IEC 62321-10-2020 Determination of certain substances in electrotechnical products – Part 10: Polycyclic aromatic hydrocarbons (PAHs) in polymers and electronics by gas chromatography-mass spectrometry (GC-MS).
6 Apparatus
The following items shall be used for the analysis:
a) 0,45 μm PTFE filter membrane.
b) 1 ml, 5 ml, 1 0 ml, 1 00 ml volumetric flasks.
c) Aluminium foil.
d) Analytical balance capable of measuring accurately to 0,000 1 g.
e) 40 ml brown or amber vessel.
f) Cryogenic grinding with liquid N 2 cooling.
g) Dry oven.
h) Furnace.
i) Extraction thimble (cellulose 30 ml, ID 22 mm, height 80 mm).
j) Funnel.
k) Glass column (size: 220 mm × 1 5 mm).
l) Glass wool (for extraction thimble).
m) Heating jackets.
n) Microlitre syringe or automatic pipettes.
o) Mini-shaker (also known as vortexer or vortex mixer).
p) Pasteur pipette.
q) Rotary evaporator.
r) Soxhlet extractors:
– 30 ml Soxhlet extractors,
– 250 ml round-bottomed flasks,
– ground-in stopper NS 29/32,
– Dimroth condenser NS 29/32,
– boiling stones (e.g. glass pearls or Raschig rings).
s) Ultrasonic extractors:
Ultrasonic bath with a minimum power of 200 W and a bath area of 706 cm 2 , corresponding to 0,28 W/cm 2 , without a basket and with an internal or external thermostat.
t) Vial for GC-MS: 2 ml sample vials with 1 00 μl glass insert and a screw cap with polytetrafluoroethylene (PTFE) gasket or depending on the analytical system, a comparable sample receptacle. Brown or amber vessels shall be used as indicated in the text of the procedure.
u) GC-MS: A gas chromatograph with a capillary column coupled to a mass spectrometric detector (electron ionization, EI) is used for the analysis. The mass spectrometric detector shall be able to perform selective ion monitoring and have an upper mass range of at least 550 m/z. The use of an autosampler is strongly recommended to ensure repeatability. Ferrules used shall not contain more than 40 % graphite (a suitable ferrule is made of 60 % polyimide and 40 % graphite) to decrease the risk that PAHs are absorbed.
v) GC column for PAH analysis: A column length of 20 m or longer has sufficient separation efficiency for PAH compounds. An example of suitable column and its separation results is given in Annex A, see Table A.2, Table A.3 and Figure A.1 . For the capillary column, 5 % phenyl, 95 % methyl polysiloxane (e.g. such as HT8, DB-EUPAH and ZB-PAH) is recommended. The preferred dimensions are 20 m in length, 0,25 mm or 0,1 8 mm in internal diameter, and 0,25 μm or 0,1 4 μm in film thickness. NOTE Based on the AfPS-GS-201 4-01 -PAK method, a nonpolar DB-5MS column is not suited for a separation of the different benzofluoranthenes listed in Table 1 .
7 Sampling As described in IEC 62321 -2, unless indicated otherwise (e.g. “using a knife”), cryogenic grinding with liquid nitrogen cooling is recommended and the samples shall be ground to pass through a 500 μm sieve before extraction. If samples are not tested immediately, they shall be stored in tightly sealed glass vessels and in a cool and dark place. It shall be confirmed that glassware is thoroughly cleaned and that all new materials that may come into contact with the sample are checked by blank analysis that they give no interference. NOTE Interferences which can affect the results can occur due to contaminations from glassware, solvents and other materials that can come into contact with the sample. Such interferences will form an artifact or will increase the detector baseline. Interferences can also come from components in samples that co-elute with the specific PAHs of interest. 8 Procedure 8.1 General instructions for the analysis The following general instructions shall be followed: The validation of the instrumentation shall include testing of potential cross contaminations between sequential samples. Additional blanks or an inverted sequence of testing will help to identify cross contaminations. See Annex C for guidance regarding labware cleaning procedures for PAH testing. To avoid decomposition of PAHs by UV light during extraction and analysis, glass equipment made from brown or amber glass shall be used.IEC 62321-10 pdf download.