Application Compendium - Agilent Technologies

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Figure 3. The FTIR spectra of four SBR rubber standards with increasing polystyrene concentrations: 0% (purple), 5% (red), 23% (green), and 45% (blue) Figure 4. FTIR calibration curve for polystyrene in SBR rubber using the 699 cm -1 peak height absorbance; R 2 =0.999. Ratio of polyethylene to vinyl acetate in PEVA Polyethylene vinyl acetate (PEVA) is very common in everyday products used in the home, sports equipment, industrial and medical applications. In the latter applications, medicines can be mixed in solution with PEVA and then the mixture dried to produce biologicallyinert, slow-release plastic implants and transdermal patches. Since the ratio of polyethylene (PE) to vinyl acetate (VA) in PEVA can affect the physical properties of the fi nal product, it is important for manufacturers to have a fast, easy measurement procedure for these components. As in the previous example, the Cary 630 FTIR spectrometer with single refl ection diamond ATR is ideal for this measurement. In this example, seven commercially-available standards of PEVA were measured with the Cary 630 FTIR system. The calibration standards used were: • Polyethylene, low density (0% vinyl acetate) • Ethylene/vinyl acetate copolymer #506 (9 wt% vinyl acetate) • Ethylene/vinyl acetate copolymer #243 (14 wt% vinyl acetate) • Ethylene/vinyl acetate copolymer #244 (18 wt% vinyl acetate) • Ethylene/vinyl acetate copolymer #245 (25 wt% vinyl acetate) • Ethylene/vinyl acetate copolymer #316 (28 wt% vinyl acetate) • Ethylene/vinyl acetate copolymer #326 (40 wt% vinyl acetate) 3
The calibration samples were measured with one minute collection times, at a resolution of 4 cm -1 . The FTIR spectra exhibit strong acetate ester carbonyl bands at 1737 cm -1 and an ester C-O stretch band at 1236 cm -1 (Figure 5) arising from polyvinyl acetate (VA). Both of these bands are ideal for quantitative analysis of the VA in the polyethylene (PE) matrix. The characteristic PE absorbance bands are located at 2921cm -1 , 2852 cm -1 , 1467 cm -1 and 720 cm -1 . The best calibration is obtained by a peak area ratio of the 1236 cm -1 VA absorbance band ratioed to the PE absorbance at 1467 cm -1 . This IR absorbance ratio technique corrects for random variables that may affect the measurement, such as contact pressure or contact area of the polymers on the ATR diamond crystal. This is important since reliable ATR measurements require the sample to make good optical contact with the diamond, and hard, round polymer beads may not contact the whole diamond surface. Absorbance 0.6 0.5 0.4 0.3 0.2 0.1 0.0 3500 Polyethylene 2921 2852 Polyvinylacetate Figure 5. Spectral overlay of the calibration standards for polyethylene vinyl acetate). The spectra are all scaled to the polyethylene absorbance. The blue spectrum is 40 wt% VA, and the red spectrum is 0% VA The resulting linear regression calibration curve from the above peak area ratio is excellent (Figure 6) with a correlation coeffi cient of R 2 = 0.999. The slope and offset for the linear regression is easily inserted into the MicroLab FTIR method editor (Figure 6), and the resultant method is now permanently calibrated. To test the robustness of the method, validation standards 1737 3000 2500 2000 1500 Wavenumber (cm-1) 1372 1236 1020 1000 1467 were made by diluting (by weight) the 9% VA with the pure PE (0% VA) standards to make 1% and 0.55% VA samples. The polymer validation samples were then dissolved in toluene and heated to 75 °C until all the polymer dissolved. The toluene mixtures were then cast as thin fi lms onto aluminum foil over a 60 °C hotplate and allowed to dry. The resulting polymer validation samples were then measured with the stored method. These validation samples were measured with a much shorter scan time (5 seconds) than the calibration set of spectra (60 seconds). This allows for multiple measurements of incoming raw materials in a very short time; this fast sample analysis is important for quality assurance and quality control (QA/QC) analysis. The speed of this analysis is also a benefi t for incoming raw materials analysis in which a batch of PEVA can have some uniformity differences, requiring sampling from multiple areas of the container or on a molded part. The results of this fast analysis (5 second) yield exceptional repeatability and accuracy (Table 1) on the validation samples. A standard deviation of nominally 0.01% VA was obtained with limits of detection (LOD) and limits of quantitation (LOQ) of 0.03 wt% VA and 0.10 wt% VA, respectively. When a sample is run using this calibrated FTIR method, the results can also be displayed in colorcoded format (Figure 7), indicating that the sample is in-spec (green), marginal (yellow), or out of spec (red). This enables an operator to get a rapid, visual indicator of the quality of the material. Table 1. VA prediction values from the calibrated VA FTIR method for validation standards at 0.55% VA and 1.00% vinyl acetate in polyethylene. These validation samples were run with only 5 second collection times 4 Validation sample 0.55% VA 1.00% VA Rep 1 0.53 0.97 Rep 2 0.54 0.96 Rep 3 0.55 0.96 Rep 4 0.56 0.96 Rep 5 0.55 0.99 Standard deviation 0.0114 0.0130 Average 0.55 0.97
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: Figure 1. Agilent Cary 630 FTIR spe
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 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 49 and 50: Authors Dr. Wayne Collins*, John Se
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 59 and 60:
Authors Dr. Wayne Collins*, John Se
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
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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
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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
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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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