Analyse des gaz -- Lignes directrices pour le prélèvement des échantillons

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DRAFT INTERNATIONAL STANDARD ISO/DIS 19230 ISO/TC 158 Secretariat: NEN Voting begins on: Voting terminates on: 2020-01-15 2020-04-08 Gas analysis — Sampling guidelines Analyse des gaz — Lignes directrices pour le prélèvement des échantillons ICS: 71.040.40 THIS DOCUMENT IS A DRAFT CIRCULATED FOR COMMENT AND APPROVAL. IT IS THEREFORE SUBJECT TO CHANGE AND MAY NOT BE REFERRED TO AS AN INTERNATIONAL STANDARD UNTIL PUBLISHED AS SUCH. IN ADDITION TO THEIR EVALUATION AS BEING ACCEPTABLE FOR INDUSTRIAL, This document is circulated as received from the committee secretariat. TECHNOLOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT INTERNATIONAL STANDARDS MAY ON OCCASION HAVE TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL TO BECOME STANDARDS TO WHICH REFERENCE MAY BE MADE IN Reference number NATIONAL REGULATIONS. ISO/DIS 19230:2020(E) 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 SUPPORTING DOCUMENTATION. ISO 2020 ---------------------- Page: 1 ---------------------- ISO/DIS 19230:2020(E) COPYRIGHT PROTECTED DOCUMENT © ISO 2020

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ISO/DIS 19230:2020 (E)
Contents

Foreword .......................................................................................................................................................................... v

Introduction.................................................................................................................................................................... vi

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

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

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

4 Sampling plan .......................................................................................................................................................... 5

5 Sampling classification ........................................................................................................................................ 6

5.1 Sampling classification of gases ....................................................................................................................... 6

5.2 Sampling classification of liquified gas .......................................................................................................... 7

6 Technical specifications ...................................................................................................................................... 8

6.1 Overview ................................................................................................................................................................... 8

6.2 General considerations for gas sampling ...................................................................................................... 8

6.2.1 Adsorption, reaction and permeation of sampling system .............................................................. 8

6.2.2 Leaks and atmospheric diffusion in the sampling system ................................................................ 8

6.2.3 Leak testing of the sampling system ......................................................................................................... 8

6.2.4 Purging of sampling system ......................................................................................................................... 9

6.2.5 Homogeneity of gas ...................................................................................................................................... 12

6.2.6 Inert-gas purging .......................................................................................................................................... 12

6.3 Possible condensation during compressed gas sampling .................................................................... 12

6.4 Main condensations for liquefied gas sampling ...................................................................................... 13

6.5 Samples that are not feasible in containers or cannot be used for analysis directly ................. 13

7 Safety guidance in sampling ........................................................................................................................... 13

7.1 Overview ................................................................................................................................................................ 13

7.2 General recommendation ................................................................................................................................ 13

7.3 Specific recommendation for sampling a certain substance .............................................................. 14

8 Sampling devices................................................................................................................................................. 14

8.1 General provision ............................................................................................................................................... 14

8.2 Sample container ................................................................................................................................................ 15

8.2.1 Sample container material ........................................................................................................................ 15

8.2.2 Structure of sample container ................................................................................................................. 16

8.2.3 Volume of sample container ..................................................................................................................... 19

8.3 Sample probe ....................................................................................................................................................... 19

8.4 Pressure reducer and flow controller ......................................................................................................... 19

8.5 Sample pump ........................................................................................................................................................ 20

8.6 Sample line ............................................................................................................................................................ 20

8.6.1 Material of sample line ............................................................................................................................... 20

8.6.2 Length and diameter of sample line ...................................................................................................... 20

8.7 Connecters and seals ......................................................................................................................................... 20

8.8 Cleaning and drying of the sampling device ............................................................................................. 21

8.9 Connection of sampling devices .................................................................................................................... 21

9 Sampling ................................................................................................................................................................ 21

9.1 Sampling method block diagram .................................................................................................................. 21

9.1.1 Overview .......................................................................................................................................................... 21

9.1.2 Block diagram of compressed gas sampling method ...................................................................... 21

9.1.3 Block diagram of liquefied gas sampling method............................................................................. 23

9.2 Quality assessment of the sampling system .............................................................................................. 24

9.3 Sampling from the gaseous phase and sampling after evaporation of liquefied gas ................. 24

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ISO/DIS 19230:2020(E)

9.4 Direct sampling ................................................................................................................................................... 24

9.4.1 General provisions ....................................................................................................................................... 24

9.4.2 Direct sampling of gas in pressure receptacles ................................................................................. 25

9.4.3 Direct sampling of gas in pipelines ........................................................................................................ 25

9.5 Indirect sampling ................................................................................................................................................ 25

9.5.1 Indirect sampling of gas in pressure receptacles ............................................................................. 25

9.5.2 Indirect sampling of gas in pipelines .................................................................................................... 26

9.5.3 Leakage test of sample container ........................................................................................................... 26

9.5.4 Storage of samples ....................................................................................................................................... 26

9.6 Sampling records ................................................................................................................................................ 27

Annex A (informative) Examples of estimation of the purging time and purging cycles for

sampling system ........................................................................................................................................... 28

Annex B (informative) Direct sampling for gas in pressure receptables .............................................. 30

Annex C (informative) Direct sampling of gas in pipelines ........................................................................ 33

Annex D (informative) Fill-empty sampling method .................................................................................... 35

Annex E (informative) Evacuated-container sampling ................................................................................ 37

Annex F (informative) Evacuated-system sampling ..................................................................................... 41

Bibliography ................................................................................................................................................................. 43

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ISO/DIS 19230:2020 (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 158 Analysis of Gases.

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.
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ISO/DIS 19230:2020(E)
Introduction

The determination of gas composition, impurity concentration and physical properties depends to a

large extent on sampling technique. The use of correct sampling techniques is an important safety and

quality critical step in gas analysis. The design, construction and selection of the sampling equipment to

avoid hazardous situations and sampling errors are important and directly influence the results

obtained. Any slight carelessness, in exactitude or mistake will seriously influence safety and the

results obtained.

Gaseous products are stored and transported in pressure receptacles in the form of compressed or

liquefied gas or through gas pipelines. The sampling methods used differ depending upon the package,

composition and delivery methods.

This document provides technical guidelines for the sampling of gases in pressure receptacles and

pipelines for analytical purposes.
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ISO/DIS 19230:2020 (E)
Gas Analysis— Sampling Guidelines
1 Scope

This document gives the basic definitions of terms and general provisions relating to sampling for

gas analysis, including sampling devices, sampling methods, sampling technical considerations, and

sampling safety.

This document applies to both direct and indirect sampling of gas in pressure receptacles and

pipelines, including pure gases and gas mixtures. Compressed and liquefied gases are both

considered.

This document applies to the sampling of processed gases and does not involve gas treatment

processes.

The sampling procedures specified are not intended for the sampling of special products which are the

subject of other International Standards, such as liquefied petroleum gases (ISO 4257) and gaseous

natural gases (ISO 10715).

Warning — The use of this document may involve a number of hazards. This document does

not specify all the safety issues associated with the use of the standard. Users of this

document are responsible for establishing measures to ensure safety whilst gas sampling. All

sampling activities should comply with national and local safety regulations.
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 3165, Sampling of chemical products for industrial use — Safety in sampling

ISO 16664, Gas analysis — Handling of calibration gases and gas mixture — Guidelines

3 Terms and definitions
For the purposes of this document, the following terms and definitions 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 http://www.electropedia.org/
3.1
gas

all materials which are present completely in gaseous form at a temperature of 20 ° C under the

absolute pressure of 0,1013 MPa
Note 1 to entry: The materials here include single mediums and mixtures.
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3.2
compressed gas

gas which, when packaged under pressure for transport, is entirely gaseous at all temperatures

above − 50 °C

Note 1 to entry: This category includes all gases with a critical temperature less than or equal to − 50 °C.

[SOURCE: ISO 10286:2015, 705]
3.3
liquified gas

gas which, when packaged under pressure for transport, is partially liquid at temperatures

above − 50 °C
[SOURCE: ISO 10286:2015, 706]
3.4
high pressure liquefied gas
gas with a critical temperature between − 50 °C and + 65 °C
[SOURCE: ISO 10286:2015, 708]
3.5
low pressure liquefied gas
gas with a critical temperature above + 65 °C
[SOURCE: ISO 10286:2015, 707]
3.6
toxic gas

gas which is known to be so toxic or corrosive to humans to pose a health hazard or which is presumed

to be toxic or corrosive to humans because it has a LC50 value for acute toxicity equal to or less than

5000 ml/m (ppm)

Note 1 to entry: Other risks such as tissue corrosiveness are sometimes associated.

[SOURCE: ISO 10286:2015, 716]
3.7
gas in pressure receptacles

gas stored in cylinders, tube, pressure drums, tanks and other pressure receptacles, and no fresh gas

replenished into the receptacles
3.8
gas in pipelines
gas delivered in pipelines during the production process
3.9
sampling device

components that comprise the sampling system mainly include sample lines, pressure

regulators/reducers, flow controllers, connectors and sample containers
3.10
sampling system

gas transmission and control system constructed by gas storage container or sample point of gas in

pipelines and various sampling devices
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ISO/DIS 19230:2020 (E)
3.11
representative sample

a sample assumed to have the same composition as the material sampled when the latter is considered

as a homogeneous whole
[SOURCE: ISO 6206:1979, 3.1.4]
3.12
direct sampling

sampling in situations where there is a direct connection between the gas to be sampled and the

analytical unit
[SOURCE: ISO 10715:1997, 2.1]
3.13
indirect sampling

sampling in situation where there is no direct connection between the gas to be sampled and the

analytical unit
[SOURCE: ISO 10715:1997, 2.7]
3.14
sampling plan

the planned procedure of selection, withdrawal and preparation of a sample or samples from a lot to

yield the required knowledge of the characteristic(s) from the final sample so that a decision can be

made regarding the lot
[SOURCE: ISO 6206:1979, 3.1.5]
3.15
spot sampling

indirect sampling from a specific part of the stream of material with a certain volume at a specific time

3.16
incremental sampling
indirect sampling by collecting a series of spot samples into a combined sample
3.17
continuous sampling

direct sampling taken continuously from a stream of material with a constant flow rate in a certain

period of time
3.18
intermittent sampling
direct sampling from a stream of material with predetermined intervals
3.19
ullage/outage

the space in the container not occupied by the material, or the distance between the material surface

and a fixed reference point at the top of the container
NOTE 1 to entry: This volume allows room for expansion.
[SOURCE: ISO 6206:1979, 3.3.14]
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3.20
sampling error

that part of the total estimation error of a characteristic due to known and acceptable deficiencies in the

sampling plan
[SOURCE: ISO 6206:1979, 3.4.10]
3.21
incremental sampler
a sampler which accumulates a series of spot samples into one composite sample
[SOURCE: ISO 10715:1997, 2.6]
3.22
low-pressure gas
gases with a pressure between 0 and 0,2 MPa at sampling temperature

NOTE 1 to entry: Except for special provisions, all pressures mentioned in this standard are gauge pressures.

3.23
high-pressure gas
gases with a pressure exceeding 0,2 MPa at sampling temperature
3.24
lag time
time taken for a representative sample to enter the instrument
[SOURCE: ISO 11042-2:1996, 3.5.1.1]
3.25
sample container
a container for collecting the gas sample when indirect sampling is necessary
[SOURCE: ISO 10715:1997, 2.14]
3.26
sample line

conduit to transfer a sample of gas from the sample place to the analytical unit or sample container

Note 1 to entry: Another word used for sample line is transfer line.
[SOURCE: ISO 14532:2014, 2.3.2.5]
3.27
sample probe

device inserted into the gas pipelines so that a representative sample of the flowing gas can be taken.

The sample probe will have a conduit to convey the sample from the flowing gas to a point external to

the pipeline
[SOURCE:ISO 14532:2014,2.3.2.6]
3.28
sampling point
a point in the gas stream where a representative sample can be collected
[SOURCE: ISO 10715:1997, 2.17]
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3.29
filling ratio

ratio of the mass of gas to the mass of water at 15 °C that would fill completely a pressure receptacle

fitted ready for use

Note 1 to entry: Synonyms are filling factor and filling degree, often expressed in kg/l or similar.

[SOURCE: ISO 10286:2015, 747]
3.30
continuous purging method
purging method by continually purging the sampling system with sample gases
3.31
fill-empty cycle purging method

purging method by sequentially filling and emptying the sampling system repeatedly with the gas to be

sampled
3.32
evacuation-gas purging cycles
purging method by evacuating the sampling system
3.33
sampling from the gaseous phase
sampling from the gaseous phase of the liquefied gas
3.34
sampling from the liquid phase
sampling from the liquid phase of the liquefied gas
3.35
sampling in liquid form

the process that takes a sample in liquid form directly from the liquid phase of the liquefied gas

3.36
sampling after evaporation

the process that takes a sample in gaseous form by vaporizing the sample from the liquid phase of the

liquefied gas
3.37
liquid valve

a device fitted to an analyser for the direct sampling of liquefied gas in liquid form, which can keep the

liquefied gas to be collected in completely liquid phase
4 Sampling plan
A feasible and complete sampling plan should be developed before sampling.

For a sampling plan, first determine the sampling type (clause 5), then consider techniques of sampling

(clause 6), to determine the appropriate sampling process (clause 9) and sampling devices (clause 8)

and sampling safety (clause 7), and then sampling (clause 9).
The scheme for sampling plan is shown in Figure 1.
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ISO/DIS 19230:2020(E)
Figure 1 —Scheme of sampling plan
5 Sampling classification
5.1 Sampling classification of gases

In this document, the sampling classification is based on whether the gas is connected to the analyser.

In addition, the sampling methods vary among different gas packaging, storage methods and sampling

purposes.

Direct sampling, if possible, is strongly recommended. In the case of indirect sampling, the potential loss

of component during the time between sampling and analysis should be studied and incorporated in the

uncertainty budget.

In general, for gas in pressure receptacles the internal composition is relatively uniform and constant.

For gases in pipelines the purpose and controls required dictate the type of sampling used. The design

of a sampling plan should consider whether the objectives of sampling are to:
• Determine the instantaneous gaseous composition
• Determine an average composition over a specified time interval
• Establish changes in concentration by repeated sampling over a specified time

• Pass continuous samples into the analyser to measure both limit and average composition

A flow chart detailing the gas sampling classification is shown in Figure 2.
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ISO/DIS 19230:2020 (E)
Figure 2 — Gas sampling classification
5.2 Sampling classification of liquified gas

When sampling liquefied gases, a representative sample is obtained by sampling from the liquid phase,

however occasionally it may also be necessary to sample the vapour phase, e.g. the gas phase

composition is frequently required in the preparation of calibration gas mixtures.

Sampling from the liquid phase is further sub-divided into sampling in liquid form or sampling after

evaporation. The method of sampling used is normally determined by a review of the physical

properties of the liquefied gas such as vapour pressure etc. Generally low temperature liquefied gases

and high pressure liquefied gases require evaporation whereas low pressure liquefied gases may be

sampled in liquid phase.

For the liquefied gas sampling classification see Figure 3 which details the sampling methods that

should be used, then follow 5.1 to determine the specific sampling type.
Liquefied gas sampling
Sampling from the liquid phase
Sampling from the gaseous phase
Sampling in liquid form Sampling after evaporation
Figure 3 — Liquified gas sampling classification
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ISO/DIS 19230:2020(E)
6 Technical specifications
6.1 Overview

For gas sampling, attention should be paid to but not limited to the following considerations to collect

sufficient representative sample.
6.2 General considerations for gas sampling
6.2.1 Adsorption, reaction and permeation of sampling system

Such problems can be minimized by choosing sampling devices of suitable materials (see clause 8 for

details).

However, some slight adsorption is difficult to overcome. In this case, the sampling system should be

heated or continuously purged for a long period of time, and quality assessment of the sampling system

should be carried out according to 9.2. The adsorption shall be considered in the uncertainty budget.

6.2.2 Leaks and atmospheric diffusion in the sampling system

Leaks in the sampling system not only result in a loss of gas from the system but also allow air to diffuse

into the system (the partial pressure of the component determines the direction of the diffusion)

thereby affecting the composition of the sample.

The sampling system should be leak tested (see 6.2.3) prior to use to ensure the sample will not be

contaminated, the composition changed, or hazardous conditions created by the ingress of air.

Furthermore, the back-diffusion of air into gas venting lines should be avoided by, for example, using

longer venting lines.
6.2.3 Leak testing of the sampling system

All connections and welds shall be tested prior to first use. During subsequent re-use of the sampling

system re-connected parts should be retested for leaks. Other parts of the system should be regularly

retested, this is particularly important for corrosive gases. When sampling toxic gases leak testing shall

be performed before each use of the sampling system. The integrity of the sampling containers and their

connection with the sampling system should also be tested.
The following test methods can be used:

a) Pressurization of the system, followed by monitoring of the static pressure with respect to time.

A pressure drop indicates a leak.

b) Evacuation of the system and monitoring the vacuum achieved. A deterioration in the vacuum

resulting in an increase in pressure indicates a leak.

c) Pressurize the system and check all connections with a leak detection solution. Following the

use of leak detection solution, the system should be purged out to ensure dryness prior to use.

d) Use of a leak detector (e.g. mass spectrometry, where the system is filled with helium and the

presence of helium outside the system is detected with the mass spectrometer).

The correct selection of a leak detection method depends upon the system requirements. For example,

leak detection solution may not detect small leaks, however,
...

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