Material Identification Through Packages using 1064nm Excitation Raman Spectroscopy
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1 Material Identification Through Packages using 1064nm Excitation Raman Spectroscopy Dr. Valerian Ciobotă Applications scientist, Europe Rigaku Analytical Devices 2012 Rigaku
2 Rigaku Founded in 1951 Family-owned & controlled Approximately 1300 employees Rigaku Analytical Devices Rigaku Owned subsidiaries Major Distributors Rigaku Analytical Devices
3 Rigaku Is well known for: X-Ray Diffraction X-Ray Fluorescence Protein Crystallography Non-destructive testing Handheld and portable Raman spectrometers Semiconductor metrology Process elemental analyzers X-Ray Sources Detectors X-Ray Optics Rigaku Analytical Devices
4 Rigaku Analytical Devices products I st Generation II nd Generation FirstGuard Progeny Xantus-2 Progeny-X Rigaku Analytical Devices
5 Outline Raman spectroscopy Raman Spectroscopy and applications Raw material identification through various packaging materials Rigaku Analytical Devices
6 Raman Spectroscopy - Measuring Principle The Raman Effect: Raman Spectroscopy is a scattering method. It is a very weak effect; only one in a million of the scattered light particles, or photons, actually exhibits the change in wavelength. incident light Sample Scattered light Stokes, lower energy (longer wavelength) than Rayleigh, <1 % Laser Scattered light with the same energy (and wavelength) as the incident light (Rayleigh), > 99% Anti-Stokes, greater energy (shorter wavelength) than Rayleigh, <<1 % Rigaku Analytical Devices
7 Raman spectroscopy and organic substances Maltose Glucose Fructose Raman intensity / a.u. Raman intensity / a.u. Raman intensity / a.u Wavenumber / cm Wavenumber / cm Wavenumber / cm Rigaku Analytical Devices
8 Raman and Fluorescence the problem the laser excitation wavelength is located in the absorption band of the fluorophore a Raman signal is overlaid by fluorescence emission Absorption Fluorescence intensity Raman wavelength / nm Rigaku Analytical Devices
9 Raman and Fluorescence the problem the laser excitation wavelength is located in the absorption band of the fluorophore a Raman signal is overlaid by fluorescence emission Absorption the solution the laser excitation wavelength has to be shifted out of the absorption band or the investigated substance has no absorption band near the laser excitation wavelength intensity Raman wavelength / nm Rigaku Analytical Devices
10 Fluorescence the Raman enemy 785 nm Intensity 1064 nm Wavenumber /cm Rigaku Analytical Devices
11 Raman spectroscopy Excellent selectivity/high resolution power Non-contact sampling through containers Water exceptionally weak scatterer Sensitive only to chemical make up of the material Fast analysis/rapid results Rigaku Analytical Devices
12 Comparison of Raman, Mid-Infrared, and Near Infrared Raman spectroscopy combines the advantages of IR spectroscopy with the advantages of NIR spectroscopy Raman spectra are easily analyzed or interpreted. IR spectra are more complex due combination bands of the same molecule groups NIR is measuring overtones and vibrational combinations It has typically broad and less specific absorptions (C-H), (N-H), and (OH) bonds Rigaku Analytical Devices
13 Comparison of Raman, Mid-Infrared, and Near Infrared NIR Spectrum Polypropylene Raman spectrum has sharp signals and therefore good chemical distinguishing power Intensity In the NIR spectrum the 1 st overtone of the O-H stretching in alcohols, phenols, organic acids occurs at ca. 1400nm. Intensity Raman Spectrum Wavelength (nm) Wavenumber cm Rigaku Analytical Devices
14 Comparison of Raman, Mid-Infrared, and Near Infrared Many materials have similar NIR spectra, therefore Require extensive use of data handling methods (chemometrics) Raman and NIR common advantage over IR, measurements can be preformed through glass and without any sample preparation But, Raman is not interfered by water like IR and NIR Example for similar NIR spectra Raman spectra Polystyrene Polyethylene PET PVC Raman intensity / a.u. Wavelength Wavenumbers / cm Rigaku Analytical Devices
15 Outline Raman spectroscopy Raman Spectroscopy and applications Raw material identification through various packaging materials Rigaku Analytical Devices
16 Raman spectra of lactose monohydrate measured through LDPE bags Lactose monohydrate Lactose monohydrate through 1 layer LDPE bag Lactose monohydrate through 2 layers LDPE bag Lactose monohydrate through 3 layers LDPE bag Lactose monohydrate through 4 layers LDPE bag LDPE bag Raman intensity Wavenumber / cm Rigaku Analytical Devices
17 Raman spectra of microcrystalline cellulose measured through LDPE bags MCC through 1 layer LDPE bag MCC through 2 layers LDPE bag MCC through 3 layers LDPE bag MCC through 4 layers LDPE bag LDPE bag Raman intensity Wavenumbers / cm Rigaku Analytical Devices
18 Raman spectra of microcrystalline cellulose measured through LDPE bags Raman intensity MCC through 1 layer LDPE bag MCC through 2 layers LDPE bag MCC through 3 layers LDPE bag MCC through 4 layers LDPE bag LDPE bag MCC 1 MCC through 1 layer 0.98 MCC through 2 layers 0.96 Wavelet Correlation Coefficient MCC through 3 layers Wavenumbers / cm -1 MCC through 4 layers Rigaku Analytical Devices
19 Raman spectra of citric acid anhydrate measured through colored LDPE bags Citric acid anhydrate Citric acid anhydrate in yellow PE bag Yellow PE bag Raman intensity Wavenumber / cm Rigaku Analytical Devices
20 Raman spectra of acetaminophen measured through black LDPE bags Acetaminophen Acetaminophen through black PE bag Raman intensity Wavenumber / cm -1 However Rigaku Analytical Devices
21 Raman spectra of acetaminophen measured through black LDPE bags it is possible to obtain a Raman spectrum from the sample as the laser burns a hole in the black bag! Rigaku Analytical Devices
22 Raman spectra of methanol measured through HDPE bottle Methanol Methanol through PE bottle PE bottle Raman intensity Wavenumber / cm Rigaku Analytical Devices
23 Raman spectra of benzyl alcohol measured through amber glass bottle Benzyl alcohol Benzyl alcohol in amber glass bottle 1l Raman intensity Wavenumber / cm Rigaku Analytical Devices
24 Raman spectra of DMSO measured through amber glass bottle DMSO DMSO in amber glass 2.5l Raman intensity Wavenumber / cm Rigaku Analytical Devices
25 Raman spectra of metformin hydrochloride measured through FIBCS sack (woven PP) Metformin hydrochloride Metformin hydrochloride through PP sack PP sack Raman intensity Wavenumber / cm Rigaku Analytical Devices
26 Raman spectra of acetaminophen measured through paper sack Acetaminophen Acetaminophen through paper bag Paper bag Raman intensity Wavenumber / cm Rigaku Analytical Devices
27 Raman spectra of calcium carbonate measured through HDPE container Calcium carbonate Calcium carbonate in HDPE container HDPE container Raman intensity Wavenumber / cm Rigaku Analytical Devices
28 Summary Packaging material LDPE clear bags Semitransparent HDPE bottles LDPE colored bags Amber glass bottles FIBCS sacks (woven PP) Paper sacks Opaque HDPE bottles Aluminum/polymer bags Black PE bags Is identification possible through this packaging material? Yes Yes Usually yes Usually yes Depends on the investigated substance Depends on the investigated substance No No No* Rigaku Analytical Devices
29 Conclusions * Raw materials cannot be measured through black PE bags without damaging the packaging material. It is important that a reference spectrum added in the library to be collected in the same packaging and same focal position as the test samples. Usually raw materials can be analyzed and identified through transparent or semi-transparent packaging using Progeny - Rigaku s1064nm excitation Raman spectrometer Rigaku Analytical Devices
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31 Your contact contact Your D-A-CH Laser 2000 GmbH Wessling Phone NORDICS Laser 2000 GmbH Stockholm Phone info@laser2000.se FRANCE Photonic Laser 2000 SAS Pessac Phone info@laser2000.fr FRANCE Telecom Laser 2000 SAS Saint-Nom la Bretèche Phone info@laser2000.fr IBERIA Laser 2000 SAS Madrid Phone info@laser2000.es
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