Leather - Chemical tests - Determination of pesticide residues content (ISO 22517:2019)

This document specifies a quantitative test method to determine 24 kinds of pesticide residues in leather by gas chromatography-mass spectrometry (GC-MS).This document is applicable to all types of leather that could release pesticides

Leder - Chemische Prüfungen - Bestimmung des Pestizidrückstandsgehalts (ISO 22517:2019)

Dieses Dokument legt ein quantitatives Prüfverfahren zur Bestimmung von 24 Arten von Pestizidrückständen in Leder mittels Gaschromatographie-Massenspektrometrie (GC MS) fest.
Dieses Dokument ist anzuwenden für alle Lederarten, die Pestizide freisetzen könnten.

Cuir - Essais chimiques - Détermination de la teneur en résidus de pesticides (ISO 22517:2019)

Usnje - Kemični preskusi - Določevanje ostankov pesticidov (ISO 22517:2019)

General Information

Status
Published
Public Enquiry End Date
02-May-2021
Publication Date
29-Aug-2021
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
25-Aug-2021
Due Date
30-Oct-2021
Completion Date
30-Aug-2021

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SLOVENSKI STANDARD
SIST EN ISO 22517:2021
01-oktober-2021
Usnje - Kemični preskusi - Določevanje ostankov pesticidov (ISO 22517:2019)

Leather - Chemical tests - Determination of pesticide residues content (ISO 22517:2019)

Leder - Chemische Prüfungen - Bestimmung des Pestizidrückstandsgehalts (ISO
22517:2019)

Cuir - Essais chimiques - Détermination de la teneur en résidus de pesticides (ISO

22517:2019)
Ta slovenski standard je istoveten z: EN ISO 22517:2021
ICS:
59.140.30 Usnje in krzno Leather and furs
65.100.99 Drugi pesticidi in Other pesticides and
agrokemikalije agrochemicals
SIST EN ISO 22517:2021 en,fr,de

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

---------------------- Page: 1 ----------------------
SIST EN ISO 22517:2021
---------------------- Page: 2 ----------------------
SIST EN ISO 22517:2021
EN ISO 22517
EUROPEAN STANDARD
NORME EUROPÉENNE
August 2021
EUROPÄISCHE NORM
ICS 59.140.30
English Version
Leather - Chemical tests - Determination of pesticide
residues content (ISO 22517:2019)

Cuir - Essais chimiques - Détermination de la teneur en Leder - Chemische Prüfungen - Bestimmung des

résidus de pesticides (ISO 22517:2019) Pestizidrückstandsgehalts (ISO 22517:2019)

This European Standard was approved by CEN on 9 August 2021.

CEN 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 CEN

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 CEN member into its own language and notified to the CEN-CENELEC Management

Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 22517:2021 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN ISO 22517:2021
EN ISO 22517:2021 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

---------------------- Page: 4 ----------------------
SIST EN ISO 22517:2021
EN ISO 22517:2021 (E)
European foreword

The text of ISO 22517:2019 has been prepared by Technical Committee ISO/IULTCS "International

Union of Leather Technologists and Chemists Societies” of the International Organization for

Standardization (ISO) and has been taken over as EN ISO 22517:2021 by Technical Committee CEN/TC

289 “Leather” the secretariat of which is held by UNI.

This European Standard shall be given the status of a national standard, either by publication of an

identical text or by endorsement, at the latest by February 2022, and conflicting national standards

shall be withdrawn at the latest by February 2022.

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

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

Any feedback and questions on this document should be directed to the users’ national standards body.

A complete listing of these bodies can be found on the CEN website.

According to the CEN-CENELEC Internal Regulations, the national standards organizations of the

following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,

Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,

Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of

North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the

United Kingdom.
Endorsement notice

The text of ISO 22517:2019 has been approved by CEN as EN ISO 22517:2021 without any modification.

---------------------- Page: 5 ----------------------
SIST EN ISO 22517:2021
---------------------- Page: 6 ----------------------
SIST EN ISO 22517:2021
INTERNATIONAL ISO
STANDARD 22517
IULTCS/IUC 38
First edition
2019-05
Leather — Chemical tests —
Determination of pesticide residues
content
Cuir — Essais chimiques — Détermination de la teneur en résidus de
pesticides
Reference numbers
ISO 22517:2019(E)
IULTCS/IUC 38:2019(E)
ISO 2019
---------------------- Page: 7 ----------------------
SIST EN ISO 22517:2021
ISO 22517:2019(E)
IULTCS/IUC 38:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved
---------------------- Page: 8 ----------------------
SIST EN ISO 22517:2021
ISO 22517:2019(E)
IULTCS/IUC 38:2019(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 1

5 Safety precautions .............................................................................................................................................................................................. 1

6 Reagents ........................................................................................................................................................................................................................ 2

7 Apparatus ..................................................................................................................................................................................................................... 2

8 Procedure..................................................................................................................................................................................................................... 3

8.1 Sample ............................................................................................................................................................................................................ 3

8.2 Extraction .................................................................................................................................................................................................... 3

8.3 Purification ................................................................................................................................................................................................. 3

8.4 Calibration solutions .......................................................................................................................................................................... 4

8.4.1 Preparation of calibration solution mixture ............................................................................................ 4

8.4.2 Preparation of calibration mixture for recovery rate ....................................................................... 4

8.5 Preparation of blank sample ....................................................................................................................................................... 4

8.6 Analysis by GC-MS ................................................................................................................................................................................ 4

8.7 Check of the analytical system ................................................................................................................................................... 4

9 E valuation of results ......................................................................................................................................................................................... 5

9.1 Calculation of results ......................................................................................................................................................................... 5

9.2 Reliability of the method ................................................................................................................................................................ 5

10 Test report ................................................................................................................................................................................................................... 5

Annex A (normative) 24 kinds of pesticide compounds .................................................................................................................. 6

Annex B (informative) GC-MS chromatographic conditions and parameters............................................................7

Annex C (informative) Retention time, quantitative and qualitative ions and ion abundance

ratios ................................................................................................................................................................................................................................. 8

Annex D (informative) Start time and dwell time of each group of detecting ions...............................................9

Annex E (informative) Chromatogram and selected ion of the 24 pesticides standard

obtained by GC-MS ...........................................................................................................................................................................................10

Annex F (informative) Recovery range of pesticides in leather (n = 6) .........................................................................11

Annex G (informative) Precision ............................................................................................................................................................................13

Bibliography .............................................................................................................................................................................................................................15

© ISO 2019 – All rights reserved iii
---------------------- Page: 9 ----------------------
SIST EN ISO 22517:2021
ISO 22517:2019(E)
IULTCS/IUC 38:2019(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/directives).

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

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso

.org/iso/foreword .html.

This document was prepared by the Chemical Tests Commission of the International Union of Leather

Technologists and Chemists Societies (IUC Commission, IULTCS) in collaboration with the European

Committee for Standardization (CEN) Technical Committee CEN/TC 289, Leather, the secretariat of

which is held by UNI, in accordance with the Agreement on technical cooperation between ISO and CEN

(Vienna Agreement).

IULTCS, originally formed in 1897, is a world-wide organization of professional leather societies to

further the advancement of leather science and technology. IULTCS has three Commissions, which

are responsible for establishing international methods for the sampling and testing of leather. ISO

recognizes IULTCS as an international standardizing body for the preparation of test methods for

leather.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/members .html.
iv © ISO 2019 – All rights reserved
---------------------- Page: 10 ----------------------
SIST EN ISO 22517:2021
ISO 22517:2019(E)
INTERNATIONAL STANDARD
IULTCS/IUC 38:2019(E)
Leather — Chemical tests — Determination of pesticide
residues content
1 Scope

This document specifies a quantitative test method to determine 24 kinds of pesticide residues in

leather by gas chromatography-mass spectrometry (GC-MS).

This document is applicable to all types of leather that could release pesticides.

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 2418, Leather — Chemical, physical and mechanical and fastness tests — Sampling location

ISO 4044, Leather — Chemical tests — Preparation of chemical test samples
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
4 Principle

The leather sample is ultrasonically extracted with a mixed solution of n-hexane and ethyl acetate

(1 + 1, volume). The extraction is detected and confirmed by GC-MS, and quantified using an external

standard method.
5 Safety precautions

5.1 The compounds of pesticides are classified as high toxicity substances. Some are persistent organic

pollutants (POPs) and suspected to be human carcinogens.

Any handling and disposal of these substances shall be in strict accordance with the applicable health

and safety requirements.

5.2 It is the user's responsibility to use safe and proper techniques when handling materials in

this test method. Consult manufacturers for specific details, such as safety data sheets and other

recommendations.

5.3 Good laboratory practice should be followed. Wear safety glasses in all laboratory areas, as well as

a dust respirator and single-use gloves while handling those compounds and leather samples.

© ISO 2019 – All rights reserved 1
---------------------- Page: 11 ----------------------
SIST EN ISO 22517:2021
ISO 22517:2019(E)
IULTCS/IUC 38:2019(E)
6 Reagents
Unless otherwise specified, analytical grade chemicals shall be used.
6.1 n-Hexane, chromatographic pure.
6.2 Ethyl acetate, chromatographic pure.
6.3 Acetonitrile, chromatographic pure.
6.4 Toluene, chromatographic pure.
6.5 n-Hexane and ethyl acetate (1 + 1, volume) mixed solution.
6.6 Acetonitrile and toluene (3 + 1, volume) mixed solution.

6.7 24 kinds of pesticide standards, as listed in Annex A, purity of 97 % or more. See Annex A for

individual details of the 24 pesticide compounds.

6.8 Standard solutions of pesticides, accurately weigh the amount of each pesticide standard, and

dissolve in a small amount of n-hexane to prepare a concentration 100 μg/ml of standard solution. A

commercially available certified solution is an alternative. The shelf life of commercially available certified

solution is given in the certificate. The shelf life of the solution prepared from powder is one month.

6.9 Standard stock solutions of pesticides, accurately pipette a certain volume of each standard

pesticide solution (6.8) into a separate volumetric flask. Dilute with n-hexane to prepare the intermediate

standard stock solution with a concentration of 1 μg/ml. The shelf life of the stock solution is one month.

6.10 Standard calibration solutions of pesticides, accurately pipette a certain volume of standard

stock solution (6.9) into a volumetric flask and dilute with n-hexane to prepare standard calibration

solutions with concentrations in the range of 10 ng/ml to 1 000 ng/ml. Prepare them before using.

7 Apparatus
Usual laboratory equipment and, in particular, the following.

7.1 Gas chromatograph (GC), with mass-selective detector (MSD) and electron impact source (EIS).

7.2 Analytical balance, weighing to an accuracy of 0,1 mg.
7.3 Laboratory balance, weighing to an accuracy of 0,01 g.
7.4 Vortex mixer.

7.5 Ultrasonic water-bath, ultrasonic frequency 40 KHz, ultrasonic power 200 W, controllable

heating.

7.6 Vacuum rotary evaporator, with vacuum control and water bath. Other types of evaporation

apparatus may be used, e.g. a water bath with a controlled flow of nitrogen over the liquid.

7.7 Solid phase extraction (SPE) system, with vacuum device and graphitized carbon black (Carb),

solid phase extraction column, 500 mg, 6 ml.
2 © ISO 2019 – All rights reserved
---------------------- Page: 12 ----------------------
SIST EN ISO 22517:2021
ISO 22517:2019(E)
IULTCS/IUC 38:2019(E)
7.8 Small volume pipetting device, 1 ml to 5 ml, and 100 μl to 1 000 μl.
7.9 Centrifuge, with a revolution speed of more than 5 000 r/min.
7.10 Stoppered polypr
...

SLOVENSKI STANDARD
oSIST prEN ISO 22517:2021
01-april-2021
Usnje - Kemični preskusi - Določevanje ostankov pesticidov (ISO 22517:2019)

Leather - Chemical tests - Determination of pesticide residues content (ISO 22517:2019)

Cuir - Essais chimiques - Détermination de la teneur en résidus de pesticides (ISO

22517:2019)
Ta slovenski standard je istoveten z: prEN ISO 22517
ICS:
59.140.30 Usnje in krzno Leather and furs
65.100.99 Drugi pesticidi in Other pesticides and
agrokemikalije agrochemicals
oSIST prEN ISO 22517:2021 en

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

---------------------- Page: 1 ----------------------
oSIST prEN ISO 22517:2021
---------------------- Page: 2 ----------------------
oSIST prEN ISO 22517:2021
INTERNATIONAL ISO
STANDARD 22517
IULTCS/IUC 38
First edition
2019-05
Leather — Chemical tests —
Determination of pesticide residues
content
Cuir — Essais chimiques — Détermination de la teneur en résidus de
pesticides
Reference numbers
ISO 22517:2019(E)
IULTCS/IUC 38:2019(E)
ISO 2019
---------------------- Page: 3 ----------------------
oSIST prEN ISO 22517:2021
ISO 22517:2019(E)
IULTCS/IUC 38:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved
---------------------- Page: 4 ----------------------
oSIST prEN ISO 22517:2021
ISO 22517:2019(E)
IULTCS/IUC 38:2019(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 1

5 Safety precautions .............................................................................................................................................................................................. 1

6 Reagents ........................................................................................................................................................................................................................ 2

7 Apparatus ..................................................................................................................................................................................................................... 2

8 Procedure..................................................................................................................................................................................................................... 3

8.1 Sample ............................................................................................................................................................................................................ 3

8.2 Extraction .................................................................................................................................................................................................... 3

8.3 Purification ................................................................................................................................................................................................. 3

8.4 Calibration solutions .......................................................................................................................................................................... 4

8.4.1 Preparation of calibration solution mixture ............................................................................................ 4

8.4.2 Preparation of calibration mixture for recovery rate ....................................................................... 4

8.5 Preparation of blank sample ....................................................................................................................................................... 4

8.6 Analysis by GC-MS ................................................................................................................................................................................ 4

8.7 Check of the analytical system ................................................................................................................................................... 4

9 E valuation of results ......................................................................................................................................................................................... 5

9.1 Calculation of results ......................................................................................................................................................................... 5

9.2 Reliability of the method ................................................................................................................................................................ 5

10 Test report ................................................................................................................................................................................................................... 5

Annex A (normative) 24 kinds of pesticide compounds .................................................................................................................. 6

Annex B (informative) GC-MS chromatographic conditions and parameters............................................................7

Annex C (informative) Retention time, quantitative and qualitative ions and ion abundance

ratios ................................................................................................................................................................................................................................. 8

Annex D (informative) Start time and dwell time of each group of detecting ions...............................................9

Annex E (informative) Chromatogram and selected ion of the 24 pesticides standard

obtained by GC-MS ...........................................................................................................................................................................................10

Annex F (informative) Recovery range of pesticides in leather (n = 6) .........................................................................11

Annex G (informative) Precision ............................................................................................................................................................................13

Bibliography .............................................................................................................................................................................................................................15

© ISO 2019 – All rights reserved iii
---------------------- Page: 5 ----------------------
oSIST prEN ISO 22517:2021
ISO 22517:2019(E)
IULTCS/IUC 38:2019(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/directives).

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

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso

.org/iso/foreword .html.

This document was prepared by the Chemical Tests Commission of the International Union of Leather

Technologists and Chemists Societies (IUC Commission, IULTCS) in collaboration with the European

Committee for Standardization (CEN) Technical Committee CEN/TC 289, Leather, the secretariat of

which is held by UNI, in accordance with the Agreement on technical cooperation between ISO and CEN

(Vienna Agreement).

IULTCS, originally formed in 1897, is a world-wide organization of professional leather societies to

further the advancement of leather science and technology. IULTCS has three Commissions, which

are responsible for establishing international methods for the sampling and testing of leather. ISO

recognizes IULTCS as an international standardizing body for the preparation of test methods for

leather.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/members .html.
iv © ISO 2019 – All rights reserved
---------------------- Page: 6 ----------------------
oSIST prEN ISO 22517:2021
ISO 22517:2019(E)
INTERNATIONAL STANDARD
IULTCS/IUC 38:2019(E)
Leather — Chemical tests — Determination of pesticide
residues content
1 Scope

This document specifies a quantitative test method to determine 24 kinds of pesticide residues in

leather by gas chromatography-mass spectrometry (GC-MS).

This document is applicable to all types of leather that could release pesticides.

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 2418, Leather — Chemical, physical and mechanical and fastness tests — Sampling location

ISO 4044, Leather — Chemical tests — Preparation of chemical test samples
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
4 Principle

The leather sample is ultrasonically extracted with a mixed solution of n-hexane and ethyl acetate

(1 + 1, volume). The extraction is detected and confirmed by GC-MS, and quantified using an external

standard method.
5 Safety precautions

5.1 The compounds of pesticides are classified as high toxicity substances. Some are persistent organic

pollutants (POPs) and suspected to be human carcinogens.

Any handling and disposal of these substances shall be in strict accordance with the applicable health

and safety requirements.

5.2 It is the user's responsibility to use safe and proper techniques when handling materials in

this test method. Consult manufacturers for specific details, such as safety data sheets and other

recommendations.

5.3 Good laboratory practice should be followed. Wear safety glasses in all laboratory areas, as well as

a dust respirator and single-use gloves while handling those compounds and leather samples.

© ISO 2019 – All rights reserved 1
---------------------- Page: 7 ----------------------
oSIST prEN ISO 22517:2021
ISO 22517:2019(E)
IULTCS/IUC 38:2019(E)
6 Reagents
Unless otherwise specified, analytical grade chemicals shall be used.
6.1 n-Hexane, chromatographic pure.
6.2 Ethyl acetate, chromatographic pure.
6.3 Acetonitrile, chromatographic pure.
6.4 Toluene, chromatographic pure.
6.5 n-Hexane and ethyl acetate (1 + 1, volume) mixed solution.
6.6 Acetonitrile and toluene (3 + 1, volume) mixed solution.

6.7 24 kinds of pesticide standards, as listed in Annex A, purity of 97 % or more. See Annex A for

individual details of the 24 pesticide compounds.

6.8 Standard solutions of pesticides, accurately weigh the amount of each pesticide standard, and

dissolve in a small amount of n-hexane to prepare a concentration 100 μg/ml of standard solution. A

commercially available certified solution is an alternative. The shelf life of commercially available certified

solution is given in the certificate. The shelf life of the solution prepared from powder is one month.

6.9 Standard stock solutions of pesticides, accurately pipette a certain volume of each standard

pesticide solution (6.8) into a separate volumetric flask. Dilute with n-hexane to prepare the intermediate

standard stock solution with a concentration of 1 μg/ml. The shelf life of the stock solution is one month.

6.10 Standard calibration solutions of pesticides, accurately pipette a certain volume of standard

stock solution (6.9) into a volumetric flask and dilute with n-hexane to prepare standard calibration

solutions with concentrations in the range of 10 ng/ml to 1 000 ng/ml. Prepare them before using.

7 Apparatus
Usual laboratory equipment and, in particular, the following.

7.1 Gas chromatograph (GC), with mass-selective detector (MSD) and electron impact source (EIS).

7.2 Analytical balance, weighing to an accuracy of 0,1 mg.
7.3 Laboratory balance, weighing to an accuracy of 0,01 g.
7.4 Vortex mixer.

7.5 Ultrasonic water-bath, ultrasonic frequency 40 KHz, ultrasonic power 200 W, controllable

heating.

7.6 Vacuum rotary evaporator, with vacuum control and water bath. Other types of evaporation

apparatus may be used, e.g. a water bath with a controlled flow of nitrogen over the liquid.

7.7 Solid phase extraction (SPE) system, with vacuum device and graphitized carbon black (Carb),

solid phase extraction column, 500 mg, 6 ml.
2 © ISO 2019 – All rights reserved
---------------------- Page: 8 ----------------------
oSIST prEN ISO 22517:2021
ISO 22517:2019(E)
IULTCS/IUC 38:2019(E)
7.8 Small volume pipetting device, 1 ml to 5 ml, and 100 μl to 1 000 μl.
7.9 Centrifuge, with a revolution speed of more than 5 000 r/min.
7.10 Stoppered polypropylene centrifuge tube, 50 ml.
7.11 Conical flask, brown, 100 ml.
7.12 Polypropylene or polyethylene syringe, 50 ml.
7.13 Polyamide membrane filter, 0,22 μm or 0,45 μm.
8 Procedure
8.1 Sample

Sample the leather in accordance with ISO 2418. If sampling in accordance with ISO 2418 is not possible

(e.g. leather from finished products like shoes, garments, etc.), details about sampling shall be given in

the test report.

Cut the leather sample into small pieces or grind the leather in accordance with ISO 4044. The pieces

shall be of 3 mm to 5 mm side length.
8.2 Extraction

8.2.1 Weigh accurately 2,00 g leather sample (to 0,01 g accuracy) with a laboratory balance (7.3) and

place in 50 ml stoppered polypropylene centrifuge tube (7.10).

8.2.2 Add 20 ml of the n-hexane and ethyl acetate (1 + 1) mixed solution (6.5) into the tube, shake for

10 min with the vortex mixer (7.4).
8.2.3 Extract in the ultrasonic water-bath (7.5) for 20 min at 25 °C ± 2 °C.

8.2.4 Centrifuge for 5 min at 5 000 r/min with centrifuge (7.9). The supernatant is transferred to the

conical flask (7.11).

8.2.5 With the residue, carry out the operations in 8.2.2 to 8.2.4 for a second time. Combine the

supernatant in the conical flask.

8.2.6 Concentrate the combined extraction by a vacuum rotary evaporator (7.6) or under gentle flow

of nitrogen at 35 °C ± 5 °C to approximately 2 ml to 5 ml.
8.3 Purification

8.3.1 Pre-rinse the Carb (7.7) with 5 ml acetonitrile and toluene (3 + 1) mixed solution (6.6).

8.3.2 Transfer the extraction solution (8.2.6) to the Carb. Rinse the conical flask twice with 3 ml

acetonitrile and toluene (3 + 1) mixed solution (6.6) and transfer the washing solutions to the Carb.

8.3.3 Rinse the Carb with 15 ml acetonitrile and toluene (3 + 1) mixed solution (6.6), collecting all the

eluent in a clean conical flask (7.11).
© ISO 2019 – All rights reserved 3
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oSIST prEN ISO 22517:2021
ISO 22517:2019(E)
IULTCS/IUC 38:2019(E)

8.3.4 Evaporate the solution (8.3.3) to approximately 1 ml using a vacuum rotary evap

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