Characterization of Poly(dimethylsiloxane)s by Time-of-Flight Secondary Ion Mass Spectrometry

Dong, Xia; Proctor, A.; Hercules, David M.

doi:10.1021/ma961018q

Cited by 54 publications

(54 citation statements)

References 35 publications

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“…The low mass range of the TOF-SIMS spectrum for PDMS deposited on silver substrate has been reported previously [19]. In our work, the dominant peaks corresponding to Si + , CH 3 Si + , C 3 H 9 Si + , and C 5 H 15 OSi 2 + were also observed at 28, 43, 73, and 147m/z, respectively, and the spectra of PDMS-2200 and PDMS-6140 were similar in this range.…”

Section: Resultssupporting

confidence: 88%

“…Rn and nR refer to a cyclic and a linear fragment containing an integral number (n) of repeating units, respectively. These two ion clusters were also observed under Ar + bombardment by Dong et al [19], who attributed those peaks to the fragments produced by ion-beam bombardment, not to oligomers originally present in the sample. Under Bi 1 + impact shown in Figure 2, not only were the ion clusters of [Rn+Ag] + and [nR+16+Ag] + still observed, but also silver cluster ions with odd number composition from Ag 13 to Ag 21 were detected.…”

Section: Resultssupporting

confidence: 64%

“…However, because the high mass range of TOF-SIMS spectra can provide information for the monomeric unit sequence [17], molecular weight distribution [18], end group identification [19], and tertiary conformation [20,21] of polymers in TOF-SIMS studies, high mass ranges obtained with different primary projectiles should be also compared.…”

Section: Introductionmentioning

confidence: 99%

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Characteristic Fragmentation of Polysiloxane Monolayer Films by Bombardment with Monatomic and Polyatomic Primary Ions in TOF-SIMS

Moon

Wells

Gardella

2011

J. Am. Soc. Mass Spectrom.

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This study reports the characteristic fragmentation patterns from two polysiloxane polymers that form ordered overlayer on silver substrates. Results are compared for the bombardment of various monatomic and polyatomic projectiles of Cs + , C 60 + (10 keV), Bi 1 + , and Bi 3 + (25 keV) in the high mass range time-of-flight secondary ion mass spectrometry (TOF-SIMS) spectra.Results are reported from sub-monolayer (solution cast) coverages of poly(dimethylsiloxane)s with the number average molecular weights (M n ) of 2200 and 6140 Da, respectively, and Langmuir-Blodgett monolayers of poly(methylphenylsiloxane) with molecular weights (MW) from 600 and 1000 Da. For each film, Bi projectiles resulted in the emission of positive silver cluster ions from the substrate under the polymer overlayer and peaks corresponding to silver cluster ions with larger mass were observed by impact of polyatomic 25 keV Bi 3 + projectiles. In addition, depending on the change of energy of Bi 3 + , a different pattern of fragments was observed. With Cs + and C 60 + impact, however, the emission of silver cluster ions was not detected. In the case of C 60 + impact for PDMS-6140, peaks corresponding to silver-cationized intact oligomers were not observed. In this paper, these results are explained by the possible bombardment mechanism for each projectile, based on its mass, energy, and split trajectories of the component atoms under the polyatomic impact.

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Section: Resultssupporting

confidence: 88%

Section: Resultssupporting

confidence: 64%

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Characteristic Fragmentation of Polysiloxane Monolayer Films by Bombardment with Monatomic and Polyatomic Primary Ions in TOF-SIMS

Moon

Wells

Gardella

2011

J. Am. Soc. Mass Spectrom.

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“…3,17,18 Figure 2 shows the TOF-SIMS spectrum of PDMS-2200, applied as a submonolayer film on silver, in the m/z 1000-4000 range (the lower m/z range, containing PDMS fragment ions, is not shown). Silver cationized PDMS oligomers, ranging in size from n = 13 to beyond 46 repeat units, are observed in Figure 2.…”

Section: Pdms 2200mentioning

confidence: 99%

Quantitative mass spectrometry of technical polymers: a comparison of several ionization methods

Yan¹,

Ammon²,

Gardella³

et al. 1998

Eur. J. Mass Spectrom.

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The development of soft ionization methods such as matrix-assisted laser desorption/ionization (MALDI), electrospray ionization (ESI) and secondary ion mass spectrometry (SIMS) has led to an increased use of mass spectrometry in characterizing technical (synthetic) polymers. In this paper, we compare the relative performance of these three ionization methods for characterizing the molecular weights, polydispersities and quantification of relative amounts of polymer components in mixtures. Two polymers used in biomaterials, poly(dimethylsiloxane) and poly(ethylene glycol), are employed as the model polymer systems for our survey because of their well-defined molecular weights and importance as surfactants in biomaterials and because many of their surface and solutionphase properties are well understood. Matrix-assisted laser desorption/ionization can be used to examine the surface and bulk composition of biomaterials, whereas secondary ion mass spectrometry is used for examining monolayer and submonolayer coverage of polymers on surfaces and electrospray ionization is suited for examination of extractables from biomaterials. Secondary ion mass spectrometry and electrospray show discriminate behavior against ionization of higher molecular weight oligomers, especially of poly(dimethylsiloxane). Matrix-assisted laser desorption/ionization appears to exhibit the best performance for reliable molecular weight determination at higher masses and polydispersity characterization as well as for quantification of components in polymer mixtures. The results are discussed within the context of the ionization mechanisms by which each soft ionization technique operates and by the attributes of the mass analyzers (time-of-flight and Fourier transform mass spectrometers) employed.

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“…28,29 In the case of low-molecular-weight PDMS (silicone 1), the relative intensity of the linear fragments (a) was high, whereas in the case of high-molecular-weight PDMS (silicone 2), the relative intensity of the cyclic fragments (F) was high. These results agree with the results of PDMS deposited on silver substrates.…”

Section: Molecular Weight Evaluation and Silicone Structurementioning

confidence: 99%

Molecular Weight Evaluation of Poly(dimethylsiloxane) on Solid Surfaces Using Silver Deposition/TOF-SIMS

Inoue¹,

Murase²,

Sugiura³

2004

ANAL. SCI.

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Molecular ions include information about end groups, functional groups and molecular weight. A method for the direct detection of these in the high mass range (m/z > 1000) from poly(dimethylsiloxane) (PDMS) on a solid surface was investigated. It was found that a TOF-SIMS analysis of silver-deposited surfaces (silver deposition/TOF-SIMS) is useful for this purpose. Using the silver-deposition/TOF-SIMS method, silver-cationized quasi-molecular ions were clearly detected from PDMS on solid surfaces, and their structure and molecular weight were evaluated. In addition, their images were observed without the interference of deposited silver. By applying to the analysis of paint defects etc., it was confirmed that this technique is useful to analyze actual industrial materials. Silver-cationized ions were detected not only from PDMS, but also from other organic materials, such as lubricant additives and oils on solid surfaces. Therefore, the silver deposition/TOF-SIMS method was proved to be useful for the analysis of ultrathin substances on solid surfaces.

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Characterization of Poly(dimethylsiloxane)s by Time-of-Flight Secondary Ion Mass Spectrometry

Cited by 54 publications

References 35 publications

Characteristic Fragmentation of Polysiloxane Monolayer Films by Bombardment with Monatomic and Polyatomic Primary Ions in TOF-SIMS

Characteristic Fragmentation of Polysiloxane Monolayer Films by Bombardment with Monatomic and Polyatomic Primary Ions in TOF-SIMS

Quantitative mass spectrometry of technical polymers: a comparison of several ionization methods

Molecular Weight Evaluation of Poly(dimethylsiloxane) on Solid Surfaces Using Silver Deposition/TOF-SIMS

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