Application Compendium - Agilent Technologies

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Author Dr. Jonah Kirkwood, Dr. John Wilson and Dr. Mustafa Kansiz Agilent Technologies, Inc. Material analysis by infrared mapping: A case study using a multilayer paint sample Application Note Introduction Agilent‟s 610 FTIR fourier transform infrared (FTIR) microscopes are routinely used for the analysis of heterogeneous materials. They provide an ability to characterize the spatial distribution of components as well as the ability to identify the specific chemical nature of a sample. Agilent‟s infrared microscopes can be used on both the microscopic and macroscopic scale using multiple measurement modes including: � transmission � reflection � attenuated total reflectance (ATR) � grazing angle reflection analysis � „large sample‟ mode using Agilent‟s large sampling side-port accessory They are ideal for advanced materials characterization as they are simple to use, provide the best sensitivity and versatility, and can be customized to suit a desired area of analysis. By adding a motorized sample stage to an Agilent Cary 610 FTIR single-element detector microscope system, the capabilities can be extended to include automated infrared mapping analysis.
Infrared mapping allows for multiple infrared spectra to be sequentially acquired from different spatiallyresolved points on the same sample and provides both spectral and spatial information, thereby facilitating the study of within-sample chemical heterogeneity. Common infrared mapping applications in material sciences include simple material characterization, the analysis of the homogeneity of coating materials, the investigation of multi-layer sample interfaces such as polymer laminates and paint cross-sections, the automated screening of samples for defects or contamination, the characterization of the total reflectance of optical surfaces and other process control applications. This paper highlights the simplicity and power of Agilent‟s Agilent Cary 610 infrared mapping microscope for the rapid and automated analysis of a multi-component paint sample. Instrumentation The infrared mapping experiment was conducted using a Cary 610 FTIR spectrometer, equipped with a 610 FTIR infrared microscope (containing a 250 micron single-element, narrow-band Mercury Cadmium Telluride detector and a motorized sample stage) operating under Resolutions Pro 5.0 software. A constant flow of dry air was used to purge the system, limiting the contributions from carbon dioxide and atmospheric water vapor. The infrared map was collected in reflection-mode using a pre-loaded grid mapping template that was customized to collect a 19 × 19 grid (totaling 361 spectra) using a 20 µm step size from an area measuring 380 × 380 microns. The infrared spectra were sequentially recorded over the range of 4000–700 cm -1 at a spectral resolution of 8 cm -1 by co-adding 16 scans per point (~40 mins for the entire infrared map). 2 Sample preparation The paint chip cross sections were prepared from vehicle paint fragments provided by a police forensic laboratory. Samples were mounted in a clear casting polyester resin, and then polished using a 12,000mesh Micromesh polishing cloth. The embedded paint fragments were microtomed to a thickness of ~10 µm, and the samples transferred to a standard glass microscope slide that was covered with aluminum foil to allow for reflection/absorption analysis. Results and discussion Infrared mapping using Agilent‟s Cary 610 FTIR Microscope allows for the automated sequential acquisition of hundreds of high-quality infrared spectra from analytical samples. Using Resolutions Pro software, mapping experiments are extremely flexible. Users can either select individual spectral collection locations themselves or use one of several grid mapping templates that can be customized to a sample, saved and re-applied later. In this experiment, a paint fragment found at an automobile crime scene was embedded in a polymer resin, then microtomed to obtain an appropriate sample thickness. This sample was deposited onto the surface of a reflective infrared support slide which was then placed on the motorized stage of the microscope. A visual image of the paint sample was acquired, followed by the sequential collection of the 361 spectra (19 × 19 grid map; 380 × 380 µm area) using automated infrared mapping. The visual image of the sample and the spectral acquisition locations are shown in Figure 1. Each spectrum in the infrared map results from a spatial resolution of 20 µm.
Page 1 and 2: MATERIALS TESTING AND RESEARCH SOLU
Page 3 and 4: When accuracy and reliability in me
Page 5 and 6: AGILENT TECHNOLOGIES APPLICATIONS F
Page 7 and 8: Figure 1. Agilent Cary 630 FTIR spe
Page 9 and 10: The calibration samples were measur
Page 11 and 12: Author Frank Higgins Agilent Techno
Page 13 and 14: Figure 1. The overlaid aliphatic be
Page 15 and 16: Author John Seelenbinder Agilent Te
Page 17 and 18: Figure 3. Sample is lightly pressed
Page 19 and 20: Author Dr. Mustafa Kansiz Agilent T
Page 21 and 22: microscopy provides for a factor of
Page 23 and 24: Standard ATR IR Image No Pressure (
Page 25 and 26: A visual inspection of the sample u
Page 27 and 28: Experimental Instrumentation To per
Page 29 and 30: Authors Jonah Kirkwood † and Must
Page 31: Spectra were collected from each lo
Page 35 and 36: The spectra in Figure 2 are visuall
Page 37 and 38: Conclusion Agilent‟s Cary 610 FTI
Page 39 and 40: Authors Dr. Wayne Collins*, John Se
Page 41 and 42: The calibration curve obtained for
Page 43 and 44: Conclusion Select ‘Peak Ratio’
Page 45 and 46: Summary This method describes a pro
Page 47 and 48: Method configuration To determine t
Page 51 and 52: The calibration curve for the deter
Page 53 and 54: Figure 6. The MicroLab PC FTIR soft
Page 55 and 56: Summary An analytically representat
Page 57 and 58: Figure 3. The Irganox 1010 peak are
Page 61 and 62: The calibration curve and equation
Page 63 and 64: Select ‘Peak Ratio’ - from the
Page 65 and 66: Summary An analytically representat
Page 67 and 68: Figure 3. The GMS peak height absor
Page 69 and 70: Advanced Atomic Force Microscopy: E
Page 71 and 72: signal) image indicating the overwh
Page 73 and 74: A dependence of surface potential o
Page 75 and 76: A B C Figure 6A-C. The topography (
Page 77 and 78: A B Figure 10A-C. The topography (A
Page 79 and 80: KFM with AM-FM operation in the int
Page 81 and 82: ibbons is only slightly different f
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References 1. G. Binnig, C.F. Quate
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Figure 1. AFM topographic image of
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100nm 100nm 350nm 100nm Figure 3. A
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to perfect hexagonal patterns, whic
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Single-pass KFM studies have been k
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images due to the difference of the
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0.5 V) of the nanowires. Additional
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appeared in the topography image. T
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of PSS component. TEM studies of mo
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Atomic Force Microscopy Studies in
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on graphite and MoS2 are shown in F
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A B C D Scan size: 5 µm. Scan size
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images of PEDOT:PSS blend, (PEDOT -
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Young’s Modulus of Dielectric ‘
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Figure 3. Young’s modulus as a fu
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Nanoindentation, Scratch, and Eleva
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The samples listed as “D” sampl
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Figure 6. Elastic modulus results f
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Figure 11. Elastic modulus results
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Sample B Figure 16. Scratch curves
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Conclusions Nanoindentation and scr
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measurement technique has been expl
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References 1. J.L. Hay, “Using In
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Theory The complex shear modulus (G
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References 1. Jain, S.K., Bhattacha
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LCCC relies on carrying out isocrat
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log Mp 5 4.6 4.2 3.8 0.5 15% Water
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Authors Wei Luan and Chunxiao Wang
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Table 1. Chemical Information of An
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Injection Volume Influence of Real
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translator into three modes on diff
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To identify the matrix influence on
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Authors Chun-Xiao Wang and Wei Luan
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Table 1. Polymer Additives in ASTM
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1 2 3 4 5 1 Tinuvin P 2 BHT 3 BHEB
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1 Tinuvin P 2 BHT 3 BHEB 4 Isonox 1
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Authors Edgar Naegele Agilent Techn
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Results and discussion To meet the
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Authors Melissa Dunkle, Gerd Vanhoe
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Experimental The analyses were perf
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Repeatability of the SFC/MS analysi
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Conclusion The combination of the A
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Introduction Phthalates form a grou
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The analytical method was applied t
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Introduction Bisphenol A (BPA) is a
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Preparation of standards BPA and BP
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Limit of Detection (LOD) and Limit
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Sample analysis The content of BPA
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The calibration for BPA and BPF, wh
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Author Stephen Ball Agilent Technol
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Results and discussion By operating
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Introduction The wavelength of UV r
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LC parameters Premixed solutions of
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Linearity A linearity study was per
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References 1. Dr. James H. Gibson,
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Instrumentation Columns: 2 x PLgel
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Authors Greg Saunders and Ben MacCr
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Authors Greg Saunders, Ben MacCreat
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Author Greg Saunders Agilent Techno
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Figure 5. Universal calibration cur
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Methods and Materials Conditions Co
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Materials and Methods A column set
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