Application Compendium - Agilent Technologies

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Results and discussion Analysis of polymer additives using SFC-APCI-MS in positive mode The test mixture, containing six typical polymer additives, was analyzed using the separation conditions given in Table 3. The separation obtained using these generic SFC conditions in APCI (+) mode is shown in Figure 1. Suffi cient resolution between all compounds is achieved in 10 minutes analysis time. The test mixture contains analytes typically added at different steps of the manufacturing process of the packaging material, including diisononylphthalate (a plasticizer), Irgaphos 168 (a tris-arylphosphite processing stabilizer), Irganox 1010 (a sterically hindered phenolic antioxidant), Tinuvin 234, and Tinuvin 440 (hindered amine light stabilizers/UV absorbers) and erucamide (a slip, antistatic, antisticking agent). All these compounds can be separated and detected using SFC and good quality mass spectra are obtained, as illustrated in Figure 2 for Irgaphos 168 and Irganox 1010. Typically, [M+H]+ ions are prevalent, except for Irganox 1010 where an ammonium adduct is detected. As shown in the TIC trace in Figure 1, erucamide and Tinuvin 440 are not chromatographically separated using the SFC conditions. However, based on their different mass spectrum, peak deconvolution using extracted ion chromatograms, clearly proves the presence of two different compounds as illustrated in Figure 1B (EIC 338 = erucamide) and Figure 1C (EIC 436 = Tinuvin 440) . 600000 400000 200000 0 120000 80000 40000 0 300000 200000 100000 0 A) TIC 1 2 3 4 5 6 7 8 9 B) EIC 338 ERU 1 2 3 4 5 6 7 8 9 C) EIC 436 T440 1 2 3 4 5 6 7 8 9 Figure 1 TIC of the SFC-APCI(+)MS analysis of the polymer additive test mixture (A) and the EIC of the two coeluting compounds erucamide (B) and Tinuvin 440 (C). 80 60 40 20 Figure 2 APCI(+) Mass spectra of A) Irgaphos 168 giving a clean spectra of the M+1 ion (647) and B) Irganox 1010 giving a spectra of the ammonium adduct (1195). Note that the spectra have different x-axis scales. 4 I168 DiDP T234 I1010 ERU, T440 100 Max: 239296 H 3C H 3 C H3C H3C CH 3 0 300 350 400 450 500 550 600 650 700 100 80 60 40 20 CH3 H3C H3C O HO (CH2) 2 C H 3 C CH 3 CH3 CH3 O) 3 P O CH2 C 4 970.5 647.5 649.4 648.5 Max: 167168 0 300 400 500 600 700 800 900 1000 1100 m/z min min min 1192.7 1196.7 1195.7 1194.7 m/z
Repeatability of the SFC/MS analysis was demonstrated by analyzing the test mixture six times. As illustrated in Table 4, excellent retention time reproducibility was obtained. Peak area repeatability was in the order of 5–10% taking into consideration that this is measured on raw peak areas obtained on extracted ion chromatograms from (APCI) scan acquisition. The analysis of the standard mixture of typical polymer additives clearly illustrates that SFC/MS is a useful tool for these type of applications. The described generic SFC/MS method can be applied to different classes of additives. It is also applicable for the analysis of other irganox, tinuvin, phthalate or amide type polymer additives. Since most polymers do not contain very complex cocktails of additives, it is in most cases not necessary to use slower modifi er programs which results in increased analysis time. Screening of polymer extract The potential of SFC/MS is also demonstrated by the analysis of an extract obtained from a polymer intended to be used for food packaging. The polymer was extracted in 15% ethanol. After 24 hours at 40 °C, the solution was analyzed. The total ion chromatogram obtained by SFC-APCI(+)MS in scan mode is shown in Figure 5. The fi rst eluting compound was determined as an antioxidant (sterically hindered phenol). Retention time Peak area Ion Average % RSD Average % RSD I168 647 3.168 0.52 1870000 9.62 DiNP 447 3.489 0.41 4995000 8.23 T234 448 4.296 0.29 3702500 8.08 I1010 1195 5.670 0.22 2417500 7.60 T440 436 6.832 0.27 2622500 8.00 ERU 338 6.899 0.21 599875 7.99 Table 4 Reproducibility data. 180000 160000 140000 120000 100000 80000 60000 40000 20000 0 Figure 5 TIC of the SFC-APCI(+)MS analysis of ethanol/water extract of polymer. 5 2 4 6 8 10 min
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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 ‘
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: Experimental The analyses were perf
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 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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Authors Greg Saunders, Ben MacCreat
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Authors Greg Saunders, Ben MacCreat
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