BS EN ISO 13734:2013

BSI Standards Publication

Natural gas — Organic

components used as odorants
— Requirements and test
methods (ISO 13734:2013)
BS EN ISO 13734:2013 BRITISH STANDARD

National foreword
This British Standard is the UK implementation of EN ISO
13734:2013. It supersedes BS EN ISO 13734:2001 which is withdrawn.
The UK participation in its preparation was entrusted to Technical
Committee PTI/15, Natural Gas and Gas Analysis.
A list of organizations represented on this committee can be
obtained on request to its secretary.
This publication does not purport to include all the necessary
provisions of a contract. Users are responsible for its correct
application.
© The British Standards Institution 2013. Published by BSI Standards
Limited 2013
ISBN 978 0 580 72971 3
ICS 75.060
Compliance with a British Standard cannot confer immunity from
legal obligations.
This British Standard was published under the authority of the
Standards Policy and Strategy Committee on 30 November 2013.
Amendments issued since publication
Date Text affected
EUROPEAN STANDARD EN ISO 13734
NORME EUROPÉENNE
EUROPÄISCHE NORM November 2013

ICS 75.060 Supersedes EN ISO 13734:2000

English Version

Natural gas - Organic components used as odorants -

Requirements and test methods (ISO 13734:2013)

Gaz naturel - Composés organiques utilisés comme Erdgas - Organische Verbindungen zur Verwendung als
odorisants - Exigences et méthodes d'essai (ISO Odoriermittel - Anforderungen und Prüfverfahren (ISO
13734:2013) 13734:2013)

This European Standard was approved by CEN on 12 October 2013.

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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, 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: Avenue Marnix 17, B-1000 Brussels

© 2013 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 13734:2013 E
worldwide for CEN national Members.
BS EN ISO 13734:2013
EN ISO 13734:2013 (E)

Foreword
This document (EN ISO 13734:2013) has been prepared by Technical Committee ISO/TC 193 "Natural gas".

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 May 2014, and conflicting national standards shall be withdrawn at the
latest by May 2014.

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN ISO 13734:2000.

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, Former Yugoslav Republic of Macedonia, France, Germany, Greece,
Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.

Endorsement notice

The text of ISO 13734:2013 has been approved by CEN as EN ISO 13734:2013 without any modification.

3
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ISO 13734:2013(E)


Contents Page

Foreword......................................................................................................................................................................................................................................... iv
Introduction...................................................................................................................................................................................................................................v
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references....................................................................................................................................................................................... 1
3 Terms and definitions...................................................................................................................................................................................... 1
4 Requirements........................................................................................................................................................................................................... 2
4.1 Recommendations of an effective odorant...................................................................................................................... 2
4.2 Composition of odorants................................................................................................................................................................. 3
4.3 Cloud point.................................................................................................................................................................................................. 3
4.4 Phase properties..................................................................................................................................................................................... 3
4.5 Evaporation residue............................................................................................................................................................................ 3
4.6 Insoluble matter..................................................................................................................................................................................... 3
4.7 Solubility in water................................................................................................................................................................................. 3
5 Handling and transport.................................................................................................................................................................................. 4
6 Tests.................................................................................................................................................................................................................................... 4
6.1 Test sample.................................................................................................................................................................................................. 4
6.2 Test documentation............................................................................................................................................................................. 4
6.3 Determination of composition................................................................................................................................................... 4
6.4 Determination of cloud point...................................................................................................................................................... 4
6.5 Determination of phase properties........................................................................................................................................ 4
6.6 Determination of evaporation residue................................................................................................................................ 4
6.7 Visual examination for solids or suspended matter................................................................................................ 5
6.8 Determination of solubility in water..................................................................................................................................... 5
7 Labelling and documentation.................................................................................................................................................................. 5
7.1 Labelling........................................................................................................................................................................................................ 5
7.2 Documentation........................................................................................................................................................................................ 6
Annex A (informative) Properties of odorants............................................................................................................................................ 7

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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. 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. 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.
The committee responsible for this document is ISO/TC 193, Natural gas.
This second edition cancels and replaces the first edition (ISO 13734:1998), which has been technically
revised. It also incorporates the Corrigendum ISO 13734:1998/Corr.1:1999.

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Introduction
Processed natural gas received from suppliers normally has little or no odour. For safety reasons, natural
gas is therefore odorized to permit the detection by smell of the gas at very low concentrations in air.
NOTE It is a common requirement that natural gas in air be readily detectable by smell at a concentration of
20 % of the lower flammability limit (LFL). The LFL of natural gas is normally taken as the volume fraction in air
of 4 % to 5 %.

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BS EN ISO 13734:2013
 BS EN ISO 13734:2013
INTERNATIONAL STANDARD ISO 13734:2013(E)

Natural gas — Organic components used as odorants —

Requirements and test methods

1 Scope
This International Standard specifies requirements and test methods for organic compounds suitable for
odorization of natural gas and natural gas substitutes for public gas supply, hereafter referred to as odorants.

2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 3007:2005, Petroleum products and crude petroleum — Determination of vapour pressure — Reid method
ISO 3015:1992, Petroleum products — Determination of cloud point
ISO 4256:1996, Liquefied petroleum gases — Determination of gauge vapour pressure — LPG method
ISO  4626:1980, Volatile organic liquids — Determination of boiling range of organic solvents used as
raw materials
ISO 14532, Natural gas — Vocabulary

3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 14532 (in particular 3.1 to 3.4)
and the following apply.
3.1
odorization
addition of odorants, normally intensely smelling organic sulfur compounds, to natural gas (normally
odourless) to allow the recognition of gas leaks by smell at very low concentration (before a build up to
a dangerous gas in air concentration can occur)
Note 1 to entry: Adapted from ISO 14532.

Note 2 to entry: Natural gas is normally odourless. The addition of an odorant to the gas fed into the distribution
system for safety reasons permits the detection of the gas by smell at very low concentrations.

3.2
odorant
intensely smelling organic chemical or combination of chemicals added to natural gas at low concentration
and capable of imparting a characteristic and distinctive (usually disagreeable) warning odour so gas
leaks can be detected at concentrations below their lower flammability limit
[SOURCE: ISO 14532]

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3.3
odour character
type of sensation of an odour
[SOURCE: ISO 14532]
Note 1 to entry: Odour character is a qualitative parameter.

3.4
odour intensity
strength of odour perception
[SOURCE: ISO 14532]
3.5
threshold concentration
concentration at which an individual has a probability of 0,5 in perceiving the odour
Note 1 to entry: To detect an odour does not imply that this odour may be identified.

3.6
odour intensity curve
relationship between odour intensity and odorant concentration in air
Note 1 to entry: The odour intensity can only be determined by the human olfactory organ.

3.7
diluent
organic liquid, normally consisting of paraffinic hydrocarbons, used to reduce the concentration of an
odorant to a suitable level at which the solution may be injected into the natural gas
3.8
cloud point
temperature at which a cloud of crystals first appears in a liquid when it is cooled under specified conditions

4 Requirements

4.1 Recommendations of an effective odorant

Gas odorants should meet the following general recommendations:
a) The gas odorant should have a strong odour at very low concentration.
b) The odour character of the odorant needs to be unpleasant, distinctive and not confusable with
other frequently occurring odours so that it is unmistakably associated with a gas leak.
c) The odour character should be the same at different dilutions of natural gas with air.
d) The odorant should be sufficiently stable during storage and when mixed with natural gas.
e) The volatility of the odorant should be high enough so that the odorant does not appreciably
condense under the conditions (temperature and pressure) existing in the pipeline system.
f) Evaporation of the gas odorant should not appreciably leave residues.
g) The odorant should be useable at low temperatures, when required.
h) The combustion of the odorant should not leave significant solid deposits.
i) The addition of the odorant to natural gas should not make the resulting gas harmful.

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These general recommendations should be assessed against the specific conditions of use of the
odorant (conditions of the natural gas transportation grid, odorization installation, type of odorant,
composition of the gas).
Experience in many countries has shown that these basic requirements are best met by organic
sulfur compounds - sulfides (thioethers) and mercaptans (thiols) - with boiling points below 130  °C.
Since primary mercaptans are easily oxidized to disulfides which have a much lower odour intensity,
mercaptan-based odorants need to predominantly contain secondary and tertiary mercaptans.
While it has been established that the above sulfur compounds fulfil the basic requirements listed above
under a) to i), other, non-sulfurous odorants have been developed and are available.

4.2 Composition of odorants

The mass fraction of the declared chemical product in the undiluted odorant shall be at least 95 %. The
composition of the odorant, and where applicable the dilution range, shall be declared by the producer
or distributor. It shall be stable over the maximum shelf time as declared by the manufacturer.
In sulfur containing odorants, the mass fraction of sulfides (thioethers) or secondary or tertiary
mercaptans (thiols) shall be at least 80 %. Primary mercaptans are more easily oxidized than secondary
or tertiary mercaptans.
For non-sulfurous odorants based on acrylates, care shall be taken e.g. by use of an appropriate additive
to avoid polymerisation.

4.3 Cloud point

The cloud point of the undried odorant, to be determined in accordance with 6.4, shall be below -30 °C.

4.4 Phase properties

4.4.1 Boiling point

The boiling point of the components of the odorants and diluent, measured in accordance with 6.5, shall
not be higher than 130 °C.

4.4.2 Vapour pressure curve

The vapour pressure curve of the odorant and eventually the diluent shall be given. It shall be determined
in accordance with 6.5.

4.5 Evaporation residue

The mass fraction of the evaporation residue, to be determined in accordance with 6.6, shall be less than
0,2 %.

4.6 Insoluble matter

Odorants shall not contain any visible insoluble matter, to be determined in accordance with 6.7.

4.7 Solubility in water

When the odorant is added to water in the way specified in 6.8, less than 2 % by volume of the odorant
shall be soluble.

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5 Handling and transport

When delivered, odorants shall be accompanied by a safety data sheet conforming to the requirements
of the country of use.
Appropriate personnel protective equipment, as specified in the safety data sheet, shall be used
when handling odorants The safety data sheet shall also give information about safe handling,
transport and storage.

6 Tests

6.1 Test sample

For type approval and control tests, the producer or supplier shall deliver at least 0,5 l of a representative
sample of the liquid odorant to a qualified test laboratory, acceptable to both producer and purchaser.

6.2 Test documentation

The following documentation shall be provided by the producer or supplier:
— a material safety data sheet (MSDS) conforming to the requirements of the country of use;
— complete details of the composition of the odorant.

6.3 Determination of composition

The composition of the odorant shall be determined by gas-chromatographic analysis. Any gas-
chromatographic method giving sufficient component separation and detection may be used.

6.4 Determination of cloud point

The cloud point shall be determined in accordance with ISO 3015 except that, contrary to the method
specified in that standard, cloud formation by water shall be taken into account; therefore the sample
shall be neither filtered nor dried. The test jar in its jacket is directly immersed in bath No. 4 specified
in Table 2 of ISO 3015:1992 having the temperature range -52 °C to -49 °C. When the temperature of
the odorant has reached -30 °C, the test jar is removed from the jacket quickly, without disturbing the
sample, and inspected for cloudiness.

6.5 Determination of phase properties

The boiling point of compounds used as odorants shall be measured in accordance with ISO 4626.
The vapour pressure curve shall be determined either in accordance with ISO  3007 or, for odorants
applicable for the odorization of liquefied petroleum gases (LPG), in accordance with ISO 4256.

6.6 Determination of evaporation residue

Insert a gas inlet tube equipped with a stopcock into one neck of a two-necked round-bottomed flask
with a volume of about 25 ml so that the tube extends nearly to the bottom of flask. Close off the other
neck with a gas outlet tube also equipped with a stopcock. It is strongly recommended that PTFE
(polytetrafluoroethylene) or other non-reactive/non-absorptive material jackets are used to seal the
ground-glass connections instead of grease and stopcocks with PTFE plugs. Weigh the assembly to an
accuracy of better than 1 mg (m0). Using a pipette or syringe, transfer about 5 ml of the odorant into the
flask. Weigh the closed flask (m1) to determine the mass of the odorant sample.
Connect the gas inlet tube to a supply of inert gas, e.g. nitrogen, to avoid the oxidation of mercaptans.
Connect the gas outlet to a cold trap or an absorber filled with activated charcoal to trap the evaporated
odorant. Evaporate the odorant by passing a stream of inert gas at about 20 ml/min through the flask,

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which is heated in a water bath at a temperature of about 20 °C to 30 °C below the boiling point of the
odorant. For odorants with high boiling points, the determination can be accelerated by reducing the
pressure. This is done by connecting the outlet of the cold trap or absorber to a vacuum pump and
replacing the gas inlet tube by a fine capillary to avoid retardation of ebullition. Flush the capillary with
an inert gas, for example nitrogen, to avoid the oxidation of mercaptans.
When all visible odorant has been evaporated, close the stopcocks, dry the flask carefully, allow it to
return to room temperature and weigh (mE(1)). Then continue the evaporation for 15 min under the
abovementioned conditions. Continue the weighing and evaporation until the difference in mass between
the last two weighings (mE(n+1) - mE(n)) is less than 1 mg. Calculate the evaporation residue R from the
last value (mE(n+1)) and the mass of the sample used, to the nearest 0,01 %, from the following equation:
mE (n+1) − m0
R= × 100
m1 − m0

6.7 Visual examination for solids or suspended matter

Take a sample of about 20 ml of the odorant in a normal test tube of about 15 mm internal diameter and
inspect it after shaking and again after a settling time of 15 min, against a light source, for insoluble material.

6.8 Determination of solubility in water

Add 5 ml of the odorant to 50 ml of a 10 % solution of sodium chloride in water in a graduated glass
cylinder (see Figure 1) with a ground-in plug. Measure the volume of the odorant in the graduated part
of the cylinder with the cylinder in the upright position (V1).
Dimensions in millimetres

Figure 1 — Cylinder for solubility determination

Keep the cylinder horizontal in a thermostatically controlled water bath at a temperature of 10 °C ± 1 °C
for 24 h. Then measure again the volume of the odorant in the graduated part of the cylinder (V2) and
calculate the solubility S to the nearest 0,1 %, from the following equation:
V1 − V2
S= × 100
V1

7 Labelling and documentation

7.1 Labelling
Odorant containers shall be clearly marked in accordance with the applicable safety and transport
regulations. The markings will normally include:
a) the name and/or registered trade mark of the producer of the odorant;
b) the designation and composition of the odorant;

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c) safety and handling instructions conforming to the requirements of the country of use (e.g. hazard
classification).

7.2 Documentation
The supplier of the odorant shall provide each user of the odorant (e.g. a gas distribution company) with
a (material) safety data sheet and additional documentation giving information about:
— the odour intensity curve of the odorant including the detection threshold of the odorant determined
in accordance with ISO standards (when and if such standards are published);
— storage conditions that will preserve the olfactory, physical and chemical properties of the odorant;
— compatibility of the liquid odorant with materials it may be in contact with before vaporization;
— indication of the odorant stability under pipeline conditions;
— indication of the odorant stability in the ground and with water;
— indication of the reactivity of the vaporized odorant with pipeline materials including seals.
The origin of this information (i.e. experimental procedure, source of data) shall be given. It is also
possible to express this information relatively to a well-known odorant such as THT.

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Annex A
(informative)

Properties of odorants

A.1 Odorant components

The components of commonly used odorants are almost exclusively sulfur containing organic compounds
which comply with the basic recommendations listed in Clause 4. They belong to the following classes
of substances:
a) alkyl sulfides (alkyl thioethers): symmetrical sulfides, e.g. C2H5-S-C2H5; asymmetrical sulfides,
e.g. CH3-S-C2H5;
b) cyclic sulfides (cyclic thioethers), e.g. C4H8S;
c) alkyl mercaptans (alkane thiols): primary mercaptans, e.g. C2H5-SH; secondary mercaptans, e.g.
(CH3)2CH-SH; tertiary mercaptans, e.g. (CH3)3C-SH.
A number of non-sulfur products have been proposed for gas odorant, for instance, norbornene and
derivatives, acrylates, pentanones, pyrazine aldehydes and mixtures of those. So far, only few of these
products are in use, based on acrylates.

A.2 Properties of sulfurous odorants

A.2.1 Olfactory properties
Mercaptans and sulfides are used as natural gas odorants because of their strong and characteristic
odour. Compared to other compounds of the class of sulfides, e.g. the simple alkyl sulfides such as
dimethylsulfide, methylethylsulfide and diethylsulfide, the cyclic sulfide tetrahydrothiophene (THT)
(thiacyclopentane) shows higher odour intensity. Mercaptans possess the highest odour intensity.

A.2.2 Physical and chemical properties

Among the physical properties of odorants, the volatility, closely related to the boiling point, is the most
important. To avoid condensation low-boiling components are preferred. When used in evaporation
odorizers, the differences between the boiling points of the odorant components in mixtures should be small.
It is not recommended to use tert.-butylmercaptan (TBM) as a single component odorant because of its high
freezing point. At low temperatures, TBM would not be sufficiently vaporized and thus not be detected.
Sulfides are chemically more stable than mercaptans. Mercaptans may be oxidized by iron oxide (rust) to
disulfides. Iron oxide also acts as a catalyst for the oxidation of mercaptans by oxygen [e.g. when LPG1)–
air mixtures are used for peak shaving]. By this reaction mercaptans are transformed into disulfides,
which have significantly lower odour intensity and also a different odour character. Tertiary mercaptans
(e.g. TBM) are more resistant to oxidation than secondary mercaptans (e.g. iso-propylmercaptan)
and secondary mercaptans are more resistant than primary mercaptans. Mixtures of branched and
unbranched mercaptans are more easily or more quickly oxidized than pure branched mercaptans.
For the odorization of pipeline gas, it is preferable to use sulfides and branched mercaptans. Mercaptans
are normally used as mixtures with sulfides. However, examples of pure products used as odorants are
THT and secondary butylmercaptan (SBM).

1) LPG = liquefied petroleum gas

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When starting gas distribution through new gas lines or when changing the odorant, it may take some
time to reach the required odorant concentration at the end of the line. This may result from the odorant
being sorbed on the pipe wall, by pipe dust, rust and incrustations or by gas condensates (odour fading).
The degree of sorption depends on several factors, for example the condition of the pipe grid, the
pressure, the temperature, the flow velocity and the physicochemical properties of odorants.
Odorized gases leaking from gas lines in the ground may lose odorants by sorption in the soil. Higher
boiling odorants such as THT will more likely be adsorbed than lower boiling odorants such as TBM.
Mercaptans may be oxidized by soil containing iron oxide to less odoriferous but more strongly sorbed
disulfides. Sorption and oxidation of odorants may vary with moisture content and the type of soil.
Degradation of odorants by micro-organisms may also occur.

A.3 Physical and chemical data of pure sulfur compounds

Some data of the most widely used sulfur compounds used as odorants pure or in a mixture are listed
in Table A.1.

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Table A.1 — List of chemical and physical properties of pure sulfur compounds

Sulfur compound Formula Molar mass Boiling point Freezing point Density
g/mol
°C °C (at 20 °C) g/cm³
Sulfides (thioether)
Dimethyl sulfide (DMS) CH3SCH3 62,14 37,3 -98,3 0,848 3
Methyl ethyl sulfide (MES) CH3SC2H5 76,16 66,7 -105,9 0,842 2
Diethyl sulfide (DES) (C2H5)2S 90,19 92,1 -103,9 0,836 2
Tetrahydrothiophene (THT) C 4H8 S 88,17 121,0 -96,1 0,998 7
Mercaptans (thiols)
Methylmercaptan (MM) a CH3SH 48,11 5,9 -123 0,866 5
(methanethiol)
Ethylmercaptan (EM)c C2H5SH 62,14 35,1 -147,8 0,831 5b
(ethanethiol)
n-Propylmercaptan (NPM) C3H7SH 76,16 67 to 68 -113,3 0,841 1
(1-propanethiol)
iso-Propylmercaptan (IPM) (CH3)2CHSH 76,16 52,6 -130,5 0,814 3
(2-propanethiol)
n-Butylmercaptan (NBM) C4H9SH 90,19 98,5 -115,7 0,841 6
(1-butanethiol)
sec.-Butylmercaptan (SBM) CH3CH(SH)C2H5 90,19 85 -165 0,829 5
(2-butanethiol)
iso-Butylmercaptan (IBM) (CH3)2CHCH2SH 90,19 88,5 < -70 0,835 7
(2-methylpropane-1-thiol)
tert.-Butylmercaptan (TBM) (CH3)3CSH 90,19 64,3 -0,5 0,794 3b
(2-methylpropane-2-thiol)
Values taken from the Handbook of Chemistry and Physics, 87th ed., CRC Press, Boca Raton, Florida, USA.
a Not used for natural gas odorization, but may naturally occur in natural gas.
b Value at 25 °C.
c Generally applied as odorant for LPG only but may occur in natural gas after conditioning involving propane or butane.

A.4 Properties of non-sulfurous odorant

Some data of the most widely used non-sulfur compounds used as odorants pure or in a mixture are
listed in Table A.2.

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Table A.2 — Physical data of non-sulfur odorant compounds of odorants in use

Odorant Formula Molar mass Boiling point Freezing point Density
g/mol °C °C (at 20 °C) g/cm³
Methyl acrylate C2H3CO2CH3 86 80 -75 0,956
Ethyl acrylate C2H3CO2C2H5 100,12 100 -72 0,922

NOTE Acrylates present a smell different to that of sulfurous odorants. Furthermore some caution is to be
taken when switching from one to the other as they may not readily fulfil 4.1 b).

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