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Technical
Specification
ISO/TS 16465
First edition
Animal and vegetable fats and
2024-01
oils — Determination of phthalates
in vegetable oils
Corps gras d’origines animale et végétale — Dosage des phtalates
dans les huiles végétales
Reference number
© ISO 2024
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ii
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Part A - Determination of DEHP . 1
4.1 Principle .1
4.2 Reagents .1
4.3 Apparatus .3
4.4 Sampling .4
4.5 Preparation of the test sample .4
4.6 Procedure .4
4.6.1 Phthalates extraction from oil .4
4.6.2 Gas Chromatography .5
4.7 Quantitative determination .6
4.7.1 Calibration curve.6
4.7.2 Quantitative determination of DEHP .6
4.8 Precision of the method.7
4.8.1 Interlaboratory test .7
4.8.2 Repeatability .8
4.8.3 Reproducibility .8
4.9 Test report .8
5 Part B - Determination of eight phthalates. 8
5.1 Principle .8
5.2 Reagents .8
5.3 Apparatus .10
5.4 Sampling .11
5.5 Preparation of the test sample . 12
5.6 Procedure . 12
5.6.1 Phthalates extraction from oil . 12
5.6.2 Gas chromatography .16
5.7 Quantitative determination .17
5.7.1 Calibration curve.17
5.7.2 Quantitative determination of phthalate .18
5.8 Precision of the method.19
5.8.1 Interlaboratory test .19
5.8.2 Repeatability .19
5.8.3 Reproducibility .19
5.9 Test report .19
Annex A (informative) Results of an interlaboratory test — Part A - Determination of DEHP .20
Annex B (informative) Results of an interlaboratory test — Part B - Determination of eight
phthalates . .21
Bibliography .25
iii
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
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in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the different types
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This document was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 11, Animal
and vegetable fats and oils.
Any feedback or questions on this document should be directed to the user’s national standards body. A
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iv
Technical Specification ISO/TS 16465:2024(en)
Animal and vegetable fats and oils — Determination of
phthalates in vegetable oils
1 Scope
This document specifies two methods for the quantitative determination of phthalates in vegetable oils by
gas chromatography-mass spectrometry (GC-MS):
— Part A for the determination of di-2-ethylhexyl phthalate (DEHP).
— Part B for the determination of eight phthalates: dimethyl phthalate (DMP), diethyl phthalate (DEP),
di-isobutyl phthalate (DIBP), dibutyl phthalate (DBP), benzylbutyl phthalate (BBP), di-2-ethylhexyl
phthalate (DEHP), di-isononyl phthalate (DINP), di-isodecyl phthalate (DIDP).
Both methods are applicable for all vegetable oils, including crude, refined and virgin.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content constitutes
requirements 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.
ISO 661, Animal and vegetable fats and oils — Preparation of test sample
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
4 Part A - Determination of DEHP
4.1 Principle
Phthalates are first extracted from oil with acetonitrile followed by dispersive-solid-phase extraction
clean-up (dispersive SPE), which is done to remove organic acids, excess water and other components using
a combination of primary secondary amine (PSA) sorbent and C18 bonded phase. Finally, the extract is
concentrated and analysed by gas chromatography-mass spectrometry (GC-MS).
4.2 Reagents
WARNING — Attention is drawn to national regulations that specify the handling of hazardous
substances, and users' obligations thereunder. Technical, organizational and personal safety
measures shall be followed.
Unless otherwise specified, use only reagents of recognized analytical grade.
4.2.1 Toluene, purity 99 % min.
4.2.2 Acetonitrile, trace organic analysis grade, purity 99 % min.
4.2.3 n-Hexane, trace organic analysis grade, purity 99 % min.
1)
4.2.4 Chromabond adsorbent Diamino (PSA), Chromabond adsorbent C18 .
NOTE These powders can be sources of contamination. To remove the conta
...