IEC SYSTEM FOR CONFIRMITY TESTING
AND CERTIFICATION OF ELECTRICAL
EQUIPMENT
COMMITTEE OF TESTING LABORATORIES
TESTING AND MEASURING EQUIPMENT/ALLOWED SUBCONTRACTING
IEC 62321-5 ED. 1.0 (2013-06)
Part 5: Determination of certain substances in electrotechnical products: Cadmium,
lead and chromium in polymers and electronics and cadmium and lead in metals by
AAS, AFS, ICP-OES and ICP-MS
(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
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IEC 62321-5 ed 1.0 (2013-06)
IEC SYSTEM FOR CONFIRMITY TESTING
AND CERTIFICATION OF ELECTRICAL
EQUIPMENT
Clause
Measurement/testing
4
4.1
Reagents
General
4.2
Reagents
2014-05-16
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. The concentration of the analyte or interfering substances
in the reagents and water shall be negligible compared to the lowest
concentration to be determined.
All reagents for ICP-MS analysis, including acids or chemicals used shall
be of high-purity: trace metals shall be less than 1  10-6 % in total.
For measurements by ICP-OES and ICP-MS, the memory effect occurs in
cases where high concentrations of elements are introduced. Dilution of the
sample solution is required for high levels of each element. If the memory
effect is not decreased by dilution, thorough washing of the equipment is
required.
Water: Grade 1 specified in ISO 3696 used for preparation and dilution of
all sample solutions
Sulfuric acid:
 Sulfuric acid: ρ(H2SO4) = 1,84 g/mL, a mass fraction of 95 %,
“trace metal” grade
 Sulfuric acid: dilution (1:2): dilute 1 volume of concentrated sulfuric
acid with 2 volumes of water
Nitric acid:
 Nitric acid: ρ(HNO3) = 1,40 g/mL, a mass fraction of 65 %, “trace
metal” grade Nitric acid, a mass fraction of 10 %, “trace metal”
grade
 Nitric acid: 0.5 mol/L, “trace metal” grade
 Nitric acid: dilution (1:2): dilute 1 volume of concentrated nitric acid
65% with 2 volumes of water
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IEC 62321-5 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
Hydrochloric acid :
 Hydrochloric acid, ρ(HCl) = 1,19 g/mL, a mass fraction of 37 %,
“trace metal” grade
 Hydrochloric acid: dilution (1:2): dilute 1 volume of concentrated
hydrochloric acid 37% with 2 volumes of water
 Hydrochloric acid, a mass fraction of 5 %, “trace metal” grade
 Hydrochloric acid, a mass fraction of 10 %, “trace metal” grade
Hydrofluoric acid: ρ(HF) = 1,18 g/mL, a mass fraction of 40 %, “trace metal”
grade
Fluoroboric acid: HBF4, a mass fraction of 50 %, “trace metal” grade
Perchloric acid: ρ(HClO4) =1,67 g/mL, a mass fraction of 70 %, “trace
metal” grade
Phosphoric acid: ρ(H3PO4) =1,69 g/mL, more than a mass fraction of 85 %,
“trace metal” grade
Hydrobromic acid: ρ(HBr) = 1,48 g/mL, a mass fraction of 47 % to 49 %,
“trace metal” grade
Boric acid(H3BO3): 50 mg/mL, a mass fraction of 5 %, “trace metal” grade
Hydrogen peroxide: ρ(H2O2) = 1,10 g/mL, a mass fraction of 30 %, “trace
metal” grade
Mixed acid:
 Mixed acid 1, two parts hydrochloric acid 37%, one part nitric acid
65% and two parts water
 Mixed acid 2, one part nitric acid 65% and three parts hydrofluoric
acid 10%.
 Mixed acid 3, three parts hydrochloric acid 37% and one part nitric
acid 65%
Potassium hydroxide (KOH), “trace metal” grade
Potassium borohydride (KBH4), “trace metal” grade
Potassium ferricyanide (K3[Fe(CN)6]), “trace metal” grade
Oxido – reduction agent:
A mass fraction of 1,5 % KBH4 – a mass fraction of 1 % K3[Fe(CN)6] in a
mass fraction of 0,2 % KOH
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IEC 62321-5 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
Reducing agents:
 Reducing agent 1, a mass fraction of 1,3 % KBH4 in a mass
fraction of 0,2 % KOH
 Reducing agent 2, a mass fraction of 2,4 % KBH4 in a mass
fraction of 0,8 % KOH
Carrier:
 Carrier 1, a mass fraction of 1,5 % HCl.
 Carrier 2, a mass fraction of 1 % HCl
Thiourea ((NH2)2CS) solution, a mass fraction of 10 %
Masking agent:
 Masking agent 1, a mass fraction of 5 % oxalic acid – a mass
fraction of 5 % potassium sulfocyanate (KSCN) – a mass fraction
of 0,5 % o-phenanthroline (C12H8N2) solution:
 Masking agent 2, a mass fraction of Thiourea 10 % – ascorbic acid
a mass fraction of 10 % solution.
Cobalt solution, 50 mg/L
Stock solution:
 Stock solution with 1 000 mg/L of Pb.
 Stock solution with 1 000 mg/ L of Cd.
 Stock solution with 1 000 mg/L of Cr.
 Stock solution with 10 000 mg/L of Fe.
 Stock solution 10 000 mg/L of Cu.
Internal standard stock solution:
 Internal standard elements that do not interfere with the target
element are used for ICP-OES and ICP-MS. Also, the presence of
these internal standard elements in the sample solution shall be at
negligible levels. Sc, In, Tb, Lu, Re, Rh, Bi and Y may be used as
internal standard elements.
 For use with ICP-OES, Sc or Y is recommended. The
recommended concentration is 1 000 mg/L.
For use with ICP-MS, Rh is recommended. The recommended
concentration is 1 000 g/L.
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IEC 62321-5 ed 1.0 (2013-06)
IEC SYSTEM FOR CONFIRMITY TESTING
AND CERTIFICATION OF ELECTRICAL
EQUIPMENT
Clause
Measurement/testing
5
5.1
Apparatus
General
5.2
Apparatus
2014-05-16
COMMITTEE OF TESTING LABORATORIES
Testing / measuring equipment / material needed Subcontracting
In general, the collection and storage of glassware are a critical part of
trace analysis, regardless of the type of sample to be analysed. Because of
the sensitivity of the Pb, Cd and Cr analysis techniques described, each
individual sampling step shall be carried out with great care. All sampling,
storage and manipulation apparatus shall be metal-free. Soak all glassware
in 10 % nitric acid for 24 h at room temperature, and then rinse thoroughly
with water.
Analytical balance capable of measuring accurately to 0,000 1 g
HF-resistant sample introduction system: system in which the sample
insertion section and torch have been treated for resistance to HF
Argon gas: gas with purity of over 99,99 %
Acetylene gas: gas with purity of over 99,99 %.
Glassware, All glassware shall be cleaned with 10 % nitric acid before use:
 Kjeldahl flask: 100 mL
 Beakers: such as 100 mL, 200 mL, 500 mL etc.
 Volumetric flasks: such as 50 mL, 100 mL, 200 mL, 500 mL,
1000 mL, etc.
 Where appropriate, other types of volumetric equipment with
acceptable precision and accuracy can be used as an alternative to
volumetric flasks
 Pipettes: such as 1 mL, 5 mL, 10 mL, 20 mL, etc.
 Watch glass
Crucibles of platinum: such as 50 mL, 150 mL, etc
Crucibles of porcelain: such as 50 mL, 150 mL, etc
PTFE/PFA equipment (polytetrafluoroethylene (PTFE)/perfluoro alkoxy
alkane resin (PFA): all equipment shall be cleaned with 10 % nitric acid
before use:
 Beakers: such as 100 mL, 200 mL, 500 mL etc.;
 Covers for breakers;
 Volumetric flasks: such as 100 mL, 200 mL, 500 mL, etc.
Micropipettes: such as 10 l, 100 l, 200 l, 500 l, 1 000 l etc
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IEC 62321-5 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
Containers: For storage of standard solution and calibrant to be made of
high-density polyethylene (PE-HD) or PFA bottles
For determination at the ultra-trace level, containers made of perfluoro
alkoxy alkane resin (PFA) or perfluoro (ethylene-propylene) plastic (FEP)
shall be used. In either case, the user shall confirm the suitability of the
container selected
Electric hot plate or heated sand bath
Muffle furnace: capable of being maintained at 550 °C  25 °C
Bunsen burner or similar type of gas burner
Digestion with aqua regia: digestion apparatus equipped with a time and
temperature microcontroller unit, a heating block thermostat, a set of
vessels, each equipped with reflux coolers and absorption vessels
Microwave digestion system equipped with a sample holder and highpressure polytetrafluoroethylene/tetrafluoroethylene modified (PTFE/TFM)
or perfluoro alkoxy alkane resin/tetrafluoroethylene modified (PFA/TFM) or
other vessels based on fluorocarbon materials
Heat-resistant thermal insulation board
Glass microfibre filter (borosilicate glass), pore size 0,45 m and a suitable
filter cup
Alternative: Inductively coupled plasma optical atomic emission
spectrometer (ICP-OES).
Alternative: Inductively coupled plasma mass spectrometer (ICP-MS)
Alternative: Atomic absorption spectrometer (AAS)
Alternative: Atomic fluorescence spectrometer (AFS).
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.
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IEC 62321-5 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 0611
PET disks for Pb, Cd, Cr
Pb, Cd, Cr, blank, < 1 mg/kg
JSAC 0612
Pb 26.1, Cd 4.5, Cr 25.5
JSAC 0613
Pb 54.6, Cd 10.0, Cr 52.0
JSAC 0614
Pb 106.8, Cd 23.8, Cr 98.6
JSAC 0615
Pb 202.2, Cd 43.4, Cr 212.8
JSAC 0621
PET disks for Hg
Hg 10.0
JSAC 0623
Hg 49.0
JSAC 0624
Hg 121.1
JSAC 0625
Hg 244.4
2
Japan Society for
Analytical Chemistry
(JSAC)
Hg blank
JSAC 0622
1
Producer/
Distributor2
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.
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IEC 62321-5 ed 1.0 (2013-06)
IEC SYSTEM FOR CONFIRMITY TESTING
AND CERTIFICATION OF ELECTRICAL
EQUIPMENT
Certified
reference
materials
Certified values (Element mg/kg)1
Description
NMIJ 8102-a
ABS pellets for Pb, Cd, Cr
Pb 108.9, Cd 10.77, Cr 27.87
NMIJ 8103-a
ABS pellets for Pb, Cd, Cr
Pb 1084, Cd 106.9, Cr 269.5
NMIJ 8105-a
ABS disc for Pb, Cd, Cr
Pb 108.28, Cd 10.70, Cr 27.51
NMIJ 8106-a
ABS disc for Pb, Cd, Cr
Pb 1076.9, Cd 107.4, Cr 268.1
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
BAM-S004
Glass for Cr(VI), Cr
Cr(VI) 94, Cr 471
BAM-229
CuZn37 alloy chips for Pb
Pb 192
Cu granules for Cd, Cr, Pb
Cd 2.57, Cr 0.89, Pb 3.27
CRM 075C
1
2
COMMITTEE OF TESTING LABORATORIES
Producer/
Distributor2
National Metrology
Institute of Japan
(NMIJ)
European Reference
Materials (ERM)
Federal Institute for
Material Research and
Testing (BAM)
Community Bureau of
Reference – BCR
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.
2014-05-16
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IEC 62321-5 ed 1.0 (2013-06)
IEC SYSTEM FOR CONFIRMITY TESTING
AND CERTIFICATION OF ELECTRICAL
EQUIPMENT
Certified
reference
materials
VDA No 001
Certified values (Element mg/kg)1
Description
Plastic granules for Cd
Cd 40.9
VDA No 002
Cd 75.9
VDA No 003
Cd 197.9
VDA No 004
Cd 407
BCR-126A
Lead crystal glass plates for Pb
Pb 222610
NIST 1276a
CuNi alloy disk for Pb, Cd
Pb 40, Cd 2
NIST 1715
Al alloy disk for Pb, Cd
Pb 150.9, Cd 50.2
NIST 1727
Sn cube for Pb
Pb 33.26
NIST 1766
Steel disk for Cr, Pb
Cr 240, Pb 30
NIST 2166
Steel chips for Cr, Pb
Cr 240, Pb 30
NIST 364
Steel chips for Cr, Pb
Cr 600, Pb 230
NIST 855a
Al alloy powder for Cr, Pb
Cr 130, Pb 190
NIST 87a
SiAl alloy chips for Cr, Pb
Cr 1100, Pb 930
1
2
COMMITTEE OF TESTING LABORATORIES
Producer/
Distributor2
Institute for Reference
Materials and
Measurements (IRMM)
National Institute for
Standards and
Technology (NIST)
National Institute for
Standards and
Technology (NIST)
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.
2014-05-16
9(10)
IEC 62321-5 ed 1.0 (2013-06)
IEC SYSTEM FOR CONFIRMITY TESTING
AND CERTIFICATION OF ELECTRICAL
EQUIPMENT
Certified
reference
materials
COMMITTEE OF TESTING LABORATORIES
Certified values (Element mg/kg)1
Description
PVC-1
PVC Granulate for Pb
Pb 8, Cd <1
PVC-2
PVC Granulate for Pb, Cd
Pb 89, Cd 35
PVC-3
PVC Granulate for Pb, Cd
Pb 837, Cd 85
PVC-01A
PVC disc
Cd, Pb, Cr, Br, Hg blank (<1)
PVC-L-04A
PVC disc for Cd, Pb, Cr, Br, Hg
Cd 100, Pb 400, Cr 400, Br 500, Hg 200
PVC-H-03A
PVC disc for Cd, Pb, Cr, Br, Hg
Cd 300, Pb 1201, Cr 1001, Br 1101, Hg 1101
1
2
Producer/
Distributor2
Fluxana
http://www.fluxana.com
Analytical Reference
Materials International
(ARMI)
http://www.armi.com
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.
2014-05-16
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IEC 62321-5 ed 1.0 (2013-06)