Determination of certain substances in electrotechnical products - Part 8: Phthalates in polymers by gas chromatography-mass spectrometry (GC-MS), gas chromatography-mass spectrometry using a pyrolyzer/thermal desorption accessory (Py/TD-GC-MS)

This part of IEC 62321 specifies two normative and two informative techniques for the
determination of di-isobutyl phthalate (DIBP), di-n-butyl phthalate (DBP), benzylbutyl
phthalate (BBP), di-(2-ethylhexyl) phthalate (DEHP), di-n-octyl phthalate (DNOP), di-isononyl
phthalate (DINP) and di-iso-decyl phthalate (DIDP) in polymers of electrotechnical products.
Gas chromatography-mass spectrometry (GC-MS) and gas chromatography-mass
spectrometry (Py/TD-GC-MS) techniques are described in the normative part of this document.
The GC-MS method is considered the referee technique for the quantitative determination of
DIBP, DBP, BBP, DEHP, DNOP, DINP and DIDP in the range of 50 mg/kg to 2 000 mg/kg.
The GC-MS coupled with a pyrolyzer/thermal desorption (TD) accessory is suitable for
screening and semi-quantitative analysis of DIBP, DBP, BBP, DEHP, DNOP, DINP, and DIDP
in polymers that are used as parts of the electrotechnical products in the range of 100 mg/kg
to 2 000 mg/kg.
The IAMS technique is suitable for screening and semi-quantitative analysis of DIBP, DBP,
BBP, DEHP, DNOP, DINP, and DIDP. Determination of DBP and DIBP, DEHP and DNOP by
IAMS has not been established due to peak and mass spectral resolution limitations.
The LC-MS technique is limited to the determination of of BBP, DEHP, DNOP, DINP, and
DIDP. Determination of DBP and DIBP by LC-MS has not been established due to peak and
mass spectral resolution limitations.
A flow chart depicting how the normative Py/TD-GC-MS and GC-MS methods and informative
methods using ion attachment mass spectrometry (IAMS) coupled with direct injection probe
(DIP) and liquid chromatography-mass spectrometry (LC-MS) can be used are provided in
annexes of this document.
These four test methods have been evaluated by the test of PE (polyethylene) and PVC
(polyvinyl chloride) materials containing individual phthalates between ~450 mg/kg to
30 000 mg/kg as depicted in the normative and informative parts of this document. The use of
the four methods described in this document for other polymer types, phthalate compounds or
concentration ranges other than those specified above has not been specifically evaluated.

Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik - Teil 8: Phthalate in Polymeren mittels Gaschromatographie-Massenspektrometrie (GC-MS), Gaschromatographie-Massenspektrometrie mit Nutzung des Zusatzes der Pyrolyse/thermischen Desorption (Py/TD-GC-MS)

Détermination de certaines substances dans les produits électrotechniques - Partie 8: Analyse des phtalates dans les polymères par chromatographie en phase gazeuse-spectrométrie de masse (GC-MS), chromatographie en phase gazeuse-spectrométrie de masse par pyrolyse/thermodésorption (Py/TD-GC-MS)

L'IEC 62321-8:2017 spécifie deux techniques normatives et deux techniques informatives de détermination de la présence de phtalate de diisobutyle (DIBP - di-isobutyl phthalate), de phtalate de dibutyle (DBP - di-n-butyl phthalate), de phtalate de benzyle et de butyle (BBP - benzylbutyl phthalate), de phtalate de bis(2-éthylhexyle) (DEHP - di-(2-ethylhexyl) phthalate), de phtalate de di-n-octyle (DNOP - di-n-octyl phthalate), de phtalate de di-isononyle (DINP - di-isononyl phthalate) et de phtalate de di-isodécyle (DIDP - di-iso-decyl phthalate) dans les polymères qui sont utilisés dans des produits électrotechniques.

Določevanje posameznih substanc v elektrotehniških izdelkih - 8. del: Ftalati v polimerih s plinsko kromatografijo-masno spektrometrijo (GC-MS), plinsko kromatografijo-masno spektrometrijo z uporabo pirolize/toplotne desorpcije (Py/TD-GC-MS)

Ta del standarda IEC 62321 določa dve normativni in dve informativni tehniki za določanje di-izobutil ftalata (DIBP), di-n-butil ftalata (DBP), butil benzil ftalata (BBP), di-2-etilheksil ftalata (DEHP), di-n-oktil ftalata (DNOP), di-izononil ftalata (DINP) in di-izo-decil ftalata (DIDP) v polimerih v elektrotehniških izdelkih.
V normativnem delu tega dokumenta sta opisani plinska kromatografija-masna spektrometrija (GC-MS) in plinska kromatografija-masna spektrometrija z uporabo pirolize/toplotne desorpcije (Py/TD-GC-MS).
Metoda GC-MS je glavna tehnika za kvantitativno določanje DIBP, DBP, BBP, DEHP, DNOP, DINP in DIDP v razponu 50–2000 mg/kg.
Metoda GC-MS z uporabo pirolize/toplotne desorpcije (TD) je primerna za presejalne preskuse in polkvantitativno analizo DIBP, DBP, BBP, DEHP, DNOP, DINP in DIDP v polimerih, ki se uporabljajo kot deli elektrotehniških izdelkov v razponu 100–2000 mg/kg.
Tehnika masne spektrometrije s pripenjanjem iona (IAMS) je primerna za presejalne preskuse in polkvantitativno analizo DIBP, DBP, BBP, DEHP, DNOP, DINP in DIDP. DBP in DIBP ter DEHP in DNOP niso določeni z masno spektrometrijo s pripenjanjem iona (IAMS) zaradi omejitev pri določanju vrhov in omejitev ločljivosti masnega spektra.
Tehnika LC-MS je omejena na določanje BBP, DEHP, DNOP, DINP in DIDP. DBP in DIBP nista določena z metodo LC-MS zaradi omejitev pri določanju vrhov in omejitev ločljivosti masnega spektra.
Diagram poteka, ki prikazuje, kako je mogoče uporabiti normativni metodi Py/TD-GC-MS in GC-MS ter informativne metode z masno spektrometrijo s pripenjanjem iona (IAMS) skupaj s sondo za neposredno injiciranje (DIP) in tekočinsko kromatografijo – masno spektrometrijo (LC-MS), je na voljo v dodatkih tega dokumenta.
Te štiri preskusne metode so bile ocenjene s preskusom PE (polietilenskih) in PVC (polivinilkloridnih) materialov, ki vsebujejo posamezne ftalate ~450–30.000 mg/kg, kot je prikazano v normativnem in informativnem delu tega dokumenta. Uporaba teh štirih metod, ki so opisane v tem dokumentu, za druge vrste polimerov, ftalatov ali razpone koncentracij, ki niso določene zgoraj, ni bila posebej ocenjena.

General Information

Status
Published
Publication Date
08-Aug-2017
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
24-Jul-2017
Due Date
28-Sep-2017
Completion Date
09-Aug-2017

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SLOVENSKI STANDARD
SIST EN 62321-8:2017
01-september-2017
'RORþHYDQMHSRVDPH]QLKVXEVWDQFYHOHNWURWHKQLãNLKL]GHONLKGHO)WDODWLY
SROLPHULKVSOLQVNRNURPDWRJUDILMRPDVQRVSHNWURPHWULMR *&06 SOLQVNR
NURPDWRJUDILMRPDVQRVSHNWURPHWULMR]XSRUDERSLUROL]HWRSORWQHGHVRUSFLMH
3\7'*&06

Determination of certain substances in electrotechnical products - Part 8: Phthalates in

polymers by gas chromatography-mass spectrometry (GC-MS), gas chromatography-
mass spectrometry using a pyrolyzer/thermal desorption accessory (Py/TD-GC-MS)
Ta slovenski standard je istoveten z: EN 62321-8:2017
ICS:
29.020 Elektrotehnika na splošno Electrical engineering in
general
31.020 Elektronske komponente na Electronic components in
splošno general
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
SIST EN 62321-8:2017 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST EN 62321-8:2017
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SIST EN 62321-8:2017
EUROPEAN STANDARD EN 62321-8
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2017
ICS 31.020; 71.040.50
English Version
Determination of certain substances in electrotechnical products
- Part 8: Phthalates in polymers by gas chromatography-mass
spectrometry (GC-MS), gas chromatography-mass spectrometry
using a pyrolyzer/thermal desorption accessory (Py/TD-GC-MS)
(IEC 62321-8:2017)

Détermination de certaines substances dans les produits Verfahren zur Bestimmung von bestimmten Substanzen in

électrotechniques - Partie 8: Analyse des phtalates dans les Produkten der Elektrotechnik - Teil 8: Phthalate in

polymères par chromatographie en phase gazeuse- Polymeren mit Pyrolyse-Gaschromatographie-

spectrométrie de masse (GC-MS), chromatographie en Massenspektrometrie (Py-GC-MS), Ionen-Anlagerungs-

phase gazeuse-spectrométrie de masse par Massenspektrometrie (IAMS), Gaschromatographie-

pyrolyse/thermodésorption (Py/TD-GC-MS) Massenspektrometrie (GC-MS) und
(IEC 62321-8:2017) Flüssigchromatographie-Massenspektrometrie (LC-MS)
(IEC 62321-8:2017)

This European Standard was approved by CENELEC on 2017-05-02. CENELEC members are bound to comply with the CEN/CENELEC

Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration.

Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC

Management Centre or to any CENELEC member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by translation

under the responsibility of a CENELEC member into its own language and notified to the CEN-CENELEC Management Centre has the

same status as the official versions.

CENELEC members are the national electrotechnical committees of Austria, Belgium, Bulgaria, Croatia, Cyprus, the Czech Republic,

Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,

Lithuania, Luxembourg, Malta, the Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden,

Switzerland, Turkey and the United Kingdom.
European Committee for Electrotechnical Standardization
Comité Européen de Normalisation Electrotechnique
Europäisches Komitee für Elektrotechnische Normung
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2017 CENELEC All rights of exploitation in any form and by any means reserved worldwide for CENELEC Members.

Ref. No. EN 62321-8:2017 E
---------------------- Page: 3 ----------------------
SIST EN 62321-8:2017
EN 62321-8:2017
European foreword
The text of document 111/416/CDV, future edition 1 of IEC 62321-8, prepared by

IEC/TC 111 "Environmental standardization for electrical and electronic products and systems" was

submitted to the IEC-CENELEC parallel vote and approved by CENELEC as EN 62321-8:2017.

The following dates are fixed:
(dop) 2018-02-02
• latest date by which the document has to be
implemented at national level by
publication of an identical national
standard or by endorsement
• latest date by which the national (dow) 2020-05-02
standards conflicting with the
document have to be withdrawn

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CENELEC shall not be held responsible for identifying any or all such patent rights.

Endorsement notice

The text of the International Standard IEC 62321-8.2017 was approved by CENELEC as a European

Standard without any modification.

In the official version, for Bibliography, the following notes have to be added for the standards

indicated:
ISO 3696 NOTE Harmonized as EN ISO 3696.
ISO/IEC 17025 NOTE Harmonized as EN ISO/IEC 17025.
IEC 62321-2:2013 NOTE Harmonized as EN 62321-2:2014.
IEC 62321-6:2015 NOTE Harmonized as EN62321-6:2016
---------------------- Page: 4 ----------------------
SIST EN 62321-8:2017
EN 62321-8:2017
Annex ZA
(normative)
Normative references to international publications
with their corresponding European publications

The following documents, in whole or in part, are normatively referenced in this document and are

indispensable for its application. For dated references, only the edition cited applies. For undated

references, the latest edition of the referenced document (including any amendments) applies.

NOTE 1 When an International Publication has been modified by common modifications, indicated by (mod), the relevant

EN/HD applies.

NOTE 2 Up-to-date information on the latest versions of the European Standards listed in this annex is available here:

www.cenelec.eu.
Publication Year Title EN/HD Year
IEC 62321-1 2013 Determination of certain substances in EN 62321-1 2013
electrotechnical products -- Part 1:
Introduction and overview
---------------------- Page: 5 ----------------------
SIST EN 62321-8:2017
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SIST EN 62321-8:2017
IEC 62321-8
Edition 1.0 2017-03
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
Determination of certain substances in electrotechnical products –
Part 8: Phthalates in polymers by gas chromatography-mass spectrometry
(GC-MS), gas chromatography-mass spectrometry using a pyrolyzer/thermal
desorption accessory (Py/TD-GC-MS)
Détermination de certaines substances dans les produits électrotechniques –
Partie 8: Analyse des phtalates dans les polymères par chromatographie en
phase gazeuse-spectrométrie de masse (GC-MS), chromatographie en phase
gazeuse-spectrométrie de masse par pyrolyse/thermodésorption (Py/TD-GC-MS)
INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
COMMISSION
ELECTROTECHNIQUE
INTERNATIONALE
ICS 31.020; 71.040.50 ISBN 978-2-8322-4144-8

Warning! Make sure that you obtained this publication from an authorized distributor.

Attention! Veuillez vous assurer que vous avez obtenu cette publication via un distributeur agréé.

® Registered trademark of the International Electrotechnical Commission
Marque déposée de la Commission Electrotechnique Internationale
---------------------- Page: 7 ----------------------
SIST EN 62321-8:2017
– 2 – IEC 62321-8:2017 © IEC 2017
CONTENTS

FOREWORD ........................................................................................................................... 6

INTRODUCTION ..................................................................................................................... 8

1 Scope .............................................................................................................................. 9

2 Normative references ...................................................................................................... 9

3 Terms, definitions and abbreviated terms ...................................................................... 10

3.1 Terms and definitions ............................................................................................ 10

3.2 Abbreviated terms ................................................................................................. 10

4 Principle ........................................................................................................................ 11

5 Reagents and materials ................................................................................................. 11

5.1 GC-MS method ..................................................................................................... 11

5.2 Py/TD-GC-MS method .......................................................................................... 12

6 Apparatus ...................................................................................................................... 12

6.1 GC-MS method ..................................................................................................... 12

6.2 Py/TD-GC-MS method .......................................................................................... 13

7 Sampling ....................................................................................................................... 14

7.1 General ................................................................................................................. 14

7.2 GC-MS method ..................................................................................................... 14

7.3 Py/TD-GC-MS method .......................................................................................... 14

8 Procedure ...................................................................................................................... 14

8.1 General instructions for the analysis ..................................................................... 14

8.1.1 Overview ....................................................................................................... 14

8.1.2 GC-MS method .............................................................................................. 14

8.1.3 Py/TD-GC-MS method ................................................................................... 14

8.2 Sample preparation ............................................................................................... 15

8.2.1 GC-MS method .............................................................................................. 15

8.2.2 Py/TD-GC-MS method ................................................................................... 16

8.3 Instrumental parameters ....................................................................................... 16

8.3.1 GC-MS method .............................................................................................. 16

8.3.2 Py/TD-GC-MS method ................................................................................... 18

8.4 Calibrants ............................................................................................................. 18

8.5 Calibration ............................................................................................................ 19

8.5.1 GC-MS method .............................................................................................. 19

8.5.2 Py/TD-GC-MS method ................................................................................... 20

9 Calculation of phthalate concentration ........................................................................... 21

9.1 GC-MS method ..................................................................................................... 21

9.2 Py/TD-GC-MS method .......................................................................................... 22

10 Precision ....................................................................................................................... 23

10.1 GC-MS method ..................................................................................................... 23

10.1.1 Threshold judgement ..................................................................................... 23

10.1.2 Repeatability and reproducibility .................................................................... 24

10.2 Py/TD-GC-MS method .......................................................................................... 25

10.2.1 Screening judgement ..................................................................................... 25

10.2.2 Repeatability and reproducibility .................................................................... 26

11 Quality assurance and control ....................................................................................... 27

11.1 General ................................................................................................................. 27

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SIST EN 62321-8:2017
IEC 62321-8:2017 © IEC 2017 – 3 –

11.2 GC-MS method ..................................................................................................... 27

11.2.1 Performance .................................................................................................. 27

11.2.2 Limit of detection (LOD) or method detection limit (MDL) and limit of

quantification (LOQ) ...................................................................................... 28

11.3 Py/TD-GC-MS method .......................................................................................... 29

11.3.1 Sensitivity ...................................................................................................... 29

11.3.2 Blank test ...................................................................................................... 29

11.3.3 Limit of detection (LOD) or method detection limit (MDL) and limit of

quantification (LOQ) ...................................................................................... 29

12 Test report ..................................................................................................................... 30

Annex A (informative) Determination of phthalates in polymers by ion attachment

mass spectrometry (IAMS) .................................................................................................... 31

A.1 Principle ............................................................................................................... 31

A.2 Reagents and materials ........................................................................................ 31

A.3 Apparatus ............................................................................................................. 31

A.4 Sampling............................................................................................................... 32

A.5 Procedure ............................................................................................................. 32

A.5.1 General instructions for the analysis .............................................................. 32

A.5.2 Sample preparation ....................................................................................... 32

A.5.3 Instrumental parameters ................................................................................ 33

A.5.4 Calibrants ...................................................................................................... 34

A.5.5 Calibration ..................................................................................................... 34

A.6 Calculation of phthalates concentration ................................................................. 35

A.7 Quality assurance and control ............................................................................... 35

A.7.1 General ......................................................................................................... 35

A.7.2 Sensitivity ...................................................................................................... 35

A.7.3 Recovery ....................................................................................................... 35

A.7.4 Blank test ...................................................................................................... 36

A.7.5 Limit of detection (LOD) or method detection limit (MDL) and limit of

quantification (LOQ) ...................................................................................... 37

A.8 Test report ............................................................................................................ 37

Annex B (informative) Determination of phthalates in polymers by liquid

chromatography-mass spectrometry(LC-MS) ........................................................................ 38

B.1 Principle ............................................................................................................... 38

B.2 Reagents and materials ........................................................................................ 38

B.3 Apparatus ............................................................................................................. 38

B.4 Sampling............................................................................................................... 39

B.5 Procedure ............................................................................................................. 39

B.5.1 General instructions for the analysis .............................................................. 39

B.5.2 Sample preparation ....................................................................................... 39

B.5.3 Instrumental parameters ................................................................................ 40

B.5.4 Calibrants ...................................................................................................... 42

B.5.5 Calibration ..................................................................................................... 42

B.6 Calculation of phthalates concentration ................................................................. 43

B.7 Quality assurance and control ............................................................................... 44

B.7.1 General ......................................................................................................... 44

B.7.2 Performance .................................................................................................. 44

B.7.3 Limit of detection (LOD) or method detection limit (MDL) and limit of

quantification (LOQ) ...................................................................................... 44

B.8 Test report ............................................................................................................ 45

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SIST EN 62321-8:2017
– 4 – IEC 62321-8:2017 © IEC 2017

Annex C (informative) Examples of chromatograms at suggested conditions ....................... 46

C.1 GC-MS method ..................................................................................................... 46

C.2 Py/TD-GC-MS method .......................................................................................... 47

C.3 LC-MS method ...................................................................................................... 47

C.4 IAMS method ........................................................................................................ 48

Annex D (informative) Verification of the EGA thermal desorption zone ............................... 51

Annex E (informative) Example of IAMS and Py/TD-GC-MS instruments .............................. 52

Annex F (informative) Example of false positive detection of phthalates ............................... 54

Annex G (informative) Examples of sample preparation for quantitative analysis of

phthalates by GC-MS ............................................................................................................ 55

G.1 General ................................................................................................................. 55

G.2 Soxhlet extraction of phthalates using proper organic solvents ............................. 55

Annex H (informative) Extraction of phthalates by dissolution in THF using sonication

and precipitation of polymer matrix ....................................................................................... 58

Annex I (informative) Commercially available reference materials considered suitable

for GC-MS and Py/TD-GC-MS............................................................................................... 60

I.1 GC-MS .................................................................................................................. 60

I.2 Py/TD-GC-MS ....................................................................................................... 60

Annex J (informative) Commercially available capillary columns considered suitable

for GC-MS and Py-GC-MS .................................................................................................... 62

Annex K (informative) Labware cleaning procedure for phthalate testing .............................. 63

K.1 With the use of a furnace (non-volumetric glassware only) .................................... 63

K.2 Without the use of a furnace (glassware and plastic-ware) .................................... 63

K.3 Estimation of cleanness of the inner areas of volumetric glassware ...................... 64

Annex L (informative) Results of international inter-laboratory study 5 ................................. 65

Annex M (informative) Sample analysis sequence ................................................................ 70

M.1 GC-MS .................................................................................................................. 70

Annex N (informative) Flow chart ......................................................................................... 71

Bibliography .......................................................................................................................... 72

Figure C.1 – Total ion current chromatogram of each phthalate (10 µg/ml, 1 µl,

splitless) ............................................................................................................................... 46

Figure C.2 – Extracted ion chromatogram of DINP (10 µg/ml, 1 µl, splitless) ......................... 46

Figure C.3 – Extracted ion chromatogram of DIDP (10 µg/ml, 1 µl, splitless) ......................... 47

Figure C.4 – Total ion current chromatogram of 100 µg/ml of phthalate mixture by

Py/TD-GC-MS ....................................................................................................................... 47

Figure C.5 – Total ion current chromatogram of 5 µg/ml of phthalate mixture by LC-MS ........ 48

Figure C.6 – Mass spectrum of each phthalate by IAMS ....................................................... 49

Figure C.7 – Total ion current chromatogram of each absolute amount (0,08 µg) of

phthalate mixture by IAMS .................................................................................................... 50

Figure C.8 – Total ion current chromatogram of approximately 0,3 mg of PVC which

contains 300 mg/kg of each phthalate mixture by IAMS (Absolute amount: 0,09 µg) ............. 50

Figure D.1 – Example of EGA thermogram of a PVC sample containing phthalates ............... 51

Figure E.1 – Example of IAMS instrument ............................................................................. 52

Figure E.2 – Example of Py/TD-GC-MS instrument ............................................................... 53

Figure F.1 – Typical laboratory wares made of plastic materials that may cause

phthalate contamination ........................................................................................................ 54

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SIST EN 62321-8:2017
IEC 62321-8:2017 © IEC 2017 – 5 –

Figure F.2 – Example of a chromatogram of a blank solvent (THF) in a plastic bottle

showing DEHP contamination. .............................................................................................. 54

Figure G.1 – Recovery ratios of Di-(2-ethylhexyl) phthalate using Soxhlet extraction

with different organic solvents ............................................................................................... 57

Figure G.2 – Comparison of recovery ratios of phthalates using different extracting

conditions ............................................................................................................................. 57

Figure I.1 – Sample preparation of reference materials ......................................................... 61

Figure N.1 – Flow chart for screening step and quantitative step .......................................... 71

Table 1 – Measurement condition of GC-MS ......................................................................... 17

Table 2 – Reference masses for the quantification of each phthalate .................................... 17

Table 3 – Measurement condition of Py/TD-GC-MS .............................................................. 18

Table 4 – Calibration standard solution of phthalates ............................................................ 19

Table 5 – IIS5 Threshold judgement...................................................................................... 23

Table 6 – IIS5 Repeatability and reproducibility .................................................................... 24

Table 7 – IIS5 screening and threshold judgement ................................................................ 25

Table 8 – IIS5 Repeatability and reproducibility .................................................................... 26

Table A.1 – Measurement condition of IAMS ......................................................................... 34

Table A.2 – Certified value of constituent phthalates in KRISS CRM 113-03-006 ................. 36

Table B.1 – Measurement condition of LC-MS ...................................................................... 42

Table B.2 – Standard stock solution concentrations .............................................................. 43

Table G.1 – Recovery ratios of phthalates according to different Soxhlet extraction

times (extracting solvent: n-hexane) ..................................................................................... 56

Table H.1 – Comparison of the efficiency of the sample preparation method of

dissolution in THF using sonication and precipitation of polymeric matrix with that of

Soxhlet extraction for soluble sample .................................................................................... 58

Table H.2 – Comparison of the efficiency of the sample preparation method of

dissolution in THF using sonication and precipitation of polymeric matrix with that of

Soxhlet extraction for insoluble samples ............................................................................... 59

Table I.1 – Example list of commercially available reference solutions considered

suitable for GC-MS ............................................................................................................... 60

Table I.2 – Example list of commercially available reference materials considered

suitable for Py/TD-GC-MS..................................................................................................... 61

Table J.1 – Example list of commercially available capillary columns considered

suitable for GC-MS and Py-GC-MS analysis ......................................................................... 62

Table L.1 – Statistical data for Py/TD-GC-MS ....................................................................... 65

Table L.2 – Statistical data for GC-MS .................................................................................. 67

Table L.3 – Statistical data for IAMS ..................................................................................... 68

Table L.4 – Statistical Data For LC-MS ................................................................................. 69

Table M.1 – Sample analysis sequence for GC-MS analysis ................................................. 70

Table M.2 – Sample analysis sequence for Py/TD-GC-MS analysis ...................................... 70

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SIST EN 62321-8:2017
– 6 – IEC 62321-8:2017 © IEC 2017
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
DETERMINATION OF CERTAIN SUBSTANCES
IN ELECTROTECHNICAL PRODUCTS –
Part 8: Phthalates in polymers by gas chromatography-mass spectrometry
(GC-MS), gas chromatography-mass spectrometry using
a pyrolyzer/thermal desorption accessory (Py/TD-GC-MS)
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

...

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