Application Compendium - Agilent Technologies

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1 Methods and Materials KEY Conclusion Conditions Samples: Polysaccharides Columns: 2 x Agilent PL aquagel-OH MIXED-M 8 µm, 300 x 7.5 mm (p/n PL1149-6801) Injection Volume: 200 µL Eluent: 0.2 M NaNO + 0.01 M 3 NaH PO 2 4 Flow Rate: 1.0 mL/min Detector Train: 390-MDS incorporating Viscometer and DRI Detector Temp: All detectors set at 40 °C The 390-MDS was chosen as part of the system as it is capable of multidetector GPC in aqueous solvents and therefore allows the complex nature of these materials to be investigated. Results and Discussion Figure 1 shows an example overlaid multi-detector chromatogram for a sample of pullulan polysaccharide. The material eluted as a broad peak. DRI Viscometer 0 min 25 Figure 1. Overlaid multi-detector chromatogram for an example of pullulan polysaccharide Figure 2 shows an overlay of the accurate molecular weight distributions of the two samples under investigation. As can be seen, they have very different molecular weight distributions. dw/dlog M 0 3 log M 7 Figure 2. Overlaid multi-detector molecular weight distributions of two samples of polysaccharide Figure 3 shows the overlaid Mark- Houwink plot of log intrinsic viscosity as a function of molecular weight for the two samples. Compared to the pullulan, the dextran shows a marked shift of the Mark-Houwink plot to lower intrinsic viscosity values at any given molecular weight. This indicates that dextran is smaller in solution than pullulan across the molecular weight range, a result of the presence of branching on the dextran molecules. The dextran plot is complex and shows some changes in slope, indicating that the degree of branching varies across the range of molecular weight, as expected for a complex material. 0.4 log IV -1.0 Blue - Dextran Green - Pullulan 3.9 log M 6.4 Figure 3. Overlaid Mark-Houwink plots for the two samples of polysaccharide The data in this application note illustrates how multi-detector GPC employing the 390-MDS can be used to clearly see structural differences between pullulan and dextran with a highly branched structure. www.agilent.com/chem This information is subject to change without notice. © Agilent Technologies, Inc. 2010 Published in UK, September 13, 2010 SI-02389
Authors Greg Saunders, Ben MacCreath Agilent Technologies, Inc. Characterization of Block Copolymers Synthesized via Transition Metal Mediated Living Radical Polymerization Application Note Introduction Polymerization reactions mediated by the presence of a transition metal have received much interest in both literature and the commercial world. These processes allow the controlled synthesis of polymers of predetermined molecular weight, polydispersity and well-defined architecture using cheap and synthetically simple procedures. Generation of a carbon radical initiates freeradical polymerization in the presence of a monomer and a suitable solvent. Termination steps are minimized by the reversible nature of the radical formation reaction. Careful tailoring of the relative reaction rates can lead to well-controlled polymerizations where termination steps are sufficiently controlled to allow polymers of polydispersity of 1.1 to be produced from the reaction. These reactions typically follow psuedo-first order kinetics. The ability to readily convert hydroxyl functional groups to active initiator groups ready for polymerization leads to a convenient synthetic pathway for the synthesis of architecturally diverse materials such as stars, blocks and grafts. One such class of polymer structures that may be prepared using this synthetic process are block copolymers. These copolymers are made up of two or more chains that contain different repeat units that are known as blocks, for example a block of polystyrene connected to a block of polymethyl methacrylate repeat units. The materials are of interest because under certain conditions they facilitate phase separation, forming nanostructures with properties that differ from the equivalent blended material or from random copolymers of the monomers used in the two blocks. Determining the molecular weight of block copolymers is not straightforward as the composition of the material affects the molecular dimensions, which in turn means that molecular weights determined by conventional GPC using only a refractive index detector are inaccurate. However, using viscometry, it is possible to determine the molecular weights of these materials by the universal calibration approach.
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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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Page 155 and 156: 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
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Page 205 and 206: Author Greg Saunders Agilent Techno
Page 207 and 208: Figure 5. Universal calibration cur
Page 209 and 210: Methods and Materials Conditions Co
Page 211 and 212: Materials and Methods A column set
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