Application Compendium - Agilent Technologies

More documents

Recommendations

Info

Experimental Calibration standards of PE/PP blends in the 35–85% PE range were prepared by dissolving different ratios of the polymers in hot (110–120 °C) tetrachloroethylene (perchloroethylene), making a roughly 3% polymer to solvent solution. The dissolved polymer mixture was then used to cast films on either PTFE coupons or KBr plates for analysis by FTIR. In the case of KBr plates, approximately 0.3 mL of the polymer solution was evenly placed on the plate. The plate was then placed on a ~70 °C hotplate until all the solvent evaporated. The coated KBr plate was allowed to cool and analysis was carried out using the Cary 630 FTIR spectrometer, equipped with a transmission sampling accessory. The ratios of the methyl IR bands (mainly PP) and the methylene CH 2 bands (both PE and PP) were used to accurately measure the weight % PE in the blend. The thickness of the film was controlled to ensure that the strongest absorbance in the 1500–1200 cm -1 region did not exceed 1.2 absorbance units (AU) and remained in the preferable 0.3–1.0 AU range (Figure 1, Y-axis). Infrared spectra recorded on these salt plate cast films consisted of 74 co-added interferograms measured at 4 cm -1 resolution. Total measurement time was 30 seconds. We developed a second, novel procedure for measuring the PE:PP blend ratio. This procedure used the same calibration solutions, but rather than salt plates, the solutions were applied to a smooth piece of PTFE. After drying in an oven at 70–80 °C, the resulting 20–50 µm thick films were easily peeled off the still warm PTFE. These self-supporting polymer cast films were then analyzed by the Cary 630 FTIR equipped with the DialPath (or TumblIR) accessory using the 100 micron pathlength cell. The polymer films easily slide between the cell windows, allowing for convenient repositioning and analysis of multiple areas of the film. This makes finding the optimal thickness (0.3–1 AU) faster, since larger pieces of polymer film can be sampled in many locations. Infrared spectra recorded of these self-supporting films consisted of 74 co-added interferograms measured at 4 cm -1 resolution. Total measurement time was 30 seconds. The new DialPath method can be used on the Agilent 4500 and 5500 FTIR spectrometers as well as the Agilent Cary 630 FTIR. The 4500 is a portable, battery operated FTIR spectrometer available with the DialPath technology. The 5500 is a dedicated, benchtop FTIR spectrometer also available with the DialPath sample interface. These instruments have the same reliable performance and patented interferometer technology as the Cary 630 FTIR, but allow for onsite and near line analysis. A calibrated method was developed and added to the Cary 630 FTIR methods library so that future unknown samples can be analyzed. The method enables an automatic calculation of the PE:PP ratio, and the numerical value and spectra of the unknown is automatically displayed and/or printed. Results and discussion: PE/PP blend cast film FTIR calibration The salt plate cast film FTIR procedure is consistent with ASTM D3900-05a (Rubber-Determination of Ethylene Units in Ethylene-Propylene Copolymers (EPM) and in Ethylene-Propylene-Diene Terpolymers (EPDM) by Infrared Spectrometry). To correct for film thickness, the absorbance of a variable component peak (in this case, PP) is measured as a ratio to another matrix peak (in this case, PE). Both the novel PTFE and the original salt plate cast film method use the same peak height ratio of the 1376 cm -1 to the 1462 cm -1 bands (Figure 1) to determine composition. The new cast film method, based on the DialPath accessory linear regression calibration plot yields R 2 =1.000 (Figure 2) and the salt plate cast film method yields the identical calibration and R 2 value. Fringing patterns are sometimes observed when smooth polymer films are measured in the mid infrared region. Fringing appears as a baseline sine wave pattern in the spectra and arises from internal reflection of the IR light inside smooth polymer films. The techniques described in this application note do not produce fringing in the areas of interest by either the salt plate or the DialPath transmission methods. In the latter case, the concave/ convex matching cell window design of the DialPath and TumblIR minimizes fringing, while providing an easy to open and clean optical cell with precise pathlength reproducibility. 2
Figure 1. The overlaid aliphatic bend region of the FTIR PE/PP blend calibration spectra. The quantitative method for %PE uses a ratio of the methyl 1376 cm -1 (mainly PP) to the 1462 cm -1 (methyl and methylene bend) band. Figure 2. The calibration plot of PE/PP blends prepared as cast films, and analyzed using the TumblIR or DialPath on the Agilent Cary 630 FTIR. The same calibration with traditional transmission compartment (film cast in salt plate) yields similar calibration results. The calibration uses the ratio of the PP band at 1376 cm -1 to that of the 1462 cm -1 band in both PE and PP. 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: Author Frank Higgins Agilent Techno
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 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
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
Page 95 and 96:
0.5 V) of the nanowires. Additional
Page 97 and 98:
appeared in the topography image. T
Page 99 and 100:
of PSS component. TEM studies of mo
Page 101 and 102:
Atomic Force Microscopy Studies in
Page 103 and 104:
on graphite and MoS2 are shown in F
Page 105 and 106:
A B C D Scan size: 5 µm. Scan size
Page 107 and 108:
images of PEDOT:PSS blend, (PEDOT -
Page 109 and 110:
Young’s Modulus of Dielectric ‘
Page 111 and 112:
Figure 3. Young’s modulus as a fu
Page 113 and 114:
Nanoindentation, Scratch, and Eleva
Page 115 and 116:
The samples listed as “D” sampl
Page 117 and 118:
Figure 6. Elastic modulus results f
Page 119 and 120:
Figure 11. Elastic modulus results
Page 121 and 122:
Sample B Figure 16. Scratch curves
Page 123 and 124:
Conclusions Nanoindentation and scr
Page 125 and 126:
measurement technique has been expl
Page 127 and 128:
References 1. J.L. Hay, “Using In
Page 129 and 130:
Theory The complex shear modulus (G
Page 131 and 132:
References 1. Jain, S.K., Bhattacha
Page 133 and 134:
LCCC relies on carrying out isocrat
Page 135 and 136:
log Mp 5 4.6 4.2 3.8 0.5 15% Water
Page 137 and 138:
Authors Wei Luan and Chunxiao Wang
Page 139 and 140:
Table 1. Chemical Information of An
Page 141 and 142:
Injection Volume Influence of Real
Page 143 and 144:
translator into three modes on diff
Page 145 and 146:
To identify the matrix influence on
Page 147 and 148:
Authors Chun-Xiao Wang and Wei Luan
Page 149 and 150:
Table 1. Polymer Additives in ASTM
Page 151 and 152:
1 2 3 4 5 1 Tinuvin P 2 BHT 3 BHEB
Page 153 and 154:
1 Tinuvin P 2 BHT 3 BHEB 4 Isonox 1
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
Page 199 and 200:
Page 201 and 202:
Page 203 and 204:
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
Page 213 and 214:
Page 215 and 216:
show all

Application Compendium - Agilent Technologies

Create successful ePaper yourself

Delete template?

Save as template?