HANDHELD FTIR BEST ON-SITE CHEMISTRY ANALYSIS SOLUTION. Presented by: Dr. Yanqia Wang

Transcription

1 HANDHELD FTIR BEST ON-SITE CHEMISTRY ANALYSIS SOLUTION Presented by: Dr. Yanqia Wang

2 Outline Background of FTIR Spectrometry and Agilent Handheld FTIR - TopScan 4300 Versatile sampling interfaces (Diamond/Ge ATR, Specular Reflection, Grazing Angle Reflection and Diffuse Reflection) to satisfy different applications. Powerful and user-friendly software to assist easy data collection and analysis qualitatively and quantitatively. Excellent outcome from real applications. Potential Applications

3 Infrared Light Heat Motion of atoms and molecules IR radiation/absorption

4 Principles of IR Spectroscopy Most organic molecules absorb light in the infrared region to yield IR absorption spectra Absorption at certain frequencies or wavenumbers corresponds specifically to certain vibrations of functional groups Absorbance of the spectral features is associated with the concentration of the certain components Qualitative and Quantitative Characterization

5 FTIR Spectrometer Key components of an FTIR spectrometer. Reference IR Source Laser Laser Moving Mirror Detector Fixed Mirror Sample Cell IR Detector

6 Smaller is Better Computer Evolution FTIR Evolution

7 Mobile FTIR (Thanks to Smaller Interferometer) 1998 Mini Size:10 ¼ x 12 x 4 ½ Weight: 10 lbs Midget Size:4 ¼ x 2 ½ x 5 ¾ Weight: 3.6 lbs 2007 Micro Size:2 ½ x 2 ¾ x 4 ¼ Weight: 1.9 lbs 2013 Nano

8 Comparison Research vs Field FTIR Spectrometer ~4x scale Source: Multiple vs Single Laser: Gas Phase vs Solid State Beam Splitter: Interchangeable vs Fixed Alignment: Multi-adjustments vs Pin in place Detector: Multiple vs Single 8

9 Performance Performance Trading Rules Number of Adjustments versus Alignment Tolerance Maximum Adjustments Optimum Performance Research system Optimum adjustments Stable Performance Field system 0 Alignment 0 Alignment Agilent portable systems are designed to have stable performance. Small changes in alignment have a minimal effect on performance. 9

10 Common Specifications Multiple Instruments from the same engine Frequency range cm -1 (ZnSe) cm -1 (KBr) Maximum Resolution 2 cm -1 Non-hygroscopic optics ZnSe beam splitter Power AC or Onboard Lithium Ion Battery Operating temperature 0⁰ to 50⁰ C Humidity 95% non-condensing

11 RELIABLE: From White Coats to Work Boots

12 Where to find a Handheld FTIR? Parking lots, Mine pits, Workshops, Warehouses, wild field Anywhere and even a regular lab Agilent Confidential

13 Moving Measurements From the Lab to the Field Analysis on Location Too big for lab / object can not be moved Faster Time to Answer Lab is too far / samples need to be sent away Deployment of Routine Analysis Program Non technical user can used field systems Increase QBD (quality by design) effort Cost savings 13 March 17, 2016

14 Requirements for Field and Routine Use Effective Performance Achieve required measurement limits Analytical performance still matters Form Factor Compact, Rugged, Portable, Versatile System needs to go where the sample is Frequent travel/inexperienced users - subjects it to shock and vibration Correct Sampling Interfaces Little or no sample prep Versatility: Multiple uses and matrices Ease of Use and Provide Answers Easy to understand, meaningful results 14

15 Handheld Opto-Chemical Instrumentation Smart Phone UV-Vis NIR FTIR QCL-MIR Light-absorption Based Raman XRF LIBS Sci-Fi do-it-all Light-interaction (e.g. Scattering,Emission) Based

16 Advantages of Handheld FTIR over other Handheld Systems FTIR can be used for both chemical qualification and quantitation Non-destructive Works for a wide variety of samples with versatile sampling interfaces Abundant spectral database and method support. Less sample restriction (e.g. fluorescence interference for Raman) Safety (Laser, X-Ray)

17 Advantages of TopScan 4300 over Other Handheld FTIR Really Handheld Truly Rugged Same optics that are used in our bench systems not a WATERED DOWN VERSION Can be used in any direction Permanently aligned optics (No dynamic alignment is necessary) High Flexibility Optics/Sealed Desiccated Compartments No need to worry about KBr beam-splitters and desiccant No need to purge your system Competitive 14 lbs 8.6 x 11.8

18 Evolution of Handheld FTIR Confidentiality Label March 17, 2016

19 Award Winning Design (TopScan 4300) Multi Functional RFID Embedded Accessory Ergonomic Design 2KG, balanced Mobile and PC Control Robust and Graceful Battery or AC Agilent Confidential

20 4300 Handheld FTIR Overview The most powerful handheld FTIR ever developed OVERVIEW Ergonomics ~4.5 lbs, balanced Engine + electronics ~60 in 3 Performance Optimized Great scan speed (5.6 scans/second@ 4 cm -1 ) MARKETS Expand existing markets Materials Energy Food WHY WE WILL BE SUCCESSFUL Proven applications Better ergonomics Increased usability Defend current market position Fast software response Agilent Confidential

21 Handheld Models Features 4300MCT 4300DTGS ExoScan 4100 Lightweight 2 kg 3.2 kg Measurement Speed 5.6 scans/sec 2.3 scans/sec 2.3 scans/second Software Response Every 0.3 sec Every 1 sec Smart Sampling RFID None Sample Interface Interchangeable Interchangeable Docking Station Yes Yes Battery Life 2+ hours 3 hours SNR >4000:1 >3000:1 >3500:1 Resolution 4 cm -1 4 cm -1 Frequency Range cm cm cm -1 Interferometer Nano Micro Detector MCT DTGS DTGS Battery Pair, Hot-swap Single Agilent Confidential

22 TopScan 4300 Advantages for Field Measurement Lighter weight, Balanced, Ergonomic 2 kg Compact size Access to difficult sample locations High performance Meets the needs of challenging applications Integrated Computer Fast response for real time answers Ease of use Straightforward application-specific software Microlab Agilent Confidential 22 March 17, 2016

23 IR Sampling Techniques Path length Specular Reflectance Sample I o I 1 Diffuse Reflectance Sample Transmittance Liquid cell Gas cell KBr pellet technique Sample Reflectance (External) Diffuse reflectance accessory Specular reflectance accessory Grazing angle reflectance accessory ATR Crystal Reflectance (Internal) ATR accessory Bulk Surface Surface Other Types of Accessories Fiber optics probe Photo-acoustic spectroscopy (PAS)

24 Attenuated Total Reflectance (ATR) Diamond/Ge ATR Surface contact required Solids or liquids Consistent path length Little or No sample Prep Infrared Energy Path Sample Evanescent Wave ~ 2 um

25 Reflectance Diffuse Reflectance Specular Reflectance

26 Handheld FTIR with Multiple Sample Interfaces Spherical ATR ID of Solids or liquids Gross surface contamination Thick coating identification - paints External Reflectance (45⁰) Metal and composite surfaces Surface oxidation, coating thickness and chemistry ID of thin coatings Grazing Angle (~82⁰) Used for smooth metal surfaces Cleaning validation Trace contaminant identification Bonding applications Diffuse Reflectance Rough samples Geology applications Heat damage applications

27 4300 Handheld FTIR - Sampling Flexibility RFID: Easily change I/F s in the field RFID Identifier Auto-sets Gain in the Field when changed Allows user to lock methods according to sampling interface Sampling interfaces available: Diffuse reflectance External Reflectance Diamond ATR Ge ATR Grazing Angle Reflectance

28 4300 Handheld FTIR - Instrument Stand Upward Looking Position Stages for External Ref, Grazing Angle, D-ATR and Ge-ATR sample interfaces Downward Looking Position Diffuse Reflectance for Powders, soils, and other complex sample media

29 How do I choose the right system for me? Laboratory or field deployable system? Choice A: Lab based system Flexibility Dedicated analysis or flexibility? Dedicated Cary 630 Interchangeable sampling interfaces Auto Recognition No alignment KBr or ZnSe Optics 5500 Series FTIR Dedicated sampling interfaces Optimized for performance No alignment ZnSe Optics Only 29 March 17, 2016

30 How do I choose the right system for me? Laboratory or field deployable system? Choice B: Combined Use System NDT Sample type: NDT or Liquids/ Powders 4300 TopScan FTIR Interchangeable sampling interfaces ZnSe Optics Battery Operated Docking Station for Laboratory Development work 4500 Series FTIR Dedicated sampling interfaces Optimized for performance Battery or Mains line ZnSe Optics for portability 30 March 17, 2016

31 How do I choose the right system for me? Laboratory or field deployable system? Choice C: Field Use system How often is it in the field? 4100 Exoscan DTGS MCT 31

32 Microlab PC Method Driven Software Visually instruct users through collection User Levels Administrator, Certification, Operator Methods Data collection Library search Quantitative Results Green, yellow, red display based on limits PC and Mobile Full collection/ prediction on mobile Sync. Between mobile and PC

33 Microlab PC - Fast Data Collection

34 Microlab PC Quant Module The latest Microlab PC has embedded a Quant module, a Simple, guided methods development package for quantitative applications. Different Quant Algorithms allows single/multiplecomponent quantitations Simple Beer s Law Classical Least Squares Inverse Least Squares (Also known as Inverse Beer s Law, or Multiple Linear Regression)

35 Microlab PC Easy Report Generation MicrolabPC component formatting Microsoft Word Add-on enables easy report formatting Multiple template function PDF generation

36 Infield Applications for Handheld 4300 Materials Coatings Coating Identification Surface cleanliness and preparation Coating wear and weathering Composites Heat and UV Damage on Composites Composite Cure Polymers UV resistance and weathering Polymer ID. Energy Wind Heat damage, coating wear and composite cure of wind blades Solar Coating performance, UV damage, Material ID Geology Ground Truth-ing Mineralogy Soil Science Food Incoming ID, Product Quality Agilent Confidential

37 Absorbance Handheld Application Heat Damage Oxidation of Carbon Composite Aircraft and other structures will increasingly be constructed from composite material Composites are susceptible to heat and oxidative damage Heat or UV Damage In service or mfg damage Chemical damage of the epoxy resin Prior to delamination Infrared provides an effective nondestructive testing to detect heat damage EN_AppNote Composites Serve as Primary Structural Material Carbon laminate Carbon sandwich Other composites Aluminum Titanium High damage Wavenumber Other Steel 5% 10% CFRP 43% Titanium 15% Aluminum 20% No damage Misc. 9% Composites 50% 1200

38 Hand Held FTIR Surface Contamination Diffuse Reflectance and Grazing Angle FTIR well suited to surface contamination Hydrocarbon and Silicone are strong absorbers Unique signal = positive ID of contaminant Different Sample Interfaces for Aluminum and Carbon Fiber Aluminum highly reflective -> Grazing angle interface Carbon fiber low reflectivity -> Diffuse Reflectance 38

39 Soil Analysis by Handheld FTIR - Soil Mid-IR signal can be correlated to key parameters (ph/hydrogen, Electrical Conductivity, Extractable Al, Ca, Mg and Total Carbon and Nitrogen) - Massive amount samples: time consuming and expensive - Comparison between benchtop and mobile FTIR (PLS-Cross Validation predictions and comparisons) 39

40 Hand Held FTIR in Art Conservation Measurement of oxalates on paint FTIR has been used for years in art conservation Typically microscopy Small samples removed from paintings for analysis Beigan s Chao-Tian Temple in Taiwan Vibrant red painted doors Stained black Soot? Algae growth? Diffuse Reflection (Non-destructive) Black covering most of door Red spots where black wore off Oxalates found on black areas Oxalates formed as a by-product of biological growth Oxalate formation and removal is a growing area of art conservation 40

41 Potential Application: Ground-Zero Chemical ID In 2015, a series of massive explosions rocked Tian Jin, a harbor city in China. Hundreds tons of different hazardous chemicals on ground zero need to be identified ASAP. Handheld FTIR is believed to be the best solution NaNO 3 KNO 3 NH 4 NO 3 NaCN 41

42 Potential Application: Melamine/Urea Formaldehyde Dinnerware ID Plastic shatter-proof dinnerware has become very popular in people s life. Melamine Formaldehyde dinnerware is widely used due to its strength and heat-resistance. While someone thinks cheaper Urea Formaldehyde can do the same thing. Fine for hot soup Melamine Formaldehyde Nothing hot 42

43 Summary Agilent Handheld FTIR provided a valid way to bring spectrometers to the samples, enable fast and accurate on-site or in-field FTIR analysis. Wide selection of sampling interfaces can meet the challenges of different applications. Easy-using software ensure customer s need for fast data collection and qualification/quantitation characterization The value of the handheld FTIR has been approved by many successful applications.

44 4300 Handheld FTIR Demonstration 44 Confidentiality Label March 17, 2016

45