Analysis of linear and cyclic oligomers in polyamide-6 without sample preparation by liquid chromatography using the sandwich injection method

Mengerink, Ynze; Peters, Ron; Kerkhoff, M. Jonell; Hellenbrand, J; Omloo, H; Andrien, J; Vestjens, M; Wal, Sj. van der

doi:10.1016/s0021-9673(00)00179-5

Cited by 27 publications

(21 citation statements)

References 20 publications

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“…The dimer C2 and trimer C3 were coeluded as a single peak whereas the other cyclic oligomers were well resolved. This peculiar behavior has been observed with cyclic polyamides as well [15]. At the moment we are unable to offer a plausible explanation.…”

Section: Mass Spectral Identificationmentioning

confidence: 66%

Separation and identification of an oligomeric light stabilizer Chimassorb 944 by gradient elution chromatography coupled with matrix-assisted laser desorption/ionization mass spectrometry

Kong

Diao

Wan

2014

Journal of Chromatography A

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Section: Mass Spectral Identificationmentioning

confidence: 66%

Separation and identification of an oligomeric light stabilizer Chimassorb 944 by gradient elution chromatography coupled with matrix-assisted laser desorption/ionization mass spectrometry

Kong

Diao

Wan

2014

Journal of Chromatography A

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“…Stoffers et al (2003) determined the total amount of laurolactam and oligomers in PA12 food packaging films by extraction with 95% ethanol at 60 C for 24 h. Begley et al (1995) determined PA6 and PA66 oligomers in a PA oven-roasting bag by dissolving the bag with a mixture of methylene chloride and hexafluoroisopropanol (HFIP) and precipitating the polymer with methanol. Mengerink et al (2000) used formic acid as the PA solvent and water as the non-solvent, determining the oligomer content in self-produced PA6. Kricheldorf et al (2003) isolated soluble fractions from a PA6 by dissolving the polymer in trifluoroethanol (TFE) and precipitating with methanol.…”

Section: Please Scroll Down For Articlementioning

confidence: 99%

“…Angeli and Marino (2007) isolated antioxidants from a PA66 powder using TFE as a PA solvent and a mixture of chloroform, isopropanol and cyclohexane as the precipitating agent. Mengerink et al (2000) introduced an alternative method for determining oligomer content by directly injecting the dissolved polymer into HPLC system, and compared direct injection with dissolution/precipitation (formic acid/ water) and extraction (methanol and water). It was shown that an extraction method clearly has a drawback, as only caprolactam, the cyclic dimer and trimer are extracted efficiently, while, for example, the cyclic hexamer is not extracted completely, even after 100 h of extraction (water or methanol).…”

Section: Please Scroll Down For Articlementioning

confidence: 99%

“…Thus, at least for the cyclic PA6 oligomers the agreement of RRFs can be considered as sufficient for their use in the estimation of the amount of migrating PA6 oligomers by HPLC-UVD. Mengerink et al (2000) showed that dissolution/ precipitation with formic acid/water is more efficient than extraction with methanol for the determination of cyclic oligomers in PA6 (see the Introduction). Consequently, in this paper a dissolution/precipitation procedure was preferred to an extraction method, also because it is less time consuming and offers the possibility of proving the completeness of isolation.…”

Section: Relative Response Factors (Rrfs)mentioning

confidence: 99%

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Cyclic oligomers in polyamide for food contact material: quantification by HPLC‐CLND and single‐substance calibration

Heimrich

Bönsch

Nickl

et al. 2012

Food Additives & Contaminants: Part A

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Cyclic oligomers are the major substances migrating from polyamide (PA) food contact materials. However, no commercial standards are available for the quantification of these substances. For the first time the quantification of cyclic oligomers was carried out by HPLC coupled with a chemiluminescence nitrogen detector (CLND) and single-substance calibration. Cyclic monomer (MW = 226 Da) and dimer (MW = 452 Da) of PA66 were synthesised and equimolar N detection of CLND to synthesised oligomers, caprolactam, 6-aminohexanoic acid (monomers of PA6) and caffeine (a typical nitrogen calibrant) was proven. Relative response factors (UVD at 210 nm) referring to caprolactam were determined for cyclic PA6 oligomers from dimer to nonamer, using HPLC-CLND in combination with a UVD. A method for quantification of cyclic oligomer content in PA materials was introduced using HPLC-CLND analysis and caffeine as a single nitrogen calibrant. The method was applied to the quantification of cyclic PA oligomers in several PA granulates. For two PA6 granulates from different manufacturers markedly different oligomer contents were analysed (19.5 versus 13.4 g kg⁻¹). The elution pattern of cyclic oligomers offers the possibility of identifying the PA type and differentiating between PA copolymers and blends.

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“…Although cyclic oligomers have been detected in polytetrahydrofurans [10] and in polyester samples [11 14] (the latter contain approximately 1 3% of cyclic species [14]), and polyamides [15,16] Number of repeat units (P) Figure 6. Dependence on the number of repeat units, P, of the ratio of fluorescence response to UV response (peak height).…”

Section: Lc-ms Investigationsmentioning

confidence: 99%

Determination of the molecular weight and other physicochemical properties of poly(bubylene glycol) 1000 by gradient RPHPLC and measurement of the ELSD, UV, and fluorescence responses

Rißler¹,

Socher²,

Glöckner³

2001

Chromatographia

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SummaryMolecular weight and other physicochemical data for poly(butylene glycol) 1000 (PBG 1000) have been determined by use of a new, highly efficient, gradient reversed-phase highperformance liquid-chromatographic (RPHPLC) procedure. Separation of the native material or its 0~, o.~-bis(1-naphthylurethane) derivative was achieved on a Cls stationary phase with a ternary acetonitrile-water-tetrahydrofu ran mobile phase. Detection was achieved by measu rement of the signal response from evaporative light scattering (ELSD), UV, and fluorescence (FD) detection.Proof that all the ohgomers contained in the sample had been separated by the method was obtained by liquid chromatography coupled with electrospray ionization time-of-flight mass spectrometry (LC-ESI-TOFMS). Itwas also confirmed by this technique that di(buf,/lene glycol) is the lowest homologue in the sample. Although the dimer was also observable in the HPLC-UV trace of the PBG 1000 0~, o.~-bis(1-naphthylurethane) derivative, it was obviously too volatile to be seen in the ELSD trace; tri(butylene glycol) was, nevertheless, still recognizable with sufficient signal intensily.Because all the homologues were separated to baseline, the method was used to calculate the number-and weight-average molecularweights, NI,7 and NI,,,,, both from peak areas and from peak heights. The best fit to data obtained from end-group titration were obtained from calculations based on the HPLC-UV response; NI,7 values of 948 and 937 were obtained from peak heights and areas, respectively NI,7 and NI,,,, values calculated from the ELSD trace obtained from native PBG 1000 were substantially (ca 10%) lower that those calculated from the UV trace obtained from the 0~, o.~-bis(1-naphthylurethane) derivative. Similar differences were also discovered by comparing the NI,7 and NI,,,, values obtained from UV and FD-values were approximately 20% higherfor FD.When the retention times of individual ohgomers, from either ELSD of the native sample or from UV-FD of the 0~, o.~-bis(1-naphthylurethane) derivative, were plotted against the number of repeat units, P, the ELSD curve approaches the UV-FD curve atvalues of Pof approximately 60. This observation can be explained by the pronounced contribution of the hydrophobic endgroups to the overall retention of PBG 1000; the effect of this decreases with increasing chain length and becomes nearly independent of Ponlyfora very high degree of polymerization.

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Analysis of linear and cyclic oligomers in polyamide-6 without sample preparation by liquid chromatography using the sandwich injection method

Cited by 27 publications

References 20 publications

Separation and identification of an oligomeric light stabilizer Chimassorb 944 by gradient elution chromatography coupled with matrix-assisted laser desorption/ionization mass spectrometry

Separation and identification of an oligomeric light stabilizer Chimassorb 944 by gradient elution chromatography coupled with matrix-assisted laser desorption/ionization mass spectrometry

Cyclic oligomers in polyamide for food contact material: quantification by HPLC‐CLND and single‐substance calibration

Determination of the molecular weight and other physicochemical properties of poly(bubylene glycol) 1000 by gradient RPHPLC and measurement of the ELSD, UV, and fluorescence responses

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