Application Compendium - Agilent Technologies

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Authors Ben MacCreath, Ian Willoughby, Greg Saunders Agilent Technologies, Inc. Analysis of Poly(styrene/butadiene) Copolymers by Conventional Gel Permeation Chromatography on the Agilent PL-GPC 50 Plus Application Note Introduction A poly(styrene/butadiene) block copolymer (SBR) mimics many of the properties of natural rubber and has applications in a wide variety of industrial areas. The characteristics are provided by the hard polystyrene chains being surrounded by a network of rubbery polybutadiene, which provides strength and flexibility over a large temperature range. The copolymer is a thermoplastic elastomer and therefore can easily be used in manufacturing by injection moulding, or blended into an existing product to increase elasticity or impart toughness. The molecular weight distribution is critical, as any homopolymer will significantly affect the resultant end properties.
Methods and Materials Conditions Columns: 2 x Agilent PLgel 5 µm MIXED-C, 300 x 7.5 mm (part number PL1110-6500) Eluent: Tetrahydrofuran (250 ppm BHT) Flow Rate: 1.0 mL/min Sample Concentration: 2.0 mg/mL Injection Volume: 100 µL Temperature: 40 °C Calibration Standards: Agilent Polystyrene EasiVial Detection: PL-GPC 50 Plus, DRI Results and Discussion Chromatograms for three poly(styrene/butadiene) block copolymer samples are shown in Figure 1. Figure 2 reveals the copolymer overlaid molecular weight distributions. Each peak eluted as a relatively narrow main peak indicative of ionic polymerization. The molecular weights of the components of the samples were different, due to a change to the synthesis conditions employed. The main peak of each sample was the block copolymer. However, one of the samples also contained a smaller peak eluting after the main peak, indicating the presence of homopolymer at lower molecular weight. Evidence of high molecular weight termination products is provided by the small peaks eluting before the main peak. The presence of these peaks is a result of imperfections in the polymerization processes used to manufacture the materials. 0 min 25 Figure 1. Chromatograms for three samples of poly(styrene/butadiene) – each sample eluted as a multi-modal distribution of relatively sharp peaks 3.7 dw/dlog M 0 4.1 log MW 6.3 Figure 2. Overlaid molecular weight distributions for the poly(styrene/ butadiene) samples Conclusion Three samples of poly(styrene/butadiene) were analyzed by conventional gel permeation chromatography on the PL-GPC 50 Plus. Distinct differences were observed arising from presence of homopolymers, along with the anticipated copolymer. This application note demonstrates how GPC may be used to assess the products of complex synthesis reactions to gain mechanistic insights into polymerization processes. www.agilent.com/chem This information is subject to change without notice. © Agilent Technologies, Inc. 2010 Published in UK, September 9, 2010 SI-02369
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MATERIALS TESTING AND RESEARCH SOLU
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When accuracy and reliability in me
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AGILENT TECHNOLOGIES APPLICATIONS F
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Figure 1. Agilent Cary 630 FTIR spe
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The calibration samples were measur
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Author Frank Higgins Agilent Techno
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Figure 1. The overlaid aliphatic be
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Author John Seelenbinder Agilent Te
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Figure 3. Sample is lightly pressed
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Author Dr. Mustafa Kansiz Agilent T
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microscopy provides for a factor of
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Standard ATR IR Image No Pressure (
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A visual inspection of the sample u
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Experimental Instrumentation To per
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Authors Jonah Kirkwood † and Must
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Spectra were collected from each lo
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Infrared mapping allows for multipl
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The spectra in Figure 2 are visuall
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Conclusion Agilent‟s Cary 610 FTI
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Authors Dr. Wayne Collins*, John Se
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The calibration curve obtained for
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Conclusion Select ‘Peak Ratio’
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Summary This method describes a pro
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Method configuration To determine t
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The calibration curve for the deter
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Figure 6. The MicroLab PC FTIR soft
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Summary An analytically representat
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Figure 3. The Irganox 1010 peak are
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The calibration curve and equation
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Select ‘Peak Ratio’ - from the
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Summary An analytically representat
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Figure 3. The GMS peak height absor
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Advanced Atomic Force Microscopy: E
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signal) image indicating the overwh
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A dependence of surface potential o
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A B C Figure 6A-C. The topography (
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A B Figure 10A-C. The topography (A
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KFM with AM-FM operation in the int
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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
Page 157 and 158: Results and discussion To meet the
Page 159 and 160: Authors Melissa Dunkle, Gerd Vanhoe
Page 161 and 162: Experimental The analyses were perf
Page 163 and 164: Repeatability of the SFC/MS analysi
Page 165 and 166: Conclusion The combination of the A
Page 167 and 168: Introduction Phthalates form a grou
Page 169 and 170: The analytical method was applied t
Page 171 and 172: Introduction Bisphenol A (BPA) is a
Page 173 and 174: Preparation of standards BPA and BP
Page 175 and 176: Limit of Detection (LOD) and Limit
Page 177 and 178: Sample analysis The content of BPA
Page 179 and 180: The calibration for BPA and BPF, wh
Page 181 and 182: Author Stephen Ball Agilent Technol
Page 183 and 184: Results and discussion By operating
Page 185 and 186: Introduction The wavelength of UV r
Page 187 and 188: LC parameters Premixed solutions of
Page 189 and 190: Linearity A linearity study was per
Page 191 and 192: References 1. Dr. James H. Gibson,
Page 193 and 194: Instrumentation Columns: 2 x PLgel
Page 195 and 196: Authors Greg Saunders and Ben MacCr
Page 197 and 198: Authors Greg Saunders, Ben MacCreat
Page 205 and 206: Author Greg Saunders Agilent Techno
Page 207: Figure 5. Universal calibration cur
Page 211 and 212: Materials and Methods A column set
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