Electrotechnical products - Determination of restricted substances - Sampling procedure - Guidelines

IEC/PAS 62596:2009(E) is a Publicly Available Specification which provides general sampling guidelines and strategies of sampling for electrotechnical products, electronic assemblies, electronic components. In order to obtain samples that can be used for analytical testing to determine the levels of restricted substances as described in the test methods of IEC 62321. Restrictions for substances will vary between geographic regions and from time to time. This document describes a generic process for the sampling of any substance which could be restricted.

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Publication Date
21-Jan-2009
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WPUB - Publication withdrawn
Completion Date
07-Mar-2014
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IEC/PAS 62596
Edition 1.0 2009-01
PUBLICLY AVAILABLE
SPECIFICATION
PRE-STANDARD

Electrotechnical products – Determination of restricted substances – Sampling
procedure – Guidelines



IEC/PAS 62596:2009(E)

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THIS PUBLICATION IS COPYRIGHT PROTECTED
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IEC/PAS 62596
Edition 1.0 2009-01
PUBLICLY AVAILABLE
SPECIFICATION
PRE-STANDARD

Electrotechnical products – Determination of restricted substances – Sampling
procedure – Guidelines


INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
PRICE CODE
XA
ICS 13.020, 43.040.10 ISBN 978-2-88910-813-8
® Registered trademark of the International Electrotechnical Commission

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– 2 – PAS 62596 © IEC:2009(E)
CONTENTS

FOREWORD.4
INTRODUCTION.5
1 Scope.6
2 Normative references .6
3 Terms, definitions and abbreviations .6
3.1 Terms and definitions .6
3.2 Abbreviations .8
4 Introduction to sampling .9
4.1 Introductory remark .9
4.2 Requirements and concerns for restricted substances .9
4.3 Complexity of electrotechnical products and related challenges .10
4.4 Strategies for sampling.11
5 Sampling .13
5.1 Introductory remark .13
5.2 Partial disassembly .13
5.2.1 Example 1: Cell phone type A – Disassembly without tools.14
5.2.2 Example 2: Cell phone type B – Partial disassembly.15
5.3 Complete disassembly.16
5.4 Partial disjointment.18
5.4.1 Introductory remark .18
5.5 Complete disjointment .20
5.5.1 Introductory remark .20
5.5.2 Typical examples of disjointment at the component level .20
5.5.3 Examples of disjointment at the base materials level – Disjointment
of integrated circuit (IC) chips.22
5.6 Considerations of sampling and disjointment .25
5.6.1 Introductory remark .25
5.6.2 Sample size required.25
5.6.3 Sample size v. detection limit .26
5.6.4 Composite testing of disjointable samples .27
5.6.5 Non-uniform “homogeneous materials” .28
5.6.6 Determination of sampling position of homogeneous materials .29
6 Conclusions and recommendations .29
Annex A (informative) Examples of procedures for sampling and disjointment .30
Annex B (informative) Probability of presence of restricted substances.40
Annex C (informative) Composite testing and sampling.42
Annex D (informative) Tools used in sampling .44
Annex E (informative) Use of XRF screening techniques in sampling.45
Bibliography.54

Figure 1 – Generic iterative procedure for sampling .11
Figure 2 – Cell phone with battery charger and camera lens cap.14
Figure 3 – Cell Phone with battery and back cover removed .15
Figure 4 – Partial disassembly of a cell phone (type B) into its major components .16

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PAS 62596 © IEC:2009(E) – 3 –
Figure 5 – Complete disassembly of the key pad .17
Figure 6 – Complete disassembly of the bottom housing.17
Figure 7 – Complete disassembly of the other housing/frame .18
Figure 8 – Components of the TFT display of the cell phone after partial disjointment.19
Figure 9 – Components of the main PWB of the cell phone after partial disjointment .19
Figure 10 – Disjointment of lead frame component.22
Figure 11 – BGA package prior to disjointment .23
Figure 12 – BGA package disjointed by the hand removal procedure .23
Figure 13 – Solder ball material collected from BGA using a hand removal procedure .24
Figure 14 – BGA solder ball removal using the ball shear procedure.24
Figure 15 – Cross-section of a 900 µm wide lead oxide-based resistor (SMD) .28
Figure A.1 – Example of methodology for sampling and disjointment .31
Figure A.2 – Methodology for sampling and disjointment.32
Figure A.3 – Sampling of DVD player.33
Figure A.4 – Sampling of CRT .34
Figure A.5 – Sampling of LCD TV .35
Figure A.6 – Sampling of PDA/phone.36
Figure A.7 – Sampling of desk fan .37
Figure A.8 – Compoments – Example 1 – thick film resistor .38
Figure D.1 – Hot gas gun for removing the electronic components .44
Figure D.2 – Vacuum pin to remove the target electronic devices .44
Figure E.1 – AC power cord, X-ray spectra of sampled sections .47
Figure E.2 – RS232 cable and its X-ray spectra .48
Figure E.3 – Cell phone charger shown partially disassembled. .48
Figure E.4 – PWB and cable of cell phone charger .49
Figure E.5 – Spots from 1,27 mm and 0,3 mm collimaters.50
Figure E.6 – Examples of substance mapping on PWBs .52
Figure E.7 – SEM-EDX image of Pb free solder with small intrusions of Pb

(size = 30 μm).53

Table 1 – Possible restricted or screening substances from a cell phone .15
Table 2 – Possible restricted substances in major components of the cell phone .16
Table 3 – Examples of disjointment for typical small electronic components .21
Table 4 – Minimum number of lead frame samples required for analytical testing .26
Table 5 – Levels of a restricted substance in a composite sample .27
Table B.1 – Probability of presence of restricted substances in materials and
components used in electrotechnical products .40
Table C.1 – Calculated maximum concentration for a composite sample based on

detection limit .43
Table C.2 – Required detection limit for a composite sample based on the maximum
allowable concentration .43
Table E.1 – Selection of samples for analysis of AC power cord .46
Table E.2 – Selection of samples (testing locations) for analysis after visual
inspection – Cell phone charger.49
Table E.3 – Results of XRF analysis at spots 1 and 2 as shown in Figure E.6.52

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INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________

ELECTROTECHNICAL PRODUCTS –
DETERMINATION OF RESTRICTED SUBSTANCES –
SAMPLING PROCEDURE – GUIDELINES

FOREWORD
1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising
all national electrotechnical committees (IEC National Committees). The object of IEC is to promote
international co-operation on all questions concerning standardization in the electrical and electronic fields. To
this end and in addition to other activities, IEC publishes International Standards, Technical Specifications,
Technical Reports, Publicly Available Specifications (PAS) and Guides (hereafter referred to as “IEC
Publication(s)”). Their preparation is entrusted to technical committees; any IEC National Committee interested
in the subject dealt with may participate in this preparatory work. International, governmental and non-
governmental organizations liaising with the IEC also participate in this preparation. IEC collaborates closely
with the International Organization for Standardization (ISO) in accordance with conditions determined by
agreement between the two organizations.
2) The formal decisions or agreements of IEC on technical matters express, as nearly as possible, an international
consensus of opinion on the relevant subjects since each technical committee has representation from all
interested IEC National Committees.
3) IEC Publications have the form of recommendations for international use and are accepted by IEC National
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between any IEC Publication and the corresponding national or regional publication shall be clearly indicated in
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equipment declared to be in conformity with an IEC Publication.
6) All users should ensure that they have the latest edition of this publication.
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8) Attention is drawn to the Normative references cited in this publication. Use of the referenced publications is
indispensable for the correct application of this publication.
9) Attention is drawn to the possibility that some of the elements of this IEC Publication may be the subject of
patent rights. IEC shall not be held responsible for identifying any or all such patent rights.
A Publicly Available Specification (PAS) is a technical specification not fulfilling the
requirements for a standard, but made available to the public.
IEC-PAS 62596 has been processed by IEC technical committee 111: Environmental
standardization for electrotechnical products and systems.
The text of this PAS is based on the This PAS was approved for
following document: publication by the P-members of the
committee concerned as indicated in
the following document
Draft PAS Report on voting
111/112/PAS 111/126/RVD

Following publication of this PAS, which is a pre-standard publication, the technical committee
or subcommittee concerned may transform it into an International Standard.
This PAS shall remain valid for an initial maximum period of 3 years starting from the
publication date. The validity may be extended for a single 3-year period, following which it
shall be revised to become another type of normative document, or shall be withdrawn.

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PAS 62596 © IEC:2009(E) – 5 –
INTRODUCTION
In the electrotechnical industry, much emphasis has been placed on minimizing the
environmental burden of its products. Waste handling, recycling, chemicals and energy
consumption are covered by regulations. Specifically, the use of materials containing lead
(Pb), mercury (Hg), cadmium (Cd) and hexavalent chromium (Cr VI), as well as two types of
brominated flame retardants (polybrominated biphenyls, PBBs, and polybrominated diphenyl
ethers, PBDEs) in electrotechnical equipment is restricted in current and proposed regional
legislation.
To demonstrate compliance with these requirements, it may be necessary to analyse
electrotechnical products for a variety of reasons:
• to supplement supply chain material declarations (companies may choose to test products
directly to determine compliance);
• companies may require their suppliers to perform analysis to support material
declarations;
• companies may perform "spot checks" of their suppliers to assess compliance
• enforcement authorities may perform testing as part of their market surveillance activities.
IEC 62321 already provides test methods for the determination of six regulated substances in
electrotechnical products. However, the preparatory steps before the analysis are critically
important in obtaining accurate, reproducible results. Prior to this PAS, there was virtually no
guidance or consensus as to how electrotechnical products should be sampled.
The purpose of this PAS is primarily to complement IEC 62321 by providing agreed guidelines
on how electrotechnical products, assemblies and components should be sampled to
determine the levels of restricted substances present.
Please note sampling and analytical testing is not the only way to obtain relevant information
on the levels of substances in an electrotechnical product or component. Experience and
knowledge of the materials used could remove the need for sampling and testing; for
example, flame retardants are never used in metals. Furthermore, analytical test reports and
material declarations received can be used to demonstrate that the levels of restricted
substances are below the required limits.

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ELECTROTECHNICAL PRODUCTS –
DETERMINATION OF RESTRICTED SUBSTANCES –
SAMPLING PROCEDURE – GUIDELINES


1 Scope
This PAS provides general sampling guidelines and strategies of sampling for electrotechnical
products, electronic assemblies, electronic components. In order to obtain samples that can
be used for analytical testing to determine the levels of restricted substances as described in
the test methods of IEC 62321. Restrictions for substances will vary between geographic
regions and from time to time. This PAS describes a generic process for the sampling of any
substance which could be restricted.
This PAS does not provide:

• Full guidance on each and every product that could be classified as electrotechnical
equipment. Since there is a huge variety of electrotechnical components, with various
structures and processes, along with the continuous innovations in the industry, it is
unrealistic to attempt to provide procedures for the disjointment of every type of
component.
• Analysis procedures to measure the levels of restricted substances. This is covered by
other standards (for example the future IEC 62321), which are referred to as the "test
standard" in this PAS.
• Guidelines for assessment of compliance.
• Guidance regarding other routes to gather additional information on restricted substances
in a product, although the information collected has relevance to the sampling strategies in
this PAS.
• Sampling procedures for packaging and packaging materials.
• Safe disassembly and mechanical disjointment instructions related to electrotechnical
products (e.g. Hg containing switches) and the recycling industry (e.g. how to handle
CRTs or the safe removal of batteries).
2 Normative references
The following referenced documents are indispensable for the application of this document.
For dated references, only the edition cited applies. For undated references, the latest edition
of the referenced document (including any amendments) applies.
IEC 62321, Electrotechnical products – Determination of levels of six restricted substances
(lead, mercury, cadmium, hexavalent chromium, polybrominated biphenyls, polybrominated
diphenyl ethers)
3 Terms, definitions and abbreviations
3.1 Terms and definitions
For the purpose of this document, the following terms and definitions apply.
NOTE As this PAS is closely related to IEC 62321, terms and definitions from that standard have not been
duplicated here.

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PAS 62596 © IEC:2009(E) – 7 –
3.1.1
electronic assembly
group of components, at least one of which is an electronic device, but in which individual
parts may be replaced without damage to the assembly
[Definition H.2.5.9, IEC 60730-1:1999]
EXAMPLE Group of components mounted on a printed wiring board.
3.1.2
electronic components
electrical or electronic devices that are not subject to disassembly without destruction or
impairment of design use. They are sometimes called electronic parts, or piece parts
[Definition 3.1.5, IEC 62239:2008]
EXAMPLE Resistors, capacitors, diodes, integrated circuits, hybrids, application specific integrated circuits,
wound components and relays.
3.1.3
composite testing
testing two or more materials as a single sample that could be mechanically disjointed if
necessary
3.1.3
electronics
electronic assembly and/or electronic component and/or field replaceable unit
3.1.4
field replaceable unit
FRU
part, component or subassembly that is easily removed (mechanically disjointed) using
ordinary tools
NOTE "Easily removed" consists of using ordinary tools to perform such functions as screwing or disconnecting,
and only without irreversibly destroying the unit.
[Definition 3.7, IEC Guide 114:2005]
3.1.5
disassembly
process of taking apart an electrotechnical product; possibly using simple hand tools such as
a screwdriver, pliers and wrenches
NOTE A disassembled unit can, in theory, be re-assembled and be made operational.
3.1.6
disjointment
process of, in principle, separating the materials by mechanical actions such as: unscrewing,
cutting, grinding, scratching and abrasive processes
NOTE A disjointed part or assembly cannot be re-assembled into an operational unit.
3.1.7
homogeneous material
material that cannot be mechanically disjoined into different materials
NOTE 1 The term "homogeneous" means "of uniform composition throughout". Examples of "homogeneous
materials" are individual types of: plastics, ceramics, glass, metals, alloys, paper, board, resins and coatings.
NOTE 2 The term "mechanically disjointed" means that the materials can, in principle, be separated by
mechanical actions such as: unscrewing, cutting, crushing, grinding and abrasive processes

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– 8 – PAS 62596 © IEC:2009(E)
3.1.8
infinite thickness
critical thickness
thickness of the specimen which, if increased, yields no increase in intensity of X-rays
measured from the sample due to their absorption by the sample matrix. This thickness varies
with the energy of X-rays
3.1.9
sampling
process of selecting a representative part or section of a product (any electrotechnical device)
for the purpose of determining by means of analysis the concentrations of restricted
substances present. Sampling can be carried out by selecting a section on an object or by
disassembly and disjointment
NOTE Representative part or section could be the lead-frame of an integrated circuit or the plastic jacket of an
electrical wire.
3.1.10
screening
analytical procedure to determine the presence or absence of substances or compounds in
the representative part or section of a product, relative to the value or values accepted as the
criterion for this decision
NOTE If the screening method produces values that are not conclusive, then additional analysis or other follow-up
actions may be necessary to make a final presence/absence decision
3.2 Abbreviations
AAS Atomic absorption spectroscopy
ABS Acrylonitrile butadiene styrene
AFS Atomic fluorescence spectroscopy
ASTM American Society for Testing and Materials
BGA Ball grid array (electronic component)
CV-AAS Cold vapour atomic absorption spectrometry
CRT Cathode ray rube (television)
DIP Dual-in-line package (electronic component)
DVD Digital versatile disc
ED XRF Energy dispersive X-ray fluorescence
EDX Energy dispersive X-ray spectroscopy
FRU Field replaceable unit
GC-MS Gas chromatography – mass spectrometry
GLP Good laboratory practice
HPLC-UV High-performance liquid chromatography – Ultraviolet
IC Integrated circuit
ICP-OES Inductively coupled plasma optical emission spectrometry
ICP-MS Inductively coupled plasma mass spectrometry
MDL Minimum detection level
LCD Liquid crystal display
MQCA Minimal quantity for chemical analysis
OEM Original equipment manufacturer
PAS Publicly Available Specification
PBB Polybrominated biphenyl

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PAS 62596 © IEC:2009(E) – 9 –
PBDE Polybrominated diphenyl ether
PC Polycarbonate
PDA Personal digital assistant
PE-HD High-density polyethylene
PS-HI High-impact polystyrene
PVC Polyvinyl chloride
PWB Printed wiring board
QA Quality assurance
SEM-EDX Scanning electron microscopy – energy dispersive XRF
SMD Surface mounted device
TFT Thin film transistor
TV Television
WD XRF Wavelength dispersive X-ray fluorescence
XRF X-ray fluorescence
4 Introduction to sampling
4.1 Introductory remark
Obtaining a sample (i.e. sampling) is the first step in analyzing electrotechnical products for
the presence of restricted substances. The strategy and process of sampling is often as
important as the analytical measurement itself. Hence an effective sampling strategy requires
a clear understanding of the electrotechnical product, reasons for the analysis, and the
requirements that are to be met.
Sampling and testing for restricted substances is performed for many reasons including:
• business-to-business for commercial release (e.g. contractual agreement between the
OEM and component manufacturer).
• compliance with regulatory limits.
• forensic/impact assessment (why the product does not satisfy contractual or legal
requirements, when did this happen, and how many products are affected?).
4.2 Requirements and concerns for restricted substances
While many governments, industry partners and other stakeholders have their own
requirements, it is not the intention of this PAS to discuss fully all of these differences.
However, awareness of different limits for regulated substances is an important step in
preparing the sampling strategy. This clause highlights the main areas of concern regarding
the requirements for restricted substances.
1. Restricted substances: Not all geographic regions or industrial partners restrict the same
substances. For example, some regions have chosen to restrict the use of only a few
specific PBDE compounds, while others have a broader restriction regarding this class of
flame-retardants. When sampling a product, component etc. it is critical to keep in mind
what are the applicable legal requirements.
2. Allowable limits for restricted substances: Generally speaking, the allowable levels of
most restricted substances are below 1 000 mg/kg. Some geographic regions and
industrial partners have limits below 1 000 mg/kg. For some product types, limits for
restricted substance are above 1 000 mg/kg, e.g. lead in copper and aluminum alloys.
3. Application of the allowable level: The manner in which the allowable level of a restricted
substance is applied to an electrotechnical product determines the sampling strategy and
how the test results are interpreted. Many geographic regions apply their allowable limits

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– 10 – PAS 62596 © IEC:2009(E)
to "homogeneous materials". In this PAS an “homogeneous material” (3.1.8) is defined as
a material that cannot be mechanically disjointed into different materials. However, the
interpretation of "homogeneous material" is not consistent across the different regions.
Some regions have defined the smallest possible amount of material to be homogeneous
(e.g. bonding wires in semiconductor chips only several microns thick), while other regions
try to apply a more pragmatic approach.
4. Applicable exemptions
...

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