Application Compendium - Agilent Technologies

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Authors Melissa Dunkle, Gerd Vanhoenacker, Frank David, Pat Sandra Research Institute for Chromatography, President Kennedypark 26, 8500 Kortrijk, Belgium Martin Vollmer Agilent Technologies, Inc. Waldbronn, Germany Determination of phthalate migration from toys Using the Agilent 1260 Infi nity Analytical SFC System with an Agilent 6130 Single Quadrupole LC/MS Application Note Consumer Products 90000 80000 70000 60000 50000 40000 30000 20000 10000 0 Abstract DBP DEHP DiNP, DiDP BBzP 2 4 6 8 10 12 14 min Supercritical fl uid chromatography (SFC) can be used for the determination of polymer additives such as phthalates that can migrate or leach out of plastics. In this Application Note, the analysis of phthalates in a migration test from PVC toys is performed using the Agilent 1260 Infi nity Analytical SFC System in combination with an Agilent 6130 Single Quadrupole LC/MS. The SFC/MS approach facilitated identifi cation and quantifi cation of mixed isomer phthalates in less than 15 minutes analysis time with good repeatability.
Introduction Phthalates form a group of well known plasticizers that are often applied to soften polymers, such as PVC, in toys. High molecular weight phthalates are used as polymer additives. Phthalates are not chemically bound to PVC and can leach out or evaporate into the environment. It has been shown that, in rodents, phthalates can act as hormone-like compounds. They therefore have to be considered as a potential health risk to humans. Some well known phthalates, such as di(ethylhexyl) phthalate (DEHP), consist of a single isomer; others, such as diisononyl phthalate (DiNP) and diisodecyl phthalate (DiDP), consist of a mixture of isomers with different branching of the alkyl groups. It poses a signifi cant analytical challenge to perform the analysis of these mixed isomer phthalates. Using capillary gas chromatography (GC), a partial separation of the individual isomers (within a sample of diisononyl or diisodecyl phthalate) is obtained, but this separation is not required since quantifi cation is done on the sum of the isomers. Conversely, no GC separation is available, allowing the complete chromatographic separation of all DiNP isomers from all DiDP isomers. Moreover, in GC/MS using electron ionization (EI), all phthalates give very similar mass spectra with a most abundant ion at m/z 149. Differentiation of both mixed isomer phthalates is only possible by using the [M-alkyl] + ion (m/z 297 for DiNP, m/z 307 for DiDP) 1 . In contrast, different HPLC techniques can cover only a portion of leachable polymers, therefore reversed-phase separation and normal phase chromatography have to be used in order to cover the complete polarity range. In addition, leachables are often obtained in apolar solvents, which require solvent exchange prior to analysis if reverse phase separation is the method of choice. SFC has an advantage because it is useful for a very broad range of analytes from polar to apolar. In addition, the analysis time is signifi cantly lower than that of HPLC methods due to the superior diffusion characteristics of the mobile phase, and due to the fact that solvent exchange is usually not required. In this Application Note, the analysis of phthalates by SFC-MS is demonstrated. By using atmospheric pressure chemical ionization (APCI), [M+H] + ions are obtained that allow good differentiation of DiNP and DiDP from each other and from other phthalates. The method was applied to the determination of DiNP from a toy, according to a procedure described by the European Commission 2 . Experimental Samples and extraction procedure Stock solutions of dibutyl phthalate (DBP), butyl benzyl phthalate (BBzP), DEHP, DiNP and DiDP were prepared at 1,000 ppm in dichloromethane and stored at 4 °C. From these 2 stock solutions, a 10 ppm mixture was prepared; additionally, a dilution series for DiNP was made from 50 ng/mL–1,000 ng/mL in MeOH. Table 1 Names, abbreviations, molecular formulae, and MW information of selected phthalates. A plasticized PVC toy was analyzed according to the offi cial procedure 2 . The extraction procedure consisted of cutting two disks from the toy (about 2.5-cm diameter, corresponding to a 10-cm² surface taking both sides into consideration). Both disks were placed into a sealable glass vessel with 30 mL of artifi cial saliva solution and three metal spheres. The container was then sealed and placed on a horizontal shaker for 30 minutes. The metal spheres were added to simulate a child chewing on the toy. The solution was then transferred to a separation funnel, to which 10 mL of cyclohexane were added. The cyclohexane layer was collected, evaporated down, and reconstituted in 1 mL of cyclohexane prior to injection. Name Abbreviation Formula MW (g/mol) Ion APCI (+) Ion mass Dibutyl phthalate DBP C 16 H 22 O 4 278.34 M+H 279 Benzylbutyl phthalate BBzP C 19 H 20 O 4 312.36 M+H 313 Di(2-ethylhexyl) phthalate DEHP C 24 H 38 O 4 390.56 M+H 391 Diisononyl phthalate DiNP C 26 H 42 O 4 418.61 M+H 419 Diisodecyl phthalate DiDP C 28 H 46 O 4 446.66 M+H 447 Agilent 1260 Infi nity SFC/MS solution Part number 1260 Infi nity Analytical SFC System consisting of: G4309A • 1260 Infi nity Degasser • Aurora Fusion A5 module • 1260 Infi nity SFC Autosampler • 1260 Infi nity SFC Binary Pump • 1290 Infi nity Thermostatted Column Compartment • 1260 Infi nity Diode Array Detector VL Plus External heating device Caloratherm heater 1260 Infi nity Micro Degasser G1379A 1100 Series Binary Pump G1312A (used as make-up fl ow pump) 6130 Quadrupole LC/MS G6130B Table 2 Instrument confi guration used in the Agilent 1260 Infi nity SFC/MS solution.
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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
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: Conclusion The combination of the A
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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