| Titre : |
Improved method for accurate and efficient analysis of chlorophenols in leather compared with conventional steam distillation operation specified by ISO 17070-2015 |
| Type de document : |
texte imprimé |
| Auteurs : |
Ze-Sheng Wang, Auteur ; He-Wei Ma, Auteur |
| Année de publication : |
2022 |
| Article en page(s) : |
p. 344-353 |
| Note générale : |
Bibliogr. |
| Langues : |
Américain (ame) |
| Catégories : |
Chlorophénols Un chlorophénol est un composé aromatique constitué d'un cycle benzénique substitué par un groupe hydroxyle (phénol) et par un ou plusieurs atomes de chlore (chlorobenzène).
Les chlorophénols sont produits par halogénation électrophile aromatique du phénol par le dichlore. Le groupe hydroxyle étant orienteur ortho-para (effet -I/+M), on obtient préférentiellement un mélange de 2-chlorophénol et de 4-chlorophénol, puis le 2,4-dichlorophénol et enfin le 2,4,6-trichlorophénol. La tétra- et pentachloration nécessitent la présence d'un catalyseur (AlCl3).
La plupart des chlorophénols sont solides à température ambiante ; ils ont un très fort goût et odeur "médical". Les chlorophénols sont couramment utilisés comme pesticides, herbicides et désinfectants.
Chromatographie en phase gazeuse
Cuirs et peaux -- Analyse
Cuirs et peaux -- Normes
Distillation
Extraction (chimie)
Normalisation
Spectrométrie de masse
|
| Index. décimale : |
675 Technologie du cuir et de la fourrure |
| Résumé : |
An improved analytical method was built based on the conventional standard method ISO 17070-2015 for the determination of 19 chlorophenols in leather. This developed method involved ultrasonic assisted extraction using methanol containing formic acid, derivatization using acetic anhydride, solid-phase extraction (SPE) cleanup with silica-gel cartridge. Final analysis of the chlorophenols compounds was performed by Gas Chromatography - Mass Spectrometry (GC-MS). Optimum conditions for sample extraction, such as time, temperature and formic acid content in methanol were studied. Satisfactory recoveries in the range of 92-105% (RSD, 2.1-7.3%) for the targets were obtained, and detection limits were in the range of 0.09-0.15 mg/kg. The developed procedure was evaluated and compared with ISO 17070-2015 which uses steam distillation for sample extraction. The method was successfully applied to determine 19 chlorophenols in series of leather samples from different origin. This study demonstrated that the ultrasonic assisted extraction, followed by acetyl derivatization and silica-gel cleanup coupled with GC-MS, can be used as an alternative to ISO 17070-2015, for detecting chlorophenols in leather. |
| Note de contenu : |
- EXPERIMENTAL : Reagents - Apparatus - Sample preparation - Sample preparation - Derivatization - Cleanup - Sample test according to ISO 17070-2015 - GC-MS analysis
- RESULTS AND DISCUSSION : Analysis of CPs with GC-MS - Optimization of extraction process - Effects of methanol on derivatization - Cleanup with silica-gel cartridge - Method validation - Linearity - Reproducibility - Limits of detection (LOD) - Comparison with ISO 17070-2015 - Analysis of real samples
- Table 1 : Target CPs with their CAS N°., pKa, retention time and detection ions
- Table 2 : Optimized parameters of the extraction conditions
- Table 3 : Analytical parameters for this investigated procedure and ISO 17050-2015 (GC-MS)
- Table 4 : Comparison of the investigated method with ISO 17070-2015
- Table 5 : Levels of the CPs found in leather samples |
| DOI : |
https://doi.org/10.34314/jalca.v117i8.5985 |
| En ligne : |
https://drive.google.com/file/d/1bLjaH7U0qsqCxfIu2zrh4YGDW77Ui_PM/view?usp=drive [...] |
| Format de la ressource électronique : |
Pdf |
| Permalink : |
https://e-campus.itech.fr/pmb/opac_css/index.php?lvl=notice_display&id=37827 |
in JOURNAL OF THE AMERICAN LEATHER CHEMISTS ASSOCIATION (JALCA) > Vol. CXVII, N° 8 (08/2022) . - p. 344-353
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Improved method for accurate and efficient analysis of chlorophenols in leather compared with conventional steam distillation operation specified by ISO 17070-2015 in JOURNAL OF THE AMERICAN LEATHER CHEMISTS ASSOCIATION (JALCA), Vol. CXVII, N° 8 (08/2022)
