prEN ISO 2613-2

Analysis of natural gas - Biomethane - Part 2: Determination of siloxane content by gas chromatography ion mobility spectrometry (ISO/DIS 2613-2:2023)

This document describes a Gas Chromatography Ion Mobility Spectroscopy (GC-IMS) method for the
determination of the concentration of siloxanes in biomethane and biogas. The method is applicable to
the siloxanes and working ranges provided in Table 1.
Table 1 — Component working ranges
Component Component abbreviation Lower limit (mg m-3) Upper limit (mg m-3)
hexamethyldisiloxane L2 0.1 10.0
octamethyltrisiloxane L3 0.1 10.0
decamethyltetrasiloxane L4 0.1 10.0
dodecamethylpentasiloxane L5 0.1 10.0
hexamethylcyclotrisiloxane D3 0.1 10.0
octamethylcyclotetrasiloxane D4 0.1 10.0
octamethylcyclotetrasiloxane D5 0.1 10.0
dodecamethylcyclohexasiloxane D6 0.3 10.0

Analyse von Erdgas - Siliziumanteil von Biomethan - Teil 2: Bestimmung des Siloxananteils durch gaschromatographische Ionenmobilitätsspektroskopie (ISO/DIS 2613-2:2023)

Analyse du gaz naturel - Biométhane - Partie 2: Détermination de la teneur en siloxanes par chromatographie en phase gazeuse spectrométrie de mobilité ionique (ISO/DIS 2613-2:2023)

Analiza zemeljskega plina - Biometan - 2. del: Določevanje siloksana s plinsko kromatografijo s spektrometrijo na osnovi mobilnosti ionov (GC-IMS) (ISO/DIS 2613-2:2023)

General Information

• Status: Not Published
• Publication Date: 09-Dec-2024
• Technical Committee: CEN/TC 408 - Project Committee - Biomethane for use in transport and injection in natural gas pipelines
• Drafting Committee: CEN/TC 408 - Project Committee - Biomethane for use in transport and injection in natural gas pipelines
• Current Stage: 4599 - Dispatch of FV draft to CMC - Finalization for Vote
• Start Date: 02-Aug-2023
• Due Date: 18-Dec-2023
• Completion Date: 02-Aug-2023
• Mandate: M/475 - Mandate to CEN for standards for biomethane for use in transport and injection in natural gas piplines
• Ref Project: oSIST prEN ISO 2613-2:2023 - Analysis of natural gas - Biomethane - Part 2: Determination of siloxane content by gas chromatography ion mobility spectrometry (ISO/DIS 2613-2:2023)

Standards Content (Sample)

SLOVENSKI STANDARD
oSIST prEN ISO 2613-2:2023
01-april-2023
Analiza zemeljskega plina - Biometan - 2. del: Določevanje siloksana s plinsko
kromatografijo s spektrometrijo na osnovi mobilnosti ionov (GC-IMS) (ISO/DIS
2613-2:2023)

Analysis of natural gas - Biomethane - Part 2: Determination of siloxane content by gas

chromatography ion mobility spectrometry (ISO/DIS 2613-2:2023)
Analyse von Erdgas - Siliziumanteil von Biomethan - Teil 2: Bestimmung des
Siloxananteils durch gaschromatographische Ionenmobilitätsspektroskopie (ISO/DIS
2613-2:2023)

Analyse du gaz naturel - Biométhane - Partie 2: Détermination de la teneur en siloxanes

par chromatographie en phase gazeuse spectrométrie de mobilité ionique (ISO/DIS
2613-2:2023)
Ta slovenski standard je istoveten z: prEN ISO 2613-2
ICS:
75.060 Zemeljski plin Natural gas
oSIST prEN ISO 2613-2:2023 en,fr,de

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

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oSIST prEN ISO 2613-2:2023
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oSIST prEN ISO 2613-2:2023
DRAFT INTERNATIONAL STANDARD
ISO/DIS 2613-2
ISO/TC 193/SC 1 Secretariat: NEN
Voting begins on: Voting terminates on:
2023-02-13 2023-05-08
Analysis of natural gas — Biomethane —
Part 2:
Determination of siloxane content by gas chromatography
ion mobility spectrometry
ICS: 75.060
This document is circulated as received from the committee secretariat.
THIS DOCUMENT IS A DRAFT CIRCULATED
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oSIST prEN ISO 2613-2:2023
ISO/DIS 2613-2:2023(E)
DRAFT INTERNATIONAL STANDARD
ISO/DIS 2613-2
ISO/TC 193/SC 1 Secretariat: NEN
Voting begins on: Voting terminates on:
Analysis of natural gas — Biomethane —
Part 2:
Determination of siloxane content by gas chromatography
ion mobility spectrometry
ICS: 75.060
This document is circulated as received from the committee secretariat.
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oSIST prEN ISO 2613-2:2023
ISO/DIS 2613-2:2022(E)
Contents Page

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

Introduction .................................................................................................................................................................................................................................v

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

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

3 Terms and definitions .................................................................................................................................................................................... 2

4 Principle ........................................................................................................................................................................................................................ 2

5 Materials ....................................................................................................................................................................................................................... 3

5.1 Calibration gases................................................................................................................................................................................... 3

5.2 Diluent gas .................................................................................................................................................................................................. 3

5.3 Carrier & drift gas................................................................................................................................................................................ 3

6 Apparatus .................................................................................................................................................................................................................... 3

6.1 GC-IMS analyser ...................................................................... ............................................................................................................... 3

6.2 Pressure regulator .............................................................................................................................................................................. 3

6.3 Dilution device ........................................................................................................................................................................................ 3

6.4 Auxiliary valves, tubing and accessories ........................................................................................................................ 4

7 Sampling ....................................................................................................................................................................................................................... 4

7.1 General ........................................................................................................................................................................................................... 4

7.2 Safety precautions ............................................................................................................................................................................... 4

7.3 Temperature control ......................................................................................................................................................................... 4

7.4 Construction materials ................................................................................................................................................................... 4

7.5 Cleanness ..................................................................................................................................................................................................... 4

7.6 Sampling of biomethane into vessels ................................................................................................................................. 5

7.7 Installation of the calibration gas cylinder ................................................................................................................... 5

7.8 Pressure control .................................................................................................................................................................................... 5

7.9 Purging of wetted flow path ......... .............................................................................................................................................. 5

7.10 Flow control .............................................................................................................................................................................................. 6

7.11 Diffusion control ................................................................................................................................................................................... 6

8 Calibration ..................................................................................................................................................................................................................6

8.1 Calibration procedure ...................................................................................................................................................................... 6

8.2 Frequency of calibration ................................................................................................................................................................ 6

9 Measurement procedure ............................................................................................................................................................................. 6

9.1 Safety precautions ............................................................................................................................................................................... 6

9.2 Analysis ......................................................................................................................................................................................................... 6

10 Expression of results ....................................................................................................................................................................................... 7

10.1 Quantities and units .......................................................................................................................................................................... 7

10.2 Uncertainty ................................................................................................................................................................................................ 7

10.3 Test report .................................................................................................................................................................................................. 7

Annex A (informative) Example of application ......................................................................................................................................... 8

Bibliography .............................................................................................................................................................................................................................10

iii
© ISO 2022 – All rights reserved
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oSIST prEN ISO 2613-2:2023
ISO/DIS 2613-2:2022(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

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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

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

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World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following

URL: www.iso.org/iso/foreword.html.

This document was prepared by Technical Committee ISO/TC 193, Natural gas, Subcommittee SC 1,

Analysis of natural gas.
A list of all parts in the ISO 2613 series can be found on the ISO website.

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.
© ISO 2022 – All rights reserved
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oSIST prEN ISO 2613-2:2023
ISO/DIS 2613-2:2022(E)
Introduction

This document describes a method for the determination of the siloxane content of biomethane that is

applicable to both laboratory and online analysis.

Siloxanes are a common contaminant in biogas, caused by their extensive use in common household

products such as cosmetics and detergents. These products eventually become entrained in waste

streams that are used to generate biogas. Additionally, siloxanes are sometimes added to digesters as

anti-foaming agents to improve generation efficiency.

If not effectively removed, siloxanes can cause damage to gas processing and vehicle injection

equipment through formation of silica deposits at high temperatures. Many gas distributors require

measurement reports to demonstrate that the resultant biomethane conforms with their requirements,

which typically includes siloxane content due to its potential to cause damage. Additionally, producers

may wish to monitor siloxane content for process optimisation purposes.

The technique described in this standard is commercially available and tailored specifically to

measuring siloxanes within biomethane at low concentrations (for instance, as specified in EN 16723-

[1] [2]
1 and EN 16723-2 ). It is suitable for use both in the laboratory and field.
© ISO 2022 – All rights reserved
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oSIST prEN ISO 2613-2:2023
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oSIST prEN ISO 2613-2:2023
DRAFT INTERNATIONAL STANDARD ISO/DIS 2613-2:2022(E)
Analysis of natural gas — Biomethane —
Part 2:
Determination of siloxane content by gas chromatography
ion mobility spectrometry
1 Scope

This document describes a Gas Chromatography – Ion Mobility Spectroscopy (GC-IMS) method for

the determination of the concentration of siloxanes in biomethane. The method is applicable to the

following siloxanes:
— hexamethyldisiloxane (L2)
— octamethyltrisiloxane (L3)
— decamethyltetrasiloxane (L4)
— dodecamethylpentasiloxane (L5)
— hexamethylcyclotrisiloxane (D3)
— octamethylcyclotetrasiloxane (D4)
— octamethylcyclotetrasiloxane (D5)
— dodecamethylcyclohexasiloxane (D6)

This document describes suitable calibration and measurement strategies to quantify siloxanes in (bio)

-3 -1

methane around and above the 0,3 mg m (14 µmol mol ) level and applies to analysis within absolute

pressure ranges of 1 bar – 2 bar, temperatures of 0 °C – 40 °C and relative humidity < 90 %.

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 6142-1, Gas analysis — Preparation of calibration gas mixtures — Part 1: Gravimetric method for Class

I mixtures

ISO 6143, Gas analysis — Comparison methods for determining and checking the composition of calibration

gas mixtures

ISO 6144, Gas analysis — Preparation of calibration gas mixtures — Static volumetric method

ISO 6145-1, Gas analysis — Preparation of calibration gas mixtures using dynamic methods — Part 1:

General aspects

ISO 6974-1, Natural gas — Determination of composition and associated uncertainty by gas

chromatography — Part 1: General guidelines and calculation of composition

ISO 6974-2, Natural gas — Determination of composition and associated uncertainty by gas

chromatography — Part 2: Uncertainty calculations
© ISO 2022 – All rights reserved
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oSIST prEN ISO 2613-2:2023
ISO/DIS 2613-2:2022(E)
ISO 7504, Gas analysis — Vocabulary
ISO 10715, Natural gas — Gas sampling
ISO 10723, Natural gas — Performance evaluation for analytical systems
ISO 14532, Natural gas — Vocabulary
ISO 14912, Gas analysis — Conversion of gas mixture composition data

ISO/IEC guide 98-3:2008, Uncertainty of measurement — Part 3: Guide to the expression of uncertainty in

me a s ur ement (GUM: 1995)
3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 7504, ISO/IEC guide 98-

3:2008, ISO 14532 and the following apply.

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 https:// www .electropedia .org/
3.1
ion mobility spectrometry
IMS

analytical method used to separate and identify ionised molecules in the gas phase based on their

mobility in a carrier gas under an electric field
4 Principle

A gaseous biomethane sample is drawn into a sample loop via a vacuum pump. The sample is injected

onto a GC column, which separates the individual components in the gas mixture. As they exit the

column, the components are ionised and passed into a drift tube. The drift tube applies an electroc field

and a f
...