ISO 787-28:2019
General methods of tests for pigments and extenders — Part 28: Determination of total content of polychlorinated biphenyls (PCB) by dissolution, cleanup and GC-MS
General methods of tests for pigments and extenders — Part 28: Determination of total content of polychlorinated biphenyls (PCB) by dissolution, cleanup and GC-MS
- Статус документа:
- Действующий
- Формат:
- Электронный (PDF)
- Количество страниц:
- 21
- Дата публикации:
- 10 мая 2019 г.
- Издание:
- ISO IS 787 edition 1 version 1
- ICS:
- 87.060.10
This document specifies a method for determining the total content of polychlorinated biphenyls (PCBs), checking for all 209 possible congeners in pigment materials. This document is applicable to a working range from1 mg/kg to 150 mg/kg. The lower quantitation limit of this method is 1 mg/kg per congener. Results below 1 mg/kg are considered to be qualitative only.
Abstract
Overview
ISO 787-28:2019 specifies a laboratory method for the determination of total polychlorinated biphenyls (PCBs) in pigment materials. The procedure targets all 209 PCB congeners, using a dissolution approach followed by cleanup and analysis by gas chromatography–mass spectrometry (GC‑MS). The method is designed for a working range of 1 mg/kg to 150 mg/kg; the lower limit of quantitation (LOQ) is 1 mg/kg per congener (results below 1 mg/kg are qualitative).
Key topics and technical requirements
- Scope: Total PCB content in pigments/ extenders, addressing occluded PCBs not accessible to surface-only extractions.
- Sampling: Representative, dry powder samples with volatiles <1% (per ISO 15528). Store in dark, capped glass containers.
- Sample preparation:
- Add 13C12‑labelled internal reference materials directly to the freshly weighed sample (no later additions).
- Dissolve sample in concentrated sulfuric acid (92–95% m/m) with sonication until homogenous; keep temperature below 50 °C.
- Optional leaching pre-step can be used for low‑chlorinated congeners.
- Cleanup:
- Sequential wet column chromatography to remove interfering species (aryl sulfuric acids, polymers, heterocycles).
- Multilayer columns are obligatory; optional steps include diatomaceous earth–sulfuric acid columns, gel permeation (size exclusion), and alumina columns.
- Separation and detection:
- Final analysis by GC‑MS, preferably using SIM mode for quantitation; a 60 m column is recommended for congener separation (30 m allowed for screening).
- Quantitation by peak area ratios of analytes to corresponding internal standards; identification uses multiple specific ion traces.
- Safety: Use analytical‑grade reagents, trained personnel, and follow PCB handling rules. UV (254 nm) is noted for spill‑decomposition procedures.
Practical applications and users
- Pigment and dye manufacturers: quality control and supplier screening to verify PCB contamination levels.
- Independent testing laboratories: routine and compliance testing for pigments and extenders used in paints, inks and coatings.
- Regulatory bodies and customs laboratories: enforcement of chemical safety limits and import/export controls.
- Paint, varnish and raw‑materials manufacturers: incoming material verification to prevent PCB introduction into formulations.
Advantages: the dissolution approach avoids underestimating total PCB content caused by occlusion within pigment crystal lattices-common shortcomings in environmental or surface‑only extraction methods.
Related standards
- ISO 15528 - Paints, varnishes and raw materials for paints and varnishes - Sampling.
- ISO 18451-1 - Pigments, dyestuffs and extenders - Terminology (general terms).
- Part of the ISO 787 series (general test methods for pigments and extenders).
Keywords: ISO 787-28:2019, PCBs in pigments, polychlorinated biphenyls, PCB congeners, GC‑MS analysis, sulfuric acid dissolution, multilayer cleanup, 13C12 internal standard, limit of quantitation.
Технические детали
- Технический комитет
- ISO/TC 256 - Pigments, dyestuffs and extenders
- SKU
- ISO 787-28:2019
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