prEN IEC 62321-3-1:2025
(Main)Determination of certain substances in electrotechnical products - Part 3-1: Screening - Lead, mercury, cadmium, total chromium total bromine, total phosphorus, total chlorine, total tin and total antimony content by x-ray fluorescence spectrometry
Determination of certain substances in electrotechnical products - Part 3-1: Screening - Lead, mercury, cadmium, total chromium total bromine, total phosphorus, total chlorine, total tin and total antimony content by x-ray fluorescence spectrometry
Détermination de certaines substances dans les produits électrotechniques - Partie 3-1: Détection de la présence de plomb, mercure, cadmium, chrome total, brome total, phosphore total, chlore total, étain total et antimoine total par la spectrométrie de fluorescence x
Določevanje posameznih snovi v elektrotehničnih izdelkih - 3-1. del: Presejanje elektrotehničnih izdelkov glede svinca, živega srebra, kadmija, celotnega kroma in celotnega broma z rentgensko fluorescenčno spektrometrijo
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-junij-2025
Določevanje posameznih snovi v elektrotehničnih izdelkih - 3-1. del: Presejanje
elektrotehničnih izdelkov glede svinca, živega srebra, kadmija, celotnega kroma in
celotnega broma z rentgensko fluorescenčno spektrometrijo
Determination of certain substances in electrotechnical products - Part 3-1: Screening -
Lead, mercury, cadmium, total chromium total bromine, total phosphorus, total chlorine,
total tin and total antimony content by X-ray fluorescence spectrometry
Détermination de certaines substances dans les produits électrotechniques - Partie 3-1:
Détection de la présence de plomb, mercure, cadmium, chrome total, brome total,
phosphore total, chlore total, étain total et antimoine total par la spectrométrie de
fluorescence x
Ta slovenski standard je istoveten z: prEN IEC 62321-3-1:2025
ICS:
13.020.01 Okolje in varstvo okolja na Environment and
splošno environmental protection in
general
29.020 Elektrotehnika na splošno Electrical engineering in
general
31.020 Elektronske komponente na Electronic components in
splošno general
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
111/813/CDV
COMMITTEE DRAFT FOR VOTE (CDV)
PROJECT NUMBER:
IEC 62321-3-1 ED2
DATE OF CIRCULATION: CLOSING DATE FOR VOTING:
2025-05-02 2025-07-25
SUPERSEDES DOCUMENTS:
111/697/CD, 111/745/CC
IEC TC 111 : ENVIRONMENTAL STANDARDIZATION FOR ELECTRICAL AND ELECTRONIC PRODUCTS AND SYSTEMS
SECRETARIAT: SECRETARY:
Italy Mr Alfonso Sturchio
OF INTEREST TO THE FOLLOWING COMMITTEES: HORIZONTAL FUNCTION(S):
TC 2,TC 9,TC 18,TC 20,TC 21,TC 23,TC 34,SC TC 111 Horizontal Basic Environment - Assessments
34D,TC 59,TC 62,SC 65B,TC 80,TC 82,TC 88,TC
91,TC 100,TC 110,TC 121,TC 124,TC 125
ASPECTS CONCERNED:
Environment
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for Vote (CDV) is submitted for parallel voting.
The CENELEC members are invited to vote through the
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This document is still under study and subject to change. It should not be used for reference purposes.
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Countries” clauses to be included should this proposal proceed. Recipients are reminded that the CDV stage is the
final stage for submitting ISC clauses. (SEE AC/22/2007 OR NEW GUIDANCE DOC).
TITLE:
Determination of certain substances in electrotechnical products - Part 3-1: Screening - Lead,
mercury, cadmium, total chromium total bromine, total phosphorus, total chlorine, total tin and
total antimony content by X-ray fluorescence spectrometry
PROPOSED STABILITY DATE: 2030
NOTE FROM TC/SC OFFICERS:
download this electronic file, to make a copy and to print out the content for the sole purpose of preparing National
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IEC CDV 62321-3-1 © IEC 2025 – 2 – 111/813/CDV
1 CONTENTS
3 1 Scope . 7
4 2 Normative references . 10
5 3 Terms, definitions and abbreviations . 10
6 4 Principle . 10
7 Overview . 10
8 Principle of test . 11
9 Explanatory comments . 11
10 5 Apparatus, equipment and materials . 12
11 XRF spectrometer . 12
12 Materials and tools . 12
13 6 Reagents . 12
14 7 Sampling . 12
15 General . 12
16 Non-destructive approach . 13
17 Destructive approach. 13
18 8 Test procedure . 13
19 General . 13
20 Preparation of the spectrometer . 14
21 Test portion . 15
22 Verification of spectrometer performance . 15
23 Tests . 17
24 Calibration . 17
25 9 Calculations . 18
26 10 Precision . 18
27 General . 18
28 Lead . 19
29 Mercury . 19
30 Cadmium . 19
31 Chromium . 19
32 Bromine. 19
33 Phosphorus, Chlorine, Tin, and Antimony . 19
34 Repeatability statement for five tested substances sorted by type of tested
35 material . 20
36 General . 20
37 Material: ABS (acrylonitrile butadiene styrene), as granules and
38 plates . 20
39 Material: PE (low density polyethtylene), as granules . 20
40 Material: PC/ABS (polycarbonate and ABS blend), as granules . 20
41 Material: HIPS (high impact polystyrene) . 21
42 Material: PVC (polyvinyl chloride), as granules . 21
43 Material: Polyolefin, as granules . 21
44 Material: Crystal glass . 21
45 Material: Glass . 21
46 Material: Lead-free solder, chips . 21
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47 Material: Si/Al Alloy, chips . 21
48 Material: Aluminum casting alloy, chips . 21
49 Material: PCB – Printed circuit board ground to less than 250 m . 22
50 Material: different plastics materials, as plates . 22
51 Reproducibility statement for five tested substances sorted by type of tested
52 material . 22
53 General . 22
54 Material: ABS (Acrylonitrile butadiene styrene), as granules and
55 plates . 22
56 Material: PE (low density polyethylene), as granules . 22
57 Material: PC/ABS (Polycarbonate and ABS blend), as granules . 23
58 Material: HIPS (high impact polystyrene) . 23
59 Material: PVC (polyvinyl chloride), as granules . 23
60 Material: Polyolefin, as granules . 23
61 Material: Crystal glass . 23
62 Material: Glass . 23
63 Material: Lead-free solder, chips . 24
64 Material: Si/Al alloy, chips . 24
65 Material: Aluminum casting alloy, chips . 24
66 Material: PCB – Printed circuit board ground to less than 250 m . 24
67 Material: different plastics materials, as plates . 24
68 11 Quality control . 24
69 Accuracy of calibration . 24
70 Control samples . 25
71 12 Special cases . 25
72 13 Test report . 25
73 Annex A (informative) Practical aspects of screening by X-ray fluorescence
74 spectrometry (XRF) and interpretation of the results . 26
75 A.1 Introductory remark . 26
76 A.2 Matrix and interference effects . 26
77 A.3 Interpretation of results (for regulated substances) . 27
78 A.4 Statistical data of the IIS2, IIS4, and IIS5 for the XRF method . 30
79 Annex B (informative) Practical examples of screening with XRF . 34
80 B.1 Introductory remark . 34
81 B.2 XRF instrumentation . 34
82 B.3 Factors affecting XRF results . 34
83 B.3.1 General . 34
84 B.3.2 Examples of screening with XRF . 35
IEC CDV 62321-3-1 © IEC 2025 – 4 – 111/813/CDV
89 INTERNATIONAL ELECTROTECHNICAL COMMISSION
90 ____________
92 DETERMINATION OF CERTAIN SUBSTANCES
93 IN ELECTROTECHNICAL PRODUCTS –
95 Part 3-1: Screening – Lead, mercury, cadmium, total chromium
96 total bromine, total phosphorus, total chlorine, total tin and total antimony
97 content by X-ray fluorescence spectrometry
99 FOREWORD
100 1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising
101 all national electrotechnical committees (IEC National Committees). The object of IEC is to promote international
102 co-operation on all questions concerning standardization in the electrical and electronic fields. To this end and
103 in addition to other activities, IEC publishes International Standards, Technical Specifications, Technical Reports,
104 Publicly Available Specifications (PAS) and Guides (hereafter referred to as “IEC Publication(s)”). Their
105 preparation is entrusted to technical committees; any IEC National Committee interested in the subject dealt with
106 may participate in this preparatory work. International, governmental and non-governmental organizations liaising
107 with the IEC also participate in this preparation. IEC collaborates closely with the International Organization for
108 Standardization (ISO) in accordance with conditions determined by agreement between the two organizations.
109 2) The formal decisions or agreements of IEC on technical matters express, as nearly as possible, an international
110 consensus of opinion on the relevant subjects since each technical committee has representation from all
111 interested IEC National Committees.
112 3) IEC Publications have the form of recommendations for international use and are accepted by IEC National
113 Committees in that sense. While all reasonable efforts are made to ensure that the technical content of IEC
114 Publications is accurate, IEC cannot be held responsible for the way in which they are used or for any
115 misinterpretation by any end user.
116 4) In order to promote international uniformity, IEC National Committees undertake to apply IEC Publications
117 transparently to the maximum extent possible in their national and regional publications. Any divergence between
118 any IEC Publication and the corresponding national or regional publication shall be clearly indicated in the latter.
119 5) IEC itself does not provide any attestation of conformity. Independent certification bodies provide conformity
120 assessment services and, in some areas, access to IEC marks of conformity. IEC is not responsible for any
121 services carried out by independent certification bodies.
122 6) All users should ensure that they have the latest edition of this publication.
123 7) No liability shall attach to IEC or its directors, employees, servants or agents including individual experts and
124 members of its technical committees and IEC National Committees for any personal injury, property damage or
125 other damage of any nature whatsoever, whether direct or indirect, or for costs (including legal fees) and
126 expenses arising out of the publication, use of, or reliance upon, this IEC Publication or any other IEC Publications.
127 8) Attention is drawn to the Normative references cited in this publication. Use of the referenced publications is
128 indispensable for the correct application of this publication.
129 9) Attention is drawn to the possibility that some of the elements of this IEC Publication may be the subject of patent
130 rights. IEC shall not be held responsible for identifying any or all such patent rights.
131 International Standard IEC 62321-3-1 has been prepared by IEC technical committee 111:
132 Environmental standardization for electrical and electronic products and systems.
133 The first edition of IEC 62321:2008 was a 'stand alone' standard that included an introduction,
134 an overview of test methods, a mechanical sample preparation as well as various test method
135 clauses.
136 The first edition of IEC 62321-3-1 is a partial replacement of IEC 62321:2008, forming a
137 structural revision and generally replacing Clauses 6 and Annex D.
138 This second edition of IEC 62321-3-1 includes the analysis of additional elements as indicators
139 for additional substances. The selection is based on IEC TR 62936:2016. There are also
140 comments about using the same methology for screening for content of critical raw materials
141 (CRMs).
IEC CDV 62321-3-1 © IEC 2025 – 5 – 111/813/CDV
143 Future parts in the IEC 62321 series will gradually replace the corresponding clauses in
144 IEC 62321:2008. Until such time as all parts are published, however, IEC 62321:2008 remains
145 valid for those clauses not yet re-published as a separate part.
146 The text of this standard is based on the following documents:
FDIS Report on voting
148 Full information on the voting for the approval of this standard can be found in the report on
149 voting indicated in the above table.
150 This publication has been drafted in accordance with the ISO/IEC Directives, Part 2.
151 A list of all parts in the IEC 62321 series can be found on the IEC website under the general
152 title: Determination of certain substances in electrotechnical products
153 The committee has decided that the contents of this publication will remain unchanged until the
154 stability date indicated on the IEC web site under "http://webstore.iec.ch" in the data related to
155 the specific publication. At this date, the publication will be
156 • reconfirmed,
157 • withdrawn,
158 • replaced by a revised edition, or
159 • amended.
IMPORTANT – The 'colour inside' logo on the cover page of this publication indicates
that it contains colours which are considered to be useful for the correct understanding
of its contents. Users should therefore print this document using a colour printer.
IEC CDV 62321-3-1 © IEC 2025 – 6 – 111/813/CDV
163 INTRODUCTION
164 The widespread use of electrotechnical products has drawn increased attention to their impact
165 on the environment. In many countries this has resulted in the adaptation of regulations
166 affecting wastes, substances and energy use of electrotechnical products.
167 The use of certain substances (e.g. lead (Pb), cadmium (Cd) and polybrominated diphenyl
168 ethers (PBDEs)) in electrotechnical products, is a source of concern in current and proposed
169 regional legislation. With the actual revision the following elements are added: phosphorus (P),
170 assuming the source of P is related to TCEP, Trixylyl-phosphate, chlorine (Cl), assuming the
171 source of Cl is related to SCCP, TCEP, TBTC, tin (Sn), assuming the source of Sn is related to
172 restricted organo-tin compounds, antimony (Sb), assuming the source of Sb is related to
173 Pyrochlore, antimony lead yellow.
174 The purpose of the IEC 62321 series is therefore to provide test methods that will allow the
175 electrotechnical industry to determine the levels of certain substances of concern in
176 electrotechnical products on a consistent global basis.
177 WARNING – Persons using this International Standard should be familiar with normal
178 laboratory practice. This standard does not purport to address all of the safety problems,
179 if any, associated with its use. It is the responsibility of the user to establish appropriate
180 safety and health practices and to ensure compliance with any national regulatory
181 conditions.
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183 DETERMINATION OF CERTAIN SUBSTANCES
184 IN ELECTROTECHNICAL PRODUCTS –
186 Part 3-1: Screening – Lead, mercury, cadmium, total chromium
187 total bromine, total phosphorus, total chlorine, total tin and total antimony
188 content by X-ray fluorescence spectrometry
190 1 Scope
191 Part 3-1 of IEC 62321 describes the screening analysis of substances, specifically lead (Pb),
192 mercury (Hg), cadmium (Cd), total chromium (Cr), total bromine (Br), total phosphorus (P),
193 assuming the source of P is related to TCEP (CAS 115-96-8), Trixylyl-phosphate (CAS 25155-
194 23-1), total chlorine (Cl), assuming the source of Cl is related to SCCP (CAS 85535-84-8),
195 TCEP (CAS 115-96-8) , TBTC (CAS 1461-22-9), total tin (Sn), assuming the source of Sn is
196 related to restricted organo-tin compounds, total antimony (Sb), assuming the source of Sb is
197 related to Pyrochlore, antimony lead yellow (CAS 8012-00-8) in uniform materials found in
198 electrotechnical products, using the analytical technique of X-ray fluorescence (XRF)
199 spectrometry.
200 The same methodology can also be used for screening of substances discussed as critical raw
201 materials in various countries (for example currently discussed in the EU: antimony (Sb), baryte,
202 bismuth (Bi), cobalt (Co), fluorspar, gallium (Ga), germanium (Ge), hafnium (Hf), indium (In),
203 magnesium (Mg), niobium (Nb), phosphorus (P), scandium (Sc), tantalum (Ta), tungsten (W),
204 vanadium (V), platinum group metals, heavy rare earth elements, light rare earth elements).
205 NOTE From EU information on critical raw materials [1] Raw materials are crucial to Europe’s economy. They form
206 a strong industrial base, producing a broad range of goods and applications used in everyday life and modern
207 technologies. Reliable and unhindered access to certain raw materials is a growing concern within the EU and across
208 the globe. To address this challenge, the European Commission has created a list of critical raw materials (CRMs)
209 for the EU, which is subject to a regular review and update. CRMs combine raw materials of high importance to the
210 EU economy and of high risk associated with their supply.
211 The method is applicable to polymers, metals and ceramic materials. The test method may be
212 applied to raw materials, individual materials taken from products and “homogenized” mixtures
213 of more than one material. Screening of a sample is performed using any type of XRF
214 spectrometer, provided it has the performance characteristics specified in this test method. Not
215 all types of XRF spectrometers are suitable for all sizes and shapes of sample. Care should be
216 taken to select the appropriate spectrometer design for the task concerned.
217 The performance of this test method has been tested for the following substances in various
218 media and within the concentration ranges as specified in Tables 1 to 5. During a Pre-IIS the
219 feasibility of the test method to be used for the added elements was tested. The results are
220 listed in the Tables 6-10.
221 NOTE The text of this document will be reviewed and will be used for a full IIS, which is
222 planned for spring 2024.
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224 Table 1 – Tested concentration ranges for lead in materials
Substance/
Lead
element
Medium/material tested
Unit of
a b d
Low- Al, Lead- Ground Crystal Poly-
Parameter ABS PE PVC
measure
c
alloy Al-Si free glass olefine
PWB
steel alloy solder
Concentration
15,7 14 190 22 000 390
or 380 to
e
mg/kg to to 30 to 174 to 240 000 to
concentration 640
954 108 930 23 000 665
range tested
a
Acrylonitrile butadiene styrene.
b
Polyethylene.
c
Printed wiring board.
d
Polyvinyl chloride.
e
This lead concentration was not detectable by instruments participating in tests.
226 Table 2 – Tested concentration ranges for mercury in materials
Substance/element Mercury
Medium/material tested
Parameter Unit of measure
a b
ABS PE
Concentration or concentration range
mg/kg 100 to 942 4 to 25
tested
a
Acrylonitrile butadiene styrene.
b
Polyethylene.
229 Table 3 – Tested concentration ranges for cadmium in materials
Substance/element Cadmium
Medium/material tested
Parameter Unit of measure
a b
Lead-free solder
ABS PE
Concentration or concentration
c
mg/kg 10 to 183 19,6 to 141
range tested
a
Acrylonitrile butadiene styrene.
b
Polyethylene.
c
This cadmium concentration was not detectable by instruments participating in tests .
231 Table 4 – Tested concentration ranges for total chromium in materials
Substance/element Chromium
Medium/material tested
Unit of
Low-
Parameter
Al, Al-Si
measure a b
ABS PE alloy Glass
alloy
steel
Concentration or
concentration range mg/kg 16 to 944 16 to 115 240 130 to 1 100 94
tested
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a
Acrylonitrile butadiene styrene.
b
Polyethylene.
233 Table 5 – Tested concentration ranges for total bromine in materials
Substance/element Bromine
Medium/material tested
Unit of
Parameter
measure
c a d b
HIPS , ABS PC/ABS PE
Concentration or concentration
mg/kg 25 to 118 400 800 to 2 400 96 to 808
range tested
a
Acrylonitrile butadiene styrene.
b
Polyethylene.
c
High impact polystyrene.
d
Polycarbonate and ABS blend.
235 Table 6 – Tested concentration ranges for total phosphorus in materials
Substance/element Phosphorus
Medium/material
Unit of
tested
Parameter
measure
plastics
Concentration or concentration
mg/kg 90 to 8300
range tested
237 Table 7 – Tested concentration ranges for total chlorine in materials
Substance/element Chlorine
Medium/material
Unit of
tested
Parameter
measure
plastics
Concentration or concentration
mg/kg 100 to 380
range tested
239 Table 8 – Tested concentration ranges for total tin in materials
Substance/element Tin
Medium/material
Unit of
tested
Parameter
measure
plastics
Concentration or concentration
mg/kg 30 to 110
range tested
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241 Table 9 – Tested concentration ranges for total antimony in materials
Substance/element Antimony
Medium/material
Unit of
tested
Parameter
measure
plastics
Concentration or concentration
mg/kg 190 to 380
range tested
243 These substances in similar media outside of the specified concentration ranges may be
244 analysed according to this test method; however, the performance has not been established for
245 this standard.
246 2 Normative references
247 The following documents, in whole or in part, are normatively referenced in this document and
248 are indispensable for its application. For dated references, only the edition cited applies. For
249 undated references, the latest edition of the referenced document (including any amendments)
250 applies.
251 IEC 62321-1, Determination of certain substances in electrotechnical products – Part 1:
252 Introduction and overview
253 IEC 62321-2, Determination of certain substances in electrotechnical products – Part 2:
254 Disassembly, disjointment and mechanical sample preparation
255 IEC/ISO Guide 98-1, Uncertainty of measurement – Part 1: Introduction to the expression of
256 uncertainty in measurement
257 3 Terms, definitions and abbreviations
258 For the purposes of this document, the terms, definitions and abbreviations given in IEC 62321-
259 1 and IEC 62321-2 apply.
260 4 Principle
261 Overview
262 The concept of 'screening' has been developed to reduce the amount of testing. Executed as a
263 predecessor to any other test analysis, the main objective of screening is to quickly determine
264 whether the screened part or section of a product:
265 – contains a certain substance at a concentration significantly higher than its value or values
266 chosen as criterion, and therefore may be deemed unacceptable.
267 – contains a certain substance at a concentration significantly lower than its value or values
268 chosen as criterion, and therefore may be deemed acceptable.
269 – contains a certain substance at a concentration so close to the value or values chosen as
270 criterion that when all possible errors of measurement and safety factors are considered,
___________
To be published.
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271 no conclusive decision can be made about the acceptable absence or presence of a certain
272 substance and, therefore, a follow-up action may be required, including further analysis
273 using verification testing procedures.
274 For the screening analysis of critical raw materials only the analysis results is important, there
275 is no interpretation with regards to a maximum threshold value required.
276 This test method is designed specifically to screen for lead, mercury, cadmium, chromium ,
277 bromine, phosphorus, chlorine, tin and antimony (Pb, Hg, Cd, Cr, Br, P, Cl, Sn, Sb) plus
278 elements required for screening for content of critical raw materials in uniform materials, which
279 occur in most electrotechnical products. Under typical circumstances, XRF spectrometry
280 provides information on the total quantity of each element present in the sample but does not
281 identify compounds or valence states of the elements. Therefore, special attention shall be paid
282 when screening for chromium, bromine, phosphorus, chlorine, tin and antimony, where the
283 result will reflect only the total chromium, total bromine, total phosphorus, total chlorine, total
284 tin and total antimony present. The presence of Cr(VI) or the brominated flame retardants PBB
285 or PBDE or TBBPA or HBCDD, or TCEP, Trixylyl-phosphate, Red phosphorus, SCCP or MCCP,
286 TBTC, restricted organo-tin compounds, Pyrochlore, or antimony lead yellow shall be confirmed
287 by a verification test procedure that identify compounds or valence states of the elements. When
288 applying this method to electronics “as received”, which, by the nature of their design, are not
289 uniform, care shall be taken in interpreting the results. Similarly, the analysis of Cr in conversion
290 coatings may be difficult due to the presence of Cr in substrate material and/or because of
291 insufficient sensitivity for Cr in typically very thin (several hundred nm) conversion coating
292 layers.
293 Screening analysis can be carried out by one of two means:
294 • non-destructively – by directly analysing the sample “as received”;
295 • destructively – by applying one or more sample preparation steps prior to analysis.
296 In the latter case, the user shall apply the procedure for sample preparation as described in
297 IEC 62321-2. This test method will guide the user in choosing the proper approach to sample
298 presentation.
299 Principle of test
300 The representative specimen of the object tested is placed in the measuring chamber or over
301 the measuring aperture of the X-ray fluorescence spectrometer. Alternatively, a measuring
302 window/aperture of a handheld, portable XRF analyser is placed flush against the surface of
303 the object tested. The analyser illuminates the specimen for a preselected measurement time
304 with a beam of X rays which in turn excite characteristic X rays of elements in the specimen.
305 The intensities of these characteristic X rays are measured and converted to mass fractions or
306 concentrations of the elements in the tested sample using a calibration implemented in the
307 analyser.
308 The fundamentals of XRF spectrometry, as well as practical aspects of sampling for XRF, are
309 covered in detail in [2, 3 and 4].
310 Explanatory comments
311 To achieve its purpose, this test method shall provide rapid, unambiguous identification of the
312 elements of interest. The test method shall provide at least a level of accuracy that is sometimes
313 described as semi-quantitative, i.e. the relative uncertainty of a result is typically 30 % or better
314 at a defined level of confidence of 68 %. Some users may tolerate higher relative uncertainty,
315 depending on their needs. This level of performance allows the user to sort materials for
316 additional testing. The overall goal is to obtain information for risk management purposes.
317 This test method is designed to allow XRF spectrometers of all designs, complexity and
318 capability to contribute screening analyses. However, the capabilities of different XRF
319 spectrometers cover such a wide range that some will be relatively inadequate in their selectivity
320 and sensitivity while others will be more than adequate. Some spectrometers will allow easy
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321 measurement of a wide range of sample shapes and sizes, while others, especially research -
322 grade WDXRF units, will be very inflexible in terms of test portions.
323 Given the above level of required performance and the wide variety of XRF spectrometers
324 capable of contributing useful measurements, the requirements for the specification of
325 procedures are considerably lower than for a high-performance test method for quantitative
326 determinations with low estimates of uncertainty.
327 This test method is based on the concept of a performance based measurement system.
328 Apparatus, sample preparation and calibration are specified in this standard in relatively general
329 terms. It is the responsibility of the user to document all procedures developed in the laboratory
330 that uses the test method. The user shall establish a written procedure for all cases denoted in
331 this method by the term “work instructions”.
332 The user of this test method shall document all relevant spectrometer and method performance
333 parameters.
334 WARNING 1 Persons using the XRF test method shall be trained in the use of XRF
335 spectrometers and the related sampling requirements.
336 WARNING 2 X rays are hazardous to humans. Care shall be taken to operate the equipment
337 in accordance with both the safety instructions provided by the manufacturer and the applicable
338 local health and occupational safety regulations.
339 5 Apparatus, equipment and materials
340 XRF spectrometer
341 An XRF spectrometer consists of an X-ray excitation source, a means of reproducible sample
342 presentation, an X-ray detector, a data processor and a control system [5, 6 and 7]:
343 a) source of X-ray excitation – X-ray tube or radio-isotope sources are commonly used;
344 b) X-ray detector (detection subsystem) – Device used to convert the energy of an X-ray photon
345 to a corresponding electric pulse of amplitude proportional to the photon energy.
346 Materials and tools
347 All materials used in the preparation of samples for XRF measurements shall be shown to be
348 free of contamination, specifically by the analytes of this test method. This means that all
349 grinding materials, solvents, fluxes, etc. shall not contain detectable quantities of Pb, Hg, Cd,
350 Cr and/or Br.
351 Tools used in the handling of samples shall be chosen to minimize contamination by the
352 analytes of this test method as well as by any other elements. Any procedures used to clean
353 the tools shall not introduce contaminants.
354 6 Reagents
355 Reagents, if any, shall be of recognized analytical grade and shall not contain detectable
356 quantities of Pb, Hg, Cd, Cr, Br, P, Cl, Sn, Sb and/or any critical raw materials.
357 7 Sampling
358 General
359 It is the responsibility of the user of this test method to define the test sample using documented
360 work instructions. The user may choose to define the test sample in a number of ways, either
IEC CDV 62321-3-1 © IEC 2025 – 13 – 111/813/CDV
361 via a non-destructive approach in which the portion to be measured is defined by the viewing
362 area of the spectrometer, or by a destructive approach in which the portion to be measured is
363 removed from the larger body of material and either measured as is, or destroyed and prepared
364 using a defined procedure.
365 Non-destructive approach
366 The user of this test method shall:
367 a) establish the area viewed by the spectrometer and place the test sample within that area,
368 taking care to ascertain that no fluorescent X-rays will be detected from materials other than
369 the defined test portion. Usually, the area viewed by the spectrometer is a section of a plane
370 delineated by the shape and boundary of the measuring window of the instrument. The area
371 of the test sample viewed by the spectrometer shall be flat. Any deviation from the flat area
372 requirement shall be documented;
373 b) make sure that a repeatable measurement geometry with a repeatable distance between
374 the spectrometer and the test portion is established;
375 c) document the steps taken to disassemble a larger object to obtain a test portion.
376 Destructive approach
377 The following points shall be taken into account in the destructive approach:
378 a) the user shall create and follow a documented work instruction for the means of destruction
379 applied to obtain the test portion, as this information is critical for correct interpretation of
380 the measurement results;
381 b) a procedure that results in a powder shall produce a material with a known or controlled
382 particle size. In cases where the particles have different chemical, phase or mineralogical
383 compositions, it is critical to reduce their size sufficiently to minimize d ifferential absorption
384 effects;
385 c) in a procedure that results in a material being dissolved in a liquid matrix, the quantity and
386 physical characteristics of the material to be dissolved shall be controlled and documented.
387 The resulting solution shall be completely homogeneous. Instructions shall be provided to
388 deal with undissolved portions to ensure proper interpretation of the measured results.
389 Instructions shall be provided for presentation of the test portion of the solution to the X -ray
390 spectrometer in a repeatable manner, i.e. in a liquid cell of specified construction and
391 dimensions;
392 d) in a procedure that results in a sample material being fused or pressed in a solid matrix, the
393 quantity and physical characteristics of the sample material shall be controlled and
394 documented. The resulting solid (fused or pressed pellet) shall be completely uniform.
395 Instructions shall be provided to deal with unmixed portions to ensure proper interpretation
396 of the measured results.
397 8 Test procedure
398 General
399 The test procedure covers preparation of the X-ray spectrometer, preparation and mounting of
400 test portions and calibration. Certain instructions are presented in general terms due to the wide
401 range of XRF equipment and the even greater variety of laboratory and test samples to which
402 this test method will be applied. However, a cardinal rule that applies without exception to all
403 spectrometers and analytical methods shall be followed; that is that the calibration and sample
404 measurements be performed under the same conditions and using the same sample preparation
405 procedures.
406 In view of the wide range of XRF spectrometer designs and the concomitant range of detection
407 capabilities, it is important to understand the limitation of the chosen instrument. Certain
408 designs may be incapable of detecting or accurately determining the composition of a very small
409 area or very thin samples. As a consequence, it is imperative that users carefully establish and
IEC CDV 62321-3-1 © IEC 2025 – 14 – 111/813/CDV
410 clearly document the performance of the test method as implemented in their laboratories. One
411 goal is to prevent false negative test results.
412 Preparation of the spectrometer
413 Prepare the spectrometer as follows:
414 a) switch on the instrument and prepare it for operation according to the manufacturer’s
415 manual. Allow the instrument to stabilize as per guidelines established by the manufacturer
416 or laboratory work instructions;
417 b) set the measurement conditions to the optimum conditions previously established by the
418 manufacturer or the laboratory.
419 Many instruments available on the market are already optimized and preset for a particular
420 application, and therefore this step might not be necessary. Otherwise, the laboratory should
421 establish optimum operating conditions for each calibration. Choices should be made to
422 optimize sensitivity and minimize spectral interferences. Excitation conditions may vary by
423 material, analyte and X-ray line energy. A list of recommended analytical X-ray lines is given in
424 Table 6.
425 Detection system settings should optimize the compromise between sensitivity and energy
426 resolution. Guidance can usually be found in the instrument manual and in literature on X-ray
427 spectrometry [2, 3 and 4].
a
428 Table 6 – Recommended X-ray lines for individual analytes
Analyte Preferred line Secondary line
L –M (Lβ ) L –M (Lα )
Lead (Pb)
2 4 1 3 4,5 1,2
L –M (Lα )
Mercury (Hg)
3 4,5 1,2
b
Cadmium (Cd) K–L (Kα )
2,3 1,2
K–L (Kα )
Chromium (Cr)
2,3 1,2
K–L (Kα ) K–M (Kβ )
Bromine (Br)
2,3 1,2 2,3 1,3
K–L (Kα )
Phosphorus (P)
2,3 1,2
K–L (Kα )
Chlorine (Cl)
2,3 1,2
K–L (Kα )
Tin (Sn)
2,3 1,2
K–L (Kα )
Antimony (Sb)
2,3 1,2
a
Other X-ray line choices may provide adequate performance. However, when deciding on alternative
analytical lines one should be aware of possible spectral interferences from other elements present in the
sample (e.g. Br K on Pb L or As K on Pb L lines; see Clause A.2 b) for more typical examples).
α α α α
b
K–L (Kα ) means that there are actually two transitions to the K shell, i.e. one from the L shell which
2,3 1,2 2
generates Kα X-rays and another from the L shell that generates Kα X- rays. However, since both energies
2 3 1
are very close, energy dispersive spectrometers cannot distinguish them and so they are analysed as one
combined K α energy.
1,2
IEC CDV 62321-3-1 © IEC 2025 – 15 – 111/813/CDV
Analyte Preferred line Secondary line
c
K–L (Kα ) L –M (Lα )
Barium (Ba)
2,3 1,2 3 4,5 1,2
L –M (Lα )
Bismuth (Bi)
3 4,5 1,2
K–L (Kα ) K–M (Kβ )
Cobalt (Co)
2,3 1,2 2,3 1,3
d
K–L (Kα )
Calcium (Ca)
2,3 1,2
K–L (Kα )
Gallium (Ga)
2,3 1,2
K–L (Kα )
Germanium (Ga)
2,3 1,2
L –M
...
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