Application Compendium - Agilent Technologies

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FTIR is widely used to identify the chemical composition of impurities present in materials, and the traditional approach to this application would be to scrape the surface of the spark plug to try to isolate a small portion from the area of interest. The materials would then be placed under the microscope and spectra would be collected. However, a simpler and completely nondestructive solution uses a micro-ATR FTIR with a large sample objective accessory (see Figure 1). The benefi t of this arrangement is that the spark plug samples can be analyzed ‘as is’, with no intricate sample preparation required. Figure 1. Top: Schematic of the patented Agilent Large Sample Microscope Objective accessory. Bottom: Photograph of the Large Sample Microscope Objective accessory. Experimental Instrumentation An Agilent Cary 610 FTIR microscope fi tted with a slide-on micro ATR and a Large Sample (LS) Objective accessory was interfaced to an Agilent Cary 660 FTIR spectrometer. The patented large sample microscope objective allows the measurement of unlimited sized samples in refl ection or ATR single-point or imaging mode. In this study, the slide-on micro Ge ATR was mounted onto the objective, which points the infrared light out towards the front of the microscope, as indicated in Figure 1. Sample analysis No sample preparation was required for the analysis. The spark plug was simply placed against the 90 degree objective of the Cary 610 FTIR microscope. The system was confi gured with standard mid-IR components (mid- IR source, KBr beamsplitter, 250 micron narrow band MCT microscope detector) with data collected at 4 cm -1 spectral resolution with 16 co-added scans (5 seconds). Results and discussion It was clear from zooming in on this spark plug that there were three areas of interest (Figure 2). These included the white lubricant, a potential contaminant (black speck) and the electrode tip with excess deposits. Figure 2. Side view during ATR analysis of three distinct sampling locations on a defective spark plug using the Agilent Large Sample Objective 2
Spectra were collected from each location in 5 seconds each. The spectra were overlaid using the Agilent Resolutions Pro software so that the data could be investigated visually, as shown in Figure 3. Figure 3. FTIR spectra acquired from three sampling locations of a spark plug overlaid using Agilent Resolutions Pro software. Each data set was acquired in 5 seconds. All three spectra of interest were searched against a large commercially available spectral database. The Resolutions Pro software provides direct access to the largest commercially available FTIR libraries, including a signifi cant number of databases that are dedicated to polymer and materials applications. Alternatively, custom-made libraries can be searched. The results of the search indicated conclusively that the white lubricant was of a silicon polymer based material. The black contaminant was identifi ed as poly(ethylene terephthalate) (PET) with the desposits on the electrode likely to consist of silicone containing oily material. In this case study, it was likely that the electrode tip deposits were derived from oil and fuel additives, which suggested that fuel and oil were leaking past worn valve guides and piston rings into the combustion chamber, causing hard starting and misfi ring. This information enabled corrective action to be taken to prevent further costly repairs and downtime due to damaged vehicle components. Conclusion The Agilent 660 FTIR interfaced to a micro-ATR 610 FTIR microscope with Large Sample Objective accessory is capable of analyzing unlimited sized samples that are diffi cult to measure using conventional FTIR whilst being nondestructive, hence enabling further analysis via other methods if required. This enabled the direct and rapid analysis of faulty spark plugs that had visible deposits encrusted on the side and center electrodes of the terminal. The use of a commercial spectral library for the identifi cation of unknown contaminants revealed that the deposits were derived from oil and fuel additives. Overall, the method is suitable to resolve component failure issues quickly and effi ciently, increasing productivity or reducing downtime in the process, and ultimately saving money. 3
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: Authors Jonah Kirkwood † and Must
Page 33 and 34: Infrared mapping allows for multipl
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
Page 83 and 84:
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
Page 191 and 192:
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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Application Compendium - Agilent Technologies

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