Application Compendium - Agilent Technologies

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Authors Dr. Wayne Collins*, John Seelenbinder † and Frank Higgins † Agilent Technologies * Wilmington, DE, USA † Danbury, CT, USA Determination of percent ethylene in ethylene-propylene statistical copolymers Analytical method Polymers Scope This method is for the determination of the statistical or randomly distributed ethylene content of ethylene-propylene copolymers. The determination is specific for ethylene and cannot be applied for the quantitation of other comonomers. The method has been validated over the range of 0.3 to 3.5% statistical content and can be used for either powder or pellet samples. Certain sorbitol-based clarifiers have been found to interfere with the determination and therefore a correction factor is necessary for resins containing these additives. This method is generally not recommended for quantitation of ethylene in filled or pigmented resins.
Summary This method describes a procedure for measuring the statistical ethylene contents in ethylene-propylene statistical copolymers. The procedure utilizes an absorption band at 733 cm -1 associated with statistically distributed ethylene for a Beer’s Law type calculation. An analytically representative sample of the copolymer resin is molded into a film of thickness between 0.5 and 0.7 mm. Molding conditions are not important to the results obtained by this method, as long as the resin is not subjected to temperatures of more than 250 °C for more than 2 to 3 minutes, and the films have a smooth, consistent surface. The sample is placed in the infrared spectrometer and the spectrum is obtained at a resolution of 4 wavenumbers or better. Using the Agilent DialPath or TumblIR accessories, the film or coupon can be inserted into the infrared beam path between the top and bottom crystals (Figure 1). Both these accessories are unique to Agilent and provide a revolutionary new way to measure thin polymer films or liquids. The horizontal mounting provides a simple, fast and reproducible mechanism to mount the sample by simply laying it down flat and rotating the crystal into position, eliminating errors and providing accurate and reliable answers — fast! The peak height of the absorbance band at 733 cm -1 is determined relative to a baseline drawn between 759 and 703 cm -1 . This value is divided by the peak height of the absorbance band at 1044 cm -1 relative to a baseline drawn between 1068 and 949 cm -1 to give the normalized absorbance at each wavenumber. The random ethylene concentrations can then be determined by comparing these values with a linear regression equation of normalized absorbance versus ethylene content for a set of standards of known ethylene content as determined by C 13 nuclear magnetic resonance spectroscopy (NMR), which is a primary analytical technique. At least three separate films are analyzed and averaged for each sample analyzed. Figure 1. The Agilent DialPath transmission cell used for polymer analysis of coupons or films Apparatus • Data is obtained using an Agilent Cary 630 FTIR spectrometer equipped with a DialPath or TumblIR sample interface with a 1000 μm path length. Equivalent FTIR spectrometers, such as the mobile or portable Agilent 5500/4500 Series FTIR, can also be used. • Hydraulic press — with heated platens capable of maintaining 200 °C and a ram force of 25,000 pounds. • Chase mold — to control thickness (optional). • Aluminum sheet — 0.05–0.18 mm thick. Calibration Standards are prepared by measuring the statistical ethylene content of a series of copolymers covering the desired range using by NMR, which is a primary analytical technique. To perform the calibration, prepare and analyze at least three films for each standard resin in accordance with the requirements of this method. All absorbance values should be less than 1.6 units. Perform a linear least squares regression of the concentration of the analyte versus normalized absorbance using all data points; do not include the 2
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 and 32: Spectra were collected from each lo
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: Conclusion Select ‘Peak Ratio’
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
Page 85 and 86: Figure 1. AFM topographic image of
Page 87 and 88: 100nm 100nm 350nm 100nm Figure 3. A
Page 89 and 90: to perfect hexagonal patterns, whic
Page 91 and 92: Single-pass KFM studies have been k
Page 93 and 94: 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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