IEC SYSTEM FOR CONFIRMITY TESTING
AND CERTIFICATION OF ELECTRICAL
EQUIPMENT
COMMITTEE OF TESTING LABORATORIES
TESTING AND MEASURING EQUIPMENT/ALLOWED SUBCONTRACTING
IEC 62321-4 ED. 1.0 (2013-06)
Part 4: Determination of certain substances in electrotechnical products: Mercury in
polymers, metals and electronics by CV-AAS, CV-AFS, ICP-OES and ICP-MS
PROVISIONAL
(to be approved at the 51st CTL Plenary meeting 2014)
R = Required to be at Lab
S = May be subcontracted
W = May be witnessed at MTL
SF = Specialized Facility
3PPS = Three Phase Power Supply required
2013-07-09
1(7)
IEC 62321-4 ed 1.0 (2013-06)
IEC SYSTEM FOR CONFIRMITY TESTING
AND CERTIFICATION OF ELECTRICAL
EQUIPMENT
Clause
Measurement/testing
4
4.1
Reagent and materials
General
4.2
Reagents
2013-07-09
COMMITTEE OF TESTING LABORATORIES
Testing / measuring equipment / material needed Subcontracting
For the determination of elements at trace level, the reagents shall be of
adequate purity. Contamination can be a major source of error when
working in the 1 ng range with the instruments. Cautious handling of the
apparatus and careful technique will minimize this problem. Therefore, only
grade 1 water shall be used. Care shall be taken that all materials in
contact with the water are Hg-free.
Chemicals used for sample preparation can be a major source of
contamination. Only reagents that are mercury-free shall be used. It is
therefore highly recommended that the blank values of the reducing agents
and the other chemicals be measured before using them for sample
preparation.
Water: Grade 1, as defined in ISO 3696, shall be used for preparation and
dilution of all sample solutions
Nitric acid (concentrated nitric acid): ρ(HNO3) = 1,4 g/mL, a mass fraction
of 65 %, trace metal grade
Nitric acid, a mass fraction of 50 %, trace metal grade
Nitric acid, 0.5 mol/L, trace metal grade
Nitric acid, a mass fraction of 1 %, trace metal grade
Nitric acid, a mass fraction of 1,5 %, trace metal grade
Nitric acid, a mass fraction of 5 % , trace metal grade
Fluoroboric acid: HBF4, a mass fraction of 50 %, trace metal grade (for
microwave digestion)
Hydrogen peroxide: H2O2, a mass fraction of 30 %, trace metal grade (for
microwave digestion)
Stock solution with 1 000 mg/L of mercury, trace metal grade
Potassium tetrahydridoborate (potassium borohyride): KBH4, trace metal
grade
Potassium permanganate: KMnO4, a mass fraction of 5 % solution, trace
metal grade
Sodium tetrahydridoborate (sodium borohydride), NaBH4, trace metal grade
Sodium hydroxide, NaOH (trace metal grade)
2(7)
S
IEC 62321-4 ed 1.0 (2013-06)
IEC SYSTEM FOR CONFIRMITY TESTING
AND CERTIFICATION OF ELECTRICAL
EQUIPMENT
Clause
Measurement/testing
4.3
Materials
5
5.1
Apparatus
General
5.2
Apparatus
2013-07-09
COMMITTEE OF TESTING LABORATORIES
Testing / measuring equipment / material needed Subcontracting
Hydrogen tetrachloroaurate (Ⅲ) tetra hydrate, HAuCl4 ･ 4H2O (trace metal
grade).
Internal standard stock solution, trace metal grade (Sc or Y for ICP-OES or
Rh for ICP-MS)
Reducing agent for CV-AAS: a mass fraction of 3 % NaBH4 in 1 % a mass
fraction of NaOH
Reducing agent for CV-AFS: a mass fraction of 1 % (m/v) KBH4 in a mass
fraction of 0, 05 % NaOH
Gold preservation stock solution for mercury (1 mL = 100 µg): it is
recommended purchasing as high purity prepared solution of AuCl3 in dilute
hydrochloric acid matrix
Diatomaceous earth
Alternative for thermal–decomposition-gold amalgamation system:
Mercury collector
In general, the collection and storage of glassware are a critical part of
mercury analysis, regardless of the type of sample to be analysed. Because
of the sensitivity of the mercury analysis techniques described, each
individual sampling step shall be carried out with great care.
Beakers, pipettes, volumetric flasks, etc. are all major sources of metal
contamination. It is essential to use mercury-free plastic or quartz
glassware for sample handling.
All sampling, storage and manipulation apparatus shall be mercury free.
Soak all glassware in 50 % nitric acid for 24 h at room temperature, and
then rinse thoroughly with water.
For measurements by ICP-OES and ICP-MS, the memory effect occurs in
cases where high concentrations of mercury are introduced. Dilution of the
sample solution is required for high levels of mercury. If the memory effect
is not decreased by dilution, thorough washing of the equipment is required.
Analytical balance capable of measuring accurately to 0,000 1 g
3(7)
S
S
IEC 62321-4 ed 1.0 (2013-06)
IEC SYSTEM FOR CONFIRMITY TESTING
AND CERTIFICATION OF ELECTRICAL
EQUIPMENT
Clause
Measurement/testing
COMMITTEE OF TESTING LABORATORIES
Testing / measuring equipment / material needed Subcontracting
Alternative for wet diggestions:
 Heating digester equipped with reaction vessels, reflux coolers and
absorption vessels (for the digestion of metals and electronics)
 Glass fibre filter 0, 45 µm
Alternative for microwave digestions:
Microwave sample preparation system equipped with a sample holder and
high-pressure polytetrafluoroethylene/tetrafluoroethylene modified
(PTFE/TFM) or perfluoro alkoxyl alkane resin /tetrafluoroethylene modified
(PFA/TFM) or other vessels based on fluorocarbon materials (for the
digestion of metals containing significant amounts of silicon (Si), zirconium
(Zr), hafnium (Hf), titanium (Ti), tantalum (Ta), niobium (Nb) or tungsten
(W), and for plastics)
 Glass microfibre filter (borosilicate glass), pore size: 0, 45 m and
a suitable filter cup
 Volumetric flasks such as 25 mL, 250 mL, etc. (PTFE-PFA
equipment or glassware). Where appropriate, other types of
volumetric equipment with acceptable precision and accuracy can
be used as alternatives to volumetric flasks
 Pipettes such as 1 mL, 2 mL, 5 mL, 10 mL, etc. (PTFE-PFA
equipment or glassware)
 Micropipettes such as 200 L, 500 Ll, 1, 000 L, etc
 Plastic containers for standards and digestion solutions. (PTFEPFA equipment)
 Cold vapour atomic absorption spectrometer (CV-AAS)
 Cold vapour atomic fluorescence spectrometer (CV-AFS)
 Inductively coupled plasma optical emission spectrometer (ICPOES)
 Inductively coupled plasma mass spectrometer (ICP-MS).
 Argon gas with a purity of at least 99, 99 %.
 Thermal decomposition-gold amalgamation system
2013-07-09
4(7)
S
IEC 62321-4 ed 1.0 (2013-06)
IEC SYSTEM FOR CONFIRMITY TESTING
AND CERTIFICATION OF ELECTRICAL
EQUIPMENT
Clause
Measurement/testing
COMMITTEE OF TESTING LABORATORIES
Testing / measuring equipment / material needed Subcontracting
Alternative: Cold Vapour - Atomic Absorption Spectrometer (CV-AAS):
equipment consisting of sample holder, (reaction cell, gas-liquid separator
and/or thermal decomposition-gold amalgamation system), optical unit,
detector, system control and data output device.
Alternative: Cold Vapour - Atomic Fluorescence Spectrometer (CV-AFS):
equipment consisting of sample holder, (reaction cell, gas-liquid separator
and
and
and/or thermal decomposition-gold amalgamation system), optical unit,
1
Clause 7
Determination of mercury in polymers, metals detector, system control and data output device.
adopted from
and electronics by alternative methods CV- Alternative: Inductively Coupled Plasma – Optical/Atomic Emission
Spectrometer (ICP-OES, ICP-AES): equipment consisting of sample
IEC 62321 Ed.
AAS, CV-AFS, ICP-OES or ICP-MS
holder, plasma torch, spray chamber, nebuliser, optical unit, detector,
1 (2008)
system control and data output device.
Alternative: Inductively Coupled Plasma - Mass Spectrometer: (ICP-MS):
equipment consisting of sample holder, ioniser, interface, ion lens, mass
separator, detector, evacuated vessel, system control and data output
device.
Annex A
Practical application of determination of
mercury in polymers,
metals and electronics by CV-AAS, AFS, ICPOES and ICP-MS
S
Note: The presence of equipment alone does not indicate a satisfactory situation. Assessors must evaluate the
equipment design, calibration, uncertainty and documentation to ensure compliance with the directions of the
standard. The requirements of ISO IEC 17025 regarding validation are applicable, as the tests of this standard
are not standardized tests.
1
IEC 62321 Ed. 1.0 (2008) Clause 7 was adopted since general analyzer details are not described in IEC 62321-4 Ed. 1.0 (2013-6). IEC 62321 Ed. 1.0 (2008) Clause 7 shall be used in conjunction with IEC
62321-4 Ed. 1.0 (2013-6) Annex A.
2013-07-09
5(7)
IEC 62321-4 ed 1.0 (2013-06)
IEC SYSTEM FOR CONFIRMITY TESTING
AND CERTIFICATION OF ELECTRICAL
EQUIPMENT
COMMITTEE OF TESTING LABORATORIES
Appendix I
Suggested certified reference materials for method validation and QA/QC purposes:
Certified
reference
materials
Certified values (Element mg/kg)1
Description
JSAC 0601-2
PET pellets for Pb, Cd, Hg, Cr (50 g)
Pb 11.6, Cd 5.2, Cr, 10.8, Hg 1.3
JSAC 0602-2
PET pellets for Pb, Cd, Hg, Cr (50 g)
Pb 109.3, Cd 51.7, Cr, 108.8, Hg 12.4
JSAC 0621
PET disks for Hg
Hg blank
JSAC 0622
Hg 10.0
JSAC 0623
Hg 49.0
JSAC 0624
Hg 121.1
JSAC 0625
Hg 244.4
NMIJ 8112-a
ABS pellets for Pb, Cd, Hg, Cr
Pb 94.98, Cd 9.383, Hg 94.10, Cr 94.47
NMIJ 8113-a
ABS pellets for Pb, Cd, Hg, Cr
Pb 945, Cd 93.93, Hg 941.5, Cr 943.6
NMIJ 8115-a
ABS discs for Pb, Cd, Hg, Cr
Pb 94.21, Cd 9.341, Hg 93.81, Cr 94.27
NMIJ 8116-a
ABS discs for Pb, Cd, Hg, Cr
Pb 940.6, Cd 93.67, Hg 938.7, Cr 943.7
ERM-EC680k
PET pellets for Pb, Cd, Hg, Cr, Br
Pb 13.6, Cd 19.6, Hg 4.64, Cr 20.2, Br 96
ERM-EC681k
PET pellets for Pb, Cd, Hg, Cr, Br
Pb 98, Cd 137, Hg 23.7, Cr 100, Br 770
1
2
Producer/
Distributor2
Japan Society for
Analytical Chemistry
(JSAC)
National Metrology
Institute of Japan
(NMIJ)
European Reference
Materials (ERM)
Values as given in table are for information only. Certified values as provided with the corresponding material data sheet by CRM producer/distributor are binding.
There is no preference for any CRM distributor. CRMs may be purchased from locally available source.
2013-07-09
6(7)
IEC 62321-4 ed 1.0 (2013-06)
IEC SYSTEM FOR CONFIRMITY TESTING
AND CERTIFICATION OF ELECTRICAL
EQUIPMENT
2013-07-09
7(7)
COMMITTEE OF TESTING LABORATORIES
IEC 62321-4 ed 1.0 (2013-06)