The world leader in serving science

Michael S. Bradley

Approachable Raman SolutionsThe Shortest Path from Problem to Answer

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Thermo Scientific Raman Spectroscopy: Discover. Solve. Assure.

• Raman Spectroscopy Discovers• Imaging provides a wide view of your sample• High spatial resolution gives specific insights• Polarization probes molecular alignment

• Raman Spectroscopy Solves• Identify materials• Probe beneath the surface (confocal)

• Raman Spectroscopy Assures• Image entire pharmaceutical tablet for composition

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• You cover a lot of ground with the DXR2xi

• Fast collection to build an image

• Intuitive, image based software

The Thermo Scientific DXR2 Raman Spectrometers

• With the DXR2 Microscope you can:

• Point and Shoot with high spatial resolution

• Map regions for step-by-step data collection

Thermo Scientific™ DXR™2 Raman microscope Thermo Scientific™ DXR™2xi Raman imaging microscope

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The Thermo Scientific DXR2 Family of Raman Spectrometers

• DXR2 System Basics:• Lasers

• 455 nm• 532 nm• 633 nm• 785 nm

• Rayleigh rejection filter• 50 cm-1 cut-off

• Apertures• Slit• Pinhole (confocal mode)

• Gratings• Standard, 5 cm-1

• High Resolution, 2 cm-1

• Detectors• CCD, EMCCD

SampleGrating Aperture

Laser

Multichannel detector

Filter

50

2DG

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Point-and-Shoot: Raman Through Evidence Bags

Single Nomex Aramid Fiber in Evidence BagSingle Nomex Aramid Fiber on Glass Slide

Single Kevlar Fiber in Evidence BagSingle Kevlar Fiber Glass Slide

400 600 800 1000 1200 1400 1600 1800 cm-1

Trace Evidence Fiber Identification

Raman Shift (cm-1)

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Point-and-Shoot: Explosive Materials

Trace TNT Specimen TNT

PETN

C-4

Raman Shift (cm-1)

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Imaging: Focus on the IMAGE

• Chemical Imaging provides visualizations of chemical differences• The individual spectra are of secondary importance

• DXR2xi sets parameters, collects data and provides real-time visual interpretation at the IMAGE level

• It’s better to work with an image than with thousands of spectra

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Imaging: Get Only What You Need

• Optimize IMAGE collection, not individual spectra• Entire image is collected in a single scan• Experimental results are clear before image collection is complete

• You can interactively balance parameters on the fly• Stop whenever the results are good enough

1 micron pixels191,000 spectra, 2 scans25 minutes

5 micron pixels30,000 spectra, 2 scans4 minutes

20 micron pixels1900 spectra, 2 scans1 minute

Better! Better?

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Surface Analysis of an Entire Painkiller Tablet: Wide Area Scan

Acetaminophen Caffeine Titanium DioxideAspirin

MCR Analysis

Collection Parameters11 × 11 mm surface area

532 nm laser, 10× objective

226,000 spectra, 25 µm pixel size

Acquisition at 550 Hz (1.8 ms/spectrum)

8 minute collect time!

Determine:• Size of each domain• Distribution of domains• Overall composition of tablet

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Very High Resolution MCR Analysis of Pharmaceuticals

Sodium Lauryl Sulfate Microcrystalline Cellulose

Acetaminophen Caffeine StarchAspirin

225 × 250 µm surface area532nm laser, 100× objective

229,000 spectra, 0.5 µm pixel sizeAcquisition parameters: 100 Hz (10 ms/spectrum)

38 Minute Collection Time

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• Strongest Raman signal from focused laser point• Weak signal from out-of-focus regions of the sample

• Non-destructive depth analysis• Dependent on aperture size and objective• Depth selected by focusing z-axis of microscope stage

Confocal Raman Microscopy

Detector

Aperture

Objective

FocusPlane

Sample

Lift sample stage

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Confocal 3D Imaging: Waveguide in LiNbO3

100X

3DNotations for Raman images

orientation.

Optical overlaid with Raman image constructedas area of ν(OH) band at 3500 cm-1

XY areas acquired at different Z depths

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Label-Free Raman Image of Live U2OS Cells

Lipids 2900 – 2950 cm-1

DNA 784 cm-1 Proteins 1640-1664 cm-1Video Image

MCR

60x Water Immersion Objective

Raman images of major biomolecular components within a living U2OS cell

Image Pixel size 0.50 microns, 8300 spectra, 3 second collect, 2:26 hr

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Septarian Nodule: A concretion of sedimentary rock where angular cavities and cracks have been filled in with other minerals

Location and Identification of Mineral Phases

Visual

5.0 x 3.4 mm27200 spectra25 µm image pixel sizeExposure Time 0.02 s100 scans

QuartzDolomite

Carbon + DolomiteCarbon + ArakiteApatite

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Zoom In To Smaller Area

More Intensive Look in a Small Area

385 x 340 µm5236 spectra5.0 µm image pixel sizeExposure Time 0.02 s100 scans

PyriteLazurite + Pyrite + Carbon

Apatite + CarbonCarbon + SideriteCarbon

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Raman Polarization

• Used to characterize:• Symmetry• Molecular orientation• Crystallinity• Morphological traits

PerpendicularParallel

n1

n2

n3

n4

DepolarizationRatio

I ┴ (VH)I ǁ (VV)

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Orientation of SWCNT on a Surface

• Developing high speed, low power semiconductors• Aligned SWCNTs are semiconducting

University of WisconsinDept. of Material Science and Engineering

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Imaged area on next slide

Quality of Alignment of SWCNT

Laser polarization parallel to SWCNT axisZ(YY)Z̅

Laser polarization perpendicular to SWCNT axisZ(XX)Z̅

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Imaging the Alignment of SWCNT

Laser polarization parallel to SWCNT axisZ(YY)Z̅

Laser polarization perpendicular to SWCNT axisZ(XX)Z̅

An orientation image created from the ratio of polarized Raman images provides a complete assessment of SWCNT alignment quality:

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Multimodal Raman Spectroscopy

• The Thermo Scientific™ iXR™ Raman Spectrometer• Uses DXR components• Designed for integration with other analytical techniques

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XPS-Raman Integration

• XPS-Raman with Thermo Scientific™ Theta Probe XPS

Name Atomic%C 76.0O 16.8Ag 4.9Si 1.3Zn 0.5Ni 0.4G Band

2D Band1D Band

RadialBreathing Modes

0.00E+00

2.00E+05

4.00E+05

6.00E+05

8.00E+05

1.00E+06

1.20E+06

01002003004005006007008009001000110012001300

Cou

nts

/ s

Binding Energy (eV)

15 Scans, 8 m 30.4 s, 400µm, CAE 200.0, 1.00 eV

Si 2s

C 1sAg 3d

O 1s

Ni 2pZn2p

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Rheo-Raman MARSXR Study of Polystearate in Hand Cream

• Combined Rheometry-Raman results• Black dots: Intensity of the CH2 twisting mode of polystearate• Green Curve: G’ (storage modulus)• Open Circles: The intensity of a non-polymer vibration

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Phase Transition Study

• A polyethylene disc was analyzed during a temperature sweep from 100º to 155 ºC• The Raman scatter was based on the CH2 twist mode (1296 cm-1) • The solid, transition and melt phases are highlighted in blue, green and yellow

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Thermo Scientific Raman Spectroscopy

Thermo Scientific™ DXR™2 Raman microscope

Thermo Scientific™ DXR™2xi Raman imaging microscope

Thermo Scientific™ Raman Analyzer Solutions

Thermo Scientific™ FirstDefender™ RM Chemical Identification System and Thermo Scientific™ TruScan™ RM

Handheld Analyzer

Thermo Scientific™ Nicolet™ iS™50 FT-IR Spectrometer with Raman Module

Thermo Scientific™ DXR™2 SmartRaman

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Serving Your Science

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Thank You

Please join me in theMaterials Science Researchsection of our booth where I’ll

address comments and questions.