ISO 3749:2022

Glass syringes — Determination of extractable tungsten

This document specifies an analytical method to quantitatively determine the water-soluble amount of tungsten (W) from the inner surface of glass syringes. The method can be applied to Luer cone, staked needle or Luer lock syringes.

Seringues en verre — Dosage du tungstène extractible

General Information

• Status: Published
• Publication Date: 08-Mar-2022
• ICS: 11.040.25 - Syringes, needles an catheters
• Technical Committee: ISO/TC 76 - Transfusion, infusion and injection, and blood processing equipment for medical and pharmaceutical use
• Drafting Committee: ISO/TC 76/WG 2 - Rigid container systems and related accessories for parenterals and injectables
• Current Stage: 6060 - International Standard published
• Start Date: 09-Mar-2022
• Due Date: 10-Jan-2023
• Completion Date: 09-Mar-2022

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 3749
First edition
2022-03
Glass syringes — Determination of
extractable tungsten
Seringues en verre — Dosage du tungstène extractible
Reference number
ISO 3749:2022(E)
© ISO 2022

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ISO 3749:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022
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: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii
  © ISO 2022 – All rights reserved

---------------------- Page: 2 ----------------------
ISO 3749:2022(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 1
6 Apparatus . 2
7 Sample preparation .2
7.1 General . 2
7.2 Siliconization . 2
7.3 Filling . 3
7.3.1 General . 3
7.3.2 Determination of the filling level . 3
7.3.3 Filling of the syringes to be tested . 4
8 Extraction by ultrasonics . 4
9 Analysis . . 5
9.1 General . 5
9.2 ICP-MS . 5
9.3 ICP-OES . 5
9.4 Quality control . 5
9.4.1 Measurement with ICP-MS or ICP-OES . 5
9.4.2 Extraction efficiency . 5
9.5 Expression of the results . 5
10 Test report . 6
Annex A (informative) Spiking of syringes . 7
iii
© ISO 2022 – All rights reserved

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ISO 3749:2022(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 Technical Committee ISO/TC 76, Transfusion, infusion and injection, and
blood processing equipment for medical and pharmaceutical use.
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 2022 – All rights reserved

---------------------- Page: 4 ----------------------
ISO 3749:2022(E)
Introduction
Glass syringes are typically produced from glass tubing via a hot-forming process.
One important step of this process is the cone formation and more importantly its opening with a pin
that has the form of a filament and that is made of material resistant to high temperatures such as
ceramics, tungsten and other.
This process is valid for the different syringe cone configurations such as Luer cone, Luer lock and also
for staked needle syringes.
In the case of tungsten pins, tungsten residuals will form on the inner surface of the cone. These
residues can affect the effectivity of the drug product e.g. causing aggregation of protein-based drugs.
For this reason, the level of soluble tungsten residues needs to be controlled in certain applications.
v
© ISO 2022 – All rights reserved

---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 3749:2022(E)
Glass syringes — Determination of extractable tungsten
1 Scope
This document specifies an analytical method to quantitatively determine the water-soluble amount of
tungsten (W) from the inner surface of glass syringes.
The method can be applied to Luer cone, staked needle or Luer lock syringes.
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 3696, Water for analytical laboratory use — Specification and test methods
ISO 11885, Water quality — Determination of selected elements by inductively coupled plasma optical
emission spectrometry (ICP-OES)
ISO 17294-2, Water quality — Application of inductively coupled plasma mass spectrometry (ICP-MS) —
Part 2: Determination of selected elements including uranium isotopes
3 Terms and definitions
No terms and definitions are listed in this document.
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 Principle
This test method is intended to be used to determine the water-soluble tungsten content of glass
syringes as produced and/or as delivered. The syringes to be tested are filled with water to their
nominal volume. They are tightly capped and then extracted by ultrasonic treatment [(75 ± 5 )°C,
...

FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 3749
ISO/TC 76
Glass syringes — Determination of
Secretariat: DIN
extractable tungsten
Voting begins on:
2021-11-12
Voting terminates on:
2022-01-07
RECIPIENTS OF THIS DRAFT ARE INVITED TO
SUBMIT, WITH THEIR COMMENTS, NOTIFICATION
OF ANY RELEVANT PATENT RIGHTS OF WHICH
THEY ARE AWARE AND TO PROVIDE SUPPOR TING
DOCUMENTATION.
IN ADDITION TO THEIR EVALUATION AS
Reference number
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
ISO/FDIS 3749:2021(E)
LOGICAL, COMMERCIAL AND USER PURPOSES,
DRAFT INTERNATIONAL STANDARDS MAY ON
OCCASION HAVE TO BE CONSIDERED IN THE
LIGHT OF THEIR POTENTIAL TO BECOME STAN-
DARDS TO WHICH REFERENCE MAY BE MADE IN
NATIONAL REGULATIONS. © ISO 2021

---------------------- Page: 1 ----------------------
ISO/FDIS 3749:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021
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: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii
  © ISO 2021 – All rights reserved

---------------------- Page: 2 ----------------------
ISO/FDIS 3749:2021(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 1
6 Apparatus . 2
7 Sample preparation .2
7.1 General . 2
7.2 Siliconization . 2
7.3 Filling . 3
7.3.1 General . 3
7.3.2 Determination of the filling level . 3
7.3.3 Filling of the syringes to be tested . 4
8 Extraction . 4
8.1 Extraction by ultrasonics . 4
9 Analysis . . 5
9.1 General . 5
9.2 ICP-MS . 5
9.3 ICP-OES . 5
9.4 Quality control . 5
9.4.1 Measurement with ICP-MS or ICP-OES . 5
9.4.2 Extraction efficiency . 5
9.5 Expression of the results . 5
10 Test report . 6
Annex A (informative) Spiking of syringes . 7
iii
© ISO 2021 – All rights reserved

---------------------- Page: 3 ----------------------
ISO/FDIS 3749:2021(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 Technical Committee ISO/TC 76, Transfusion, infusion and injection, and
blood processing equipment for medical and pharmaceutical use.
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 2021 – All rights reserved

---------------------- Page: 4 ----------------------
ISO/FDIS 3749:2021(E)
Introduction
Glass syringes are typically produced from glass tubing via a hot-forming process.
One important step of this process is the cone formation and more importantly its opening with a pin
that has the form of a filament and that is made of material resistant to high temperatures such as
ceramics, tungsten and other.
This process is valid for the different syringe cone configurations such as Luer cone, Luer lock and also
for staked needle syringes.
In the case of tungsten pins, tungsten residuals will form on the inner surface of the cone. These
residues can affect the effectivity of the drug product (e.g. causing aggregation of protein-based drugs).
For this reason, the level of soluble tungsten residues needs to be controlled in certain applications.
v
© ISO 2021 – All rights reserved

---------------------- Page: 5 ----------------------
FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 3749:2021(E)
Glass syringes — Determination of extractable tungsten
1 Scope
This document specifies an analytical method to quantitatively determine the water-soluble amount of
tungsten (W) from the inner surface of glass syringes.
The method can be applied to Luer cone, staked needle or Luer lock syringes.
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 3696, Water for analytical laboratory use — Specification and test methods
ISO 17294-2, Water quality — Application of inductively coupled plasma mass spectrometry (ICP-MS) —
Part 2: Determination of selected elements including uranium isotopes
ISO 11885, Water quality — Determination of selected elements by inductively coupled plasma optical
emission spectrometry (ICP-OES)
3 Terms and definitions
No terms and definitions are listed in this document.
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
...