IEC 62321-10:2020 pdf free download – Determination of certain substances in electrotechnical products
1 Scope
This part of lEC 62321 specifies one normative technique for the determination of polycyclicaromatic hydrocarbons (PAHs) in polymers of electrotechnical products. These PAHs canespecially be found in the plastic and rubber parts of a wide range of consumer articles. Theyare present as impurities in some of the raw materials used in the production of such articles,in particular in extender oils and in carbon black.They are not added intentionally to the articlesand do not perform any specific function as constituents of the plastic or rubber parts.
The gas chromatography-mass spectrometry (GC-MS) test method is suitable for thedetermination of polycyclic aromatic hydrocarbons (PAHs).
These test methods have been evaluated for use with plastics and rubbers.These test methodshave been evaluated for use with ABs (acrylonitrile butadiene styrene) containing individualPAHs ranging from 37,2 mg/kg to 119 mg/kg and rubbers containing individual PAHs rangingfrom 1 mg/kg to 221,2 mg/kg.
WARNING – This document does not purport to address all of the safety concerns, if any,associated with its use. It is the responsibility of the user of this document to establishappropriate safety and health practices and determine the applicability of regulatory limitationsprior to use.
This horizontal standard is primarily intended for use by technical committees in the preparationof standards in accordance with the principles laid down in lEC Guide 108.
One of the responsibilities of a technical committee is,wherever applicable, to make use ofhorizontal standards in the preparation of its publications. The contents of this horizontalstandard will not apply unless specifically referred to or included in the relevant publications.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their contentconstitutes requirements of this document.For dated references, only the edition cited applies.For undated references,the latest edition of the referenced document (including anyamendments) applies.
IEC 62321-1;2013,Determination of certain substances in electrotechnical products – Part 1:lntroduction and overview
IEC 62321-2,Determination of certain substances in electrotechnical products – Part 2:Disassembly, disjointment and mechanical sample preparation
ISO 3696,Water for analytical laboratory use – Specification and test methods
8.2.1Ultrasonic extraction
The following steps shall be followed for sample extraction:
The samples shall be pre-cut less than 5 mm x 5 mm andor milled by cryogenic grinding withliquid N2 cooling or cut sample materials to 2 mm to 3 mm. Quantitatively transfer500 mg ± 10 mg of the sample into the vessel (Clause 6 e)).
a) Weigh 500 mg ± 10 mg of the sample into a 40 ml amber vessel(Clause 6 e)).Record themass to the nearest 0,1 mg.
b) Add 20 ul of the surrogate standard (Clause 5 f)) (100 ug/ml) into the 40 ml amber vessel.
c) Transfer 20 ml of toluene(Clause 5 d)) and 20 ul of internal standard(8.4.4 c)) (100 ug/ml) to the 40 ml amber vessels (Clause 6 e)).
d) Place it in an ultrasonic extractor(Clause 6 s)) and sonicate it for about 1 h at 60 “C and then allow to cool at room temperature after the extraction of the sample.
e) Allow the polymer to settle or filter the mixture through a 0,45 um PTFE membrane.8.2.2Soxhlet extraction
For the Soxhlet extraction step the following procedure is applied:
a) Quantitatively transfer 500 mg : 10 mg of the sample into a cellulose extraction thimble for Soxhlet extraction.Record the mass to the nearest 0,1 mg.
b)Allow the sample to be transferred through a funnel into the extraction thimble.To ensure a quantitative transfer, the funnel should be rinsed with approximately 10 ml of toluene.
c) 10 ul of the surrogate standard (8.4.5 d)) (50 ug/ml) is added.
d) Cover the thimble with glass wool to prevent the sample from floating.
e)Approximately 120 ml of toluene is used for extraction under reflux.Allow the sample to be extracted for at least 6 h with 6 to 8 cycles per hour.Shorter extraction times may result inlower recoveries of the analyses.
f) After six hours of reflux,the extract is concentrated to about 2 ml using a vacuum rotary evaporator.10 ul of the internal standard(8.4.4 d))(50 ug/ml) is then added and the extractis diluted with toluene to 5 ml.
g) The diluted sample is transferred into a 2 ml GC samplelauto sample vial with a PTFE coated seal.