS • MONOCHROMATOR • SAMPLE COMPARTMENT • DETECTOR • Accessories

4. UV/VIS/NIR기 본 이 론

5. Units • For spectroscopy purposes, we choose to characterize light in the UV/Vis regions in terms of wavelength expressed in Nanometers Nanometers (nm) 1 nm= m 1.000.000.000

6. The Cary UV-Vis family • Cary 50 • Cary 100 • Cary 300 • Cary 400 • Cary 500 • Cary 500i • DEEP UV

7. Molecular Instrumentation Cary 500 The Cary 500 spectrophotometer is a Top-of-the-line UV-Vis-NIR instrument

8. FLOW CHART • Sourcea broad band of electromagnetic radiation • Monochromatorentrance slit, dispersion device, exit slit selection of a desired wavelength • Sample area • Detector(s)measure intensity of radiation • Readout

9. UV/VIS/NIR Spectrophotometer Monochromator Light source Sample Light detector  Abs  Concentration Spectrum

10. SOURCE LAMPS

11. VIS LAMP Used to measure non-atomic absorption Useful from 300-3500nm Fill gas is iodine Light emission through excited tungsten at every window

12. Anode Aperature Quartz Window Thermionic Cathode Deuterium Lamp • Used to measure non-atomic absorption • Useful from 190 - 425nm • Fill gas is Deuterium (D2) • Discharge current excites D2 gas • High light emission through discharge aperature

13. The power of Xenon • Single light source (Xenon Flash lamp) • Only flashes when you are taking a reading • Does not heat up the sample • Does not degrade photosensitive samples • Outstanding performance in the UV, visible and infrared range (190 - 3500nm.) • Low noise • Excellent Flash repeatability • Reliable starting

14. Source turret • Removable Lamp turret • Three positions Visible Deuterium Third source (Mercury), laser etc. • Source change (UV-Vis) 350nm 1.장점

15. UV/VIS/NIR Spectrophotometer Monochromator Light source Sample Light detector  Abs  Concentration Spectrum

16. Optical construction of a Monochromator Ebert Monochromator Entrance Slit Exit Slit Grating

17. Optical construction of a Monochromator Czerny-Turner Monochromator Entrance Slit Exit Slit Grating

18. Double “out of plane” Littrow Grating Side view Slits Mirror Slits Grating Top view Mirror

19. 실제적인 Optics LOW STRAY LIGHT N5 N9R N2 N6 N10 N8 N7 N12 N3 N4 N1 N9S N13 N11 N10

20. Sealed Nitrogen Purging Separate purging plumbing for mono. & sample compartment Sealed Nitrogen purging for entire optical path: • Improved performance in the low UV and NIR where atmospheric water absorbs

21. Relationship: Absorbance and Transmittance • Transmittance %T Absorbance 1 100 % 0 0.1 10 % 1 0.01 1 % 2 0.001 0.1% 3 0.0001 0.01% 4 0.00001 0.001% 5 0.000001 0.0001% 6 2.장점

22. UV/VIS/NIR Spectrophotometer Monochromator Light source Sample Light detector  Abs  Concentration Spectrum

23. Sample CompartmentSingle Beam Instruments Monochromator Detector Sample

24. Sample CompartmentDual Beam Instruments Reference Detector Beam-Splitter Monochromator Sample Detector Sample

25. Beam-Splitter Reference Monochromator Sample Sample CompartmentDouble Beam Instruments Detector

26. 실제적인 Optics N5 N9R N2 N6 N10 N8 N7 N12 N3 N4 N1 N9S N13 N11 N10

27. Non-Measurement Phase Stepping (NMPS) Conventional scanning Dark Reference Sample Grating moves Grating continues Sample measured at to move different wavelength NMPS to reference Dark Reference Sample NMPS results in very accurate measurements! Chopper moves Grating stops Sample measured at only during same Wavelength as NMFS of the reference chopper cycle 3.장점

28. Non-Measurement Phase Stepping (NMPS) NMFS ensures that the measured photometric value at a particular wavelength will remain the same regardless of the scan speed. These overlaid scans show the same sample measured at 1800, 900, 600, 450 and 200 nm/min

29. UV/VIS/NIR Spectrophotometer Monochromator Light source Sample Light detector  Abs  Concentration Spectrum

30. Cary 500 Sample Detector • Photomultiplier Tube R928 • Easy exchange • Sensitive to both position on its surface and the angle of incidence that the light reaches the detector. PMT Detector 4.장점

31. Pbs detector • PbS--Lead Sulfide photocell • Electrothermally cooled • Stabilized near 0° Celsius (ZERO)

32. Silicon Detector • Reference Detector • The reference beam is measured using a Silicon detector. • Used to perform measurements in the following modes;Ratio Sample beam verses Reference (Double beam)Sample or Reference only (Single beam) Reference Detector

34. CARY500의 장점 • 1기기의 우수성과 다양성 • 2국내외의 다양한 USER확보 • 3다양한 APPLICATION 지원 • 4신속하고 정확한 SERVICE 지원 • 5SOFTWARE의 편리성 • 6ADL기능

35. Accessories

36. UV Accessories

37. Cuvettes

38. Cuvettes Cary 50/100/300/400/500 Flow Cells Micro cells Rectangular Cells Cylindrical Cells

39. Cell Holder Accessories

40. Cell Holders Cary 50/100/300/400/500 00-100468-00 00-100467-00 01-100269-00 02-101253-00 01-102601-90 66-100140-00 01-100599-00

41. Solid Sample Holder Accessories

42. Solid Sample Holder accessories Cary 50/100/300/400/500 Cary 400/500 Cary 100/300 Cary 50

43. Solid Sample Holder accessories Cary 50/100/300/400/500 Cary 100/300Thin Film HolderAccessory Cary 100/300Sunglass HolderAccessory Brewster AngleHolderAccessory Cary 400/500Thin Film HolderAccessory

44. Diffuse Reflectance Accessories

45. Components of reflection • The two components of reflection. Rs represents specular reflection. Rd represents diffuse reflection.

46. Diffuse reflectance accessories Cary 400/500 • Varian DRA (internal) • 110 mm diameter Sphere coated with PTFE. (density of approximately 1 g/cm3.) On board Electronics In-built PMT (R928) and NIR (PbS) detector(NIR detector not temperature controlled) • Wavelength range: 250-2500nm • The beam ports occupy 3%of the sphere’s diffusing area. • Service Manual 85-101135-00

47. Diffuse reflectance accessory • Varian DRA (internal) • Optical design

48. Position 'D' measures diffuse reflectance only. Position 'S' measures total reflectance by including the specular component.

49. Diffuse reflectance accessories • Labshere DRA-CA-5500 • Sphere 150 mm diameter coated with Spectralon PTFE. On board Electronics In-built PMT and NIR detector(NIR detector not temperature controlled) No Sample size limitations (Sample/Reference ports outside instrument)Center mount measurementsEdwards attachment (rotate the sample) • measure absorptance inside sphere insteadof reflectance(transmitted light is also integrated) • Port to surface area ratio <5%

50. Diffuse reflectance accessories • Labshere DRA-CA-5500D Downward viewing sphere Same features and specificationsas for DRA-CA-5500 Except downward viewing • Measurements of • Pastes • Powders • Loose Particulates • Liquids • Port to surface area ratio is <5%