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Identification of VOCs from natural rubber by different headspace techniques coupled using GC-MS.

Talanta (2018-09-29)
Nor H Kamarulzaman, Nhat Le-Minh, Richard M Stuetz
ABSTRACT

Different extraction procedures were evaluated to assess their potential for measuring volatile organic compounds (VOCs) from raw rubber materials. Four headspace sampling techniques (SHS, DHS, HS-SPME and µ-CTE) were studied. Each method was firstly optimised to ensure their reliability in performance. Passive sampling was also compared as a rapid identification of background VOCs. 352 VOCs were identified, 71 from passive sampling and 281 from active headspace sampling, with 62 not previously reported (hexanenitrile, octanone, decanal, indole, aniline, anisole, alpha-pinene as well as pentanol and butanol). The volatiles belonged to a broad range of chemical classes (ketones, aldehydes, aromatics, acids, alkanes, alcohol and cyclic) with their thermal effects (lower boiling points) greatly affecting their abundance at a higher temperature. Micro-chamber (µ-CTE) was found to be the most suitability for routine assessments due to its operational efficiency (rapidity, simplicity and repeatability), identifying 115 compounds from both temperatures (30 °C and 60 °C). Whereas, HS-SPME a widely applied headspace technique, only identified 75 compounds and DHS identified 74 VOCs and SHS only 17 VOCs. Regardless of the extraction technique, the highest extraction efficiency corresponded to aromatics and acids, and the lowest compound extraction were aldehyde and hydrocarbon. The interaction between techniques and temperature for all chemical groups were evaluated using two-way ANOVA (p-value is 0.000197) explaining the highly significant interactions between factors.

MATERIALS
Product Number
Brand
Product Description

Supelco
SPME fiber assortment kit 2, for use with autosampler, needle size 23 ga
Supelco
SPME StableFlex fiber assortment kit, needle size 23 ga, for use with autosampler
Supelco
SPME fiber assortment kit 4, for use with autosampler, needle size 23 ga
Supelco
SPME fiber assembly, Carbowax-Polyethylene Glycol (PEG) Coating, needle size 23 ga, df 60 μm (PEG), for use with autosampler
Supelco
SPME fiber assembly, Carbowax-Polyethylene Glycol (PEG) Coating, needle size 23 ga, df 60 μm (PEG), metal alloy fiber, for use with manual holder
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), for use with autosampler, needle size 23 ga, metal alloy fiber
Supelco
SPME fiber assortment kit 5, needle size 23 ga, for use with autosampler
Supelco
SPME fiber assortment kit 2, for use with manual holder, needle size 24 ga
Supelco
SPME fiber assortment kit 1, for use with autosampler, needle size 24 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), fused silica fiber, df 65 μm (PDMS/DVB), for use with manual holder, needle size 23 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 24 ga, for use with autosampler
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 24 ga, for use with manual holder
Supelco
SPME fiber assortment kit 1, for use with manual holder, needle size 24 ga
Supelco
SPME StableFlex fiber assortment kit, for use with manual holder
Supelco
SPME fiber assortment kit 4, for use with manual holder, size 24 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 24 ga, StableFlex, for use with manual holder
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 24 ga, StableFlex, for use with autosampler
Supelco
SPME fiber assortment kit 2, for use with autosampler, size 24 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), for use with autosampler, needle size 23 ga
Supelco
SPME fiber assortment kit 1, for use with autosampler, needle size 23 ga
Supelco
SPME StableFlex fiber assortment kit, for use with autosampler, needle size 24 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 23 ga, PDMS/DVB StableFlex, for use with autosampler
Supelco
SPME fiber assortment kit 4, for use with autosampler, size 24 ga
Supelco
IonSense® PDMS/DVB SPE-it Tips, pkg of 96 ea
Supelco
SPME LC Tips, C18, tray of 96 ea
Sigma-Aldrich
2-Heptanone, 99%
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 100 μm (PDMS), for use with autosampler, needle size 24 ga
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 7 μm (PDMS), needle size 24 ga, for use with manual holder
Supelco
SPME fiber assembly polyacrylate (PA), df 85 μm (PA), for use with autosampler, needle size 24 ga
Supelco
SPME Sampling Stand, for use with 4 mL vials