SIST EN 13194:2015
(Main)Chemicals used for treatment of water intended for human consumption - Acetic Acid
Chemicals used for treatment of water intended for human consumption - Acetic Acid
This European Standard is applicable to acetic acid used for treatment of water intended for human consumption. It describes the characteristics of acetic acid and specifies the requirements and the corresponding test methods for acetic acid. It gives information on its use in water treatment.
Produkte zur Aufbereitung von Wasser für den menschlichen Gebrauch - Essigsäure
Diese Europäische Norm gilt für Essigsäure zur Aufbereitung von Wasser für den menschlichen Gebrauch. Sie beschreibt die Eigenschaften von Essigsäure und legt die Anforderungen sowie die entsprechenden Prüfverfahren für Essigsäure fest. Sie enthält Angaben zu deren Anwendung in der Wasseraufbereitung.
Produits chimiques utilisés pour le traitement de l'eau destinée à la consommation humaine - Acide acétique
La présente Norme européenne s'applique à l'acide acétique utilisé pour le traitement de l'eau destinée à la consommation humaine. Elle décrit les caractéristiques de l'acide acétique et spécifie les exigences et les méthodes d'essai correspondantes. Elle donne des informations pour son emploi dans le traitement de l'eau.*
Kemikalije, ki se uporabljajo za pripravo pitne vode - Ocetna kislina
General Information
Relations
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kemikalije, ki se uporabljajo za pripravo pitne vode - Ocetna kislinaProdukte zur Aufbereitung von Wasser für den menschlichen Gebrauch - EssigsäureProduits chimiques utilisés pour le traitement de l'eau destinée à la consommation humaine - Acide acétiqueChemicals used for treatment of water intended for human consumption - Acetic Acid71.100.80Chemicals for purification of water13.060.20Pitna vodaDrinking waterICS:Ta slovenski standard je istoveten z:EN 13194:2015SIST EN 13194:2015en,fr,de01-junij-2015SIST EN 13194:2015SLOVENSKI
STANDARDSIST EN 13194:20081DGRPHãþD
SIST EN 13194:2015
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 13194
March 2015 ICS 71.100.80 Supersedes EN 13194:2008English Version
Chemicals used for treatment of water intended for human consumption - Acetic Acid
Produits chimiques utilisés pour le traitement de l'eau destinée à la consommation humaine - Acide acétique
Produkte zur Aufbereitung von Wasser für den menschlichen Gebrauch - Essigsäure This European Standard was approved by CEN on 20 December 2014.
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 © 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13194:2015 ESIST EN 13194:2015
EN 13194:2015 (E) 2 Contents Page Foreword .4 Introduction .5 1 Scope .6 2 Normative references .6 3 Description .6 3.1 Identification .6 3.1.1 Chemical name .6 3.1.2 Synonym or common name .6 3.1.3 Relative molecular mass .6 3.1.4 Empirical formula.6 3.1.5 Chemical formula .6 3.1.6 CAS Registry Number ) .7 3.1.7 EINECS reference ) .7 3.2 Commercial form .7 3.3 Physical properties .7 3.3.1 Appearance .7 3.3.2 Density .7 3.3.3 Solubility in water .7 3.3.4 Vapour pressure (at 20 °C) .7 3.3.5 Boiling point at 100 kPa ) .7 3.3.6 Melting point .7 3.3.7 Specific heat .7 3.3.8 Viscosity, dynamic.8 3.3.9 Critical temperature (for gas) .8 3.3.10 Critical pressure (for gas) .8 3.3.11 Physical hardness .8 3.4 Chemical properties .8 4 Purity criteria .8 4.1 General .8 4.2 Composition of commercial product .8 4.3 Impurities and main by-products .8 4.4 Chemical parameters .9 5 Test methods .9 5.1 Sampling .9 5.1.1 Relevant Standards .9 5.1.2 Sampling from drums and bottles .9 5.1.3 Sampling from tanks and tankers . 10 5.2 Analysis . 10 5.2.1 Acetic acid (main product) . 10 5.2.2 Impurities . 11 5.2.3 Chemical parameters . 15 6 Labelling - Transportation - Storage . 17 6.1 Means of delivery . 17 6.2 Labelling according to the EU legislation ) . 17 6.3 Transportation regulations and labelling . 18 6.4 Marking . 19 6.5 Storage . 19 SIST EN 13194:2015
EN 13194:2015 (E) 3 6.5.1 General . 19 6.5.2 Long term stability . 19 6.5.3 Storage incompatibilities . 19 Annex A (informative)
General information on acetic acid . 20 A.1 Origin . 20 A.1.1 Raw materials . 20 A.1.2 Manufacturing process . 20 A.2 Use . 20 A.2.1 Function. 20 A.2.2 Form in which it is used . 20 A.2.3 Treatment dose . 20 A.2.4 Means of application . 21 A.2.5 Secondary effects . 21 A.2.6 Removal of excess product . 21 Annex B (normative)
General rules relating to safety . 22 B.1 Rules for safe handling and use . 22 B.2 Emergency procedures . 22 B.2.1 First aid . 22 B.2.2 Spillage . 22 B.2.3 Fire . 22 Bibliography . 23
SIST EN 13194:2015
EN 13194:2015 (E) 4 Foreword This document (EN 13194:2015) has been prepared by Technical Committee CEN/TC 164 “Water supply”, the secretariat of which is held by AFNOR. 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 September 2015, and conflicting national standards shall be withdrawn at the latest by September 2015. This document supersedes EN 13194:2008. 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. Significant technical difference between this edition and EN 13194:2008 is as follows: a) deletion of reference to EU Directive 67/548/EEC of June 27, 1967 in order to take into account the latest Regulation in force (see [3]); b) 6.2 – updating of risk and safety labelling according to EU Regulation [3] and its latest Adaptations to Technical Progress). 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. SIST EN 13194:2015
EN 13194:2015 (E) 5 Introduction In respect of potential adverse effects on the quality of water intended for human consumption, caused by the product covered by this European Standard: a) this European Standard provides no information as to whether the product may be used without restriction in any of the Member States of the EU or EFTA; b) it should be noted that, while awaiting the adoption of verifiable European criteria, existing national regulations concerning the use and/or the characteristics of this product remain in force. NOTE Conformity with this European Standard does not confer or imply acceptance or approval of the product in any of the Member States of the EU or EFTA. The use of the product covered by this European Standard is subject to regulation or control by National Authorities. SIST EN 13194:2015
EN 13194:2015 (E) 6 1 Scope This European Standard is applicable to acetic acid used for treatment of water intended for human consumption. It describes the characteristics of acetic acid and specifies the requirements and the corresponding test methods for acetic acid. It gives information on its use in water treatment.* 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. EN 1233, Water quality — Determination of chromium — Atomic absorption spectrometric methods EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696) EN ISO 12846, Water quality — Determination of mercury — Method using atomic absorption spectrometry (AAS) with and without enrichment (ISO 12846) ISO 17378-1, Water quality — Determination of arsenic and antimony — Part 1: Method using hydride generation atomic fluorescence spectrometry (HG-AFS) ISO 3165, Sampling of chemical products for industrial use — Safety in sampling ISO 6206, Chemical products for industrial use — Sampling — Vocabulary ISO 8288:1986, Water quality — Determination of cobalt, nickel, copper, zinc, cadmium and lead — Flame atomic absorption spectrometric methods ISO 9965, Water quality — Determination of selenium — Atomic absorption spectrometric method (hydride technique) 3 Description 3.1 Identification 3.1.1 Chemical name Acetic acid, ethanoic acid. 3.1.2 Synonym or common name Glacial acetic acid. 3.1.3 Relative molecular mass 60,05 3.1.4 Empirical formula C2H4O2 3.1.5 Chemical formula CH3COOH SIST EN 13194:2015
EN 13194:2015 (E) 7 3.1.6 CAS Registry Number 1) 64-19-7 3.1.7 EINECS reference 2) 200-580-7 3.2 Commercial form The product is available as colourless liquid. 3.3 Physical properties 3.3.1 Appearance The product is colourless liquid at 20 °C. 3.3.2 Density The density at 20 °C is given in Table 1. Table 1 — Density Concentration mass fraction % Density g/ml 80 1,068 to 1,072 99,85 1,049 to 1,050 3.3.3 Solubility in water Miscible. 3.3.4 Vapour pressure (at 20 °C) 1,57 kPa (for pure acetic acid) 3.3.5 Boiling point at 100 kPa 3) 118 °C (for pure acetic acid) 3.3.6 Melting point 16,2 °C (for pure acetic acid) 3.3.7 Specific heat 2,047 kJ/(kg K) at 20 °C (for pure acetic acid)
1) Chemical Abstracts Service Registry Number. 2) European Inventory of Existing Commercial Chemical Substances. 3) 100 kPa = 1 bar. SIST EN 13194:2015
EN 13194:2015 (E) 8 3.3.8 Viscosity, dynamic 1,222 mPa.s at 20 °C (for pure acetic acid) 3.3.9 Critical temperature (for gas) Not applicable. 3.3.10 Critical pressure (for gas) Not applicable. 3.3.11 Physical hardness Not applicable. 3.4 Chemical properties Acetic acid is a weak acid. 4 Purity criteria 4.1 General This European Standard specifies the minimum purity requirements for acetic acid used for the treatment of water intended for human consumption. Limits are given for impurities commonly present in the product. Depending on the raw material and the manufacturing process other impurities may be present and, if so, this shall be notified to the user and when necessary to relevant authorities. Users of this product should check the national regulations in order to clarify whether it is of appropriate purity for treatment of water intended for human consumption, taking into account raw water quality, required dosage, contents of other impurities and additives used in the product not stated in the product standard. Limits have been given for impurities and chemicals parameters where these are likely to be present in significant quantities from the current production process and raw materials. If the production process or raw materials leads to significant quantities of impurities, by-products or additives being present, this shall be notified to the user. 4.2 Composition of commercial product The product shall contain a minimum mass fraction of 80 percent acetic acid. NOTE The commercial product may contain up to a mass fraction of 20 % water. 4.3 Impurities and main by-products The product shall conform to the requirements specified in Table 2. SIST EN 13194:2015
EN 13194:2015 (E) 9 Table 2 — Impurities Impurity Limit in mg/kg of pure acetic acid Formic acid max. 500 Acetaldehyde max. 50 4.4 Chemical parameters NOTE For the purpose of this European Standard, “chemical parameters” are those defined in the EU Directive 98/83/EC of 3 November 1998 (see [2]). The content of chemical parameters shall conform to the requirements specified in Table 3. Table 3 — Chemical parameters Parameter Limit in mg/kg of pure acetic acid Arsenic (As) max. 0,5 Cadmium (Cd) max. 0,5 Chromium (Cr) max. 0,5 Mercury (Hg) max. 0,5 Nickel (Ni) max. 0,5 Lead (Pb) max. 0,5 Antimony (Sb) max. 0,5 Selenium (Se) max. 0,5 NOTE Cyanide does not exist in the acetic acid medium. Pesticides and polycyclic aromatic hydrocarbons are not by-products of the manufacturing process. 5 Test methods 5.1 Sampling 5.1.1 Relevant Standards Observe the general recommendations of ISO 3165 and take account of ISO 6206. 5.1.2 Sampling from drums and bottles 5.1.2.1 General 5.1.2.1.1 Mix the contents of the container to be sampled by shaking the container, by rolling it or by rocking it from side to side, taking care not to damage the container or spill any of the liquid. 5.1.2.1.2 If the design of the container is such (for example, a narrow-necked bottle) that it is impracticable to use a sampling implement, take a sample by pouring after the contents have been thoroughly mixed. Otherwise, proceed as described in 5.1.2.1.3. 5.1.2.1.3 Examine the surface of the liquid. If there are signs of surface contamination, take samples from the surface as described in 5.1.2.2; otherwise, take samples as described in 5.1.2.3. SIST EN 13194:2015
EN
...
SLOVENSKI STANDARD
kSIST FprEN 13194:2014
01-september-2014
Kemikalije, ki se uporabljajo za pripravo pitne vode - Ocetna kislina
Chemicals used for treatment of water intended for human consumption - Acetic Acid
Produkte zur Aufbereitung von Wasser für den menschlichen Gebrauch - Essigsäure
Produits chimiques utilisés pour le traitement de l'eau destinée à la consommation
humaine - Acide acétique
Ta slovenski standard je istoveten z: FprEN 13194
ICS:
13.060.20 Pitna voda Drinking water
71.100.80 .HPLNDOLMH]DþLãþHQMHYRGH Chemicals for purification of
water
kSIST FprEN 13194:2014 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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kSIST FprEN 13194:2014
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kSIST FprEN 13194:2014
EUROPEAN STANDARD
FINAL DRAFT
FprEN 13194
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2014
ICS 71.100.80 Will supersede EN 13194:2008
English Version
Chemicals used for treatment of water intended for human
consumption - Acetic Acid
Produits chimiques utilisés pour le traitement de l'eau Produkte zur Aufbereitung von Wasser für den
destinée à la consommation humaine - Acide acétique menschlichen Gebrauch - Essigsäure
This draft European Standard is submitted to CEN members for unique acceptance procedure. It has been drawn up by the Technical
Committee CEN/TC 164.
If this draft becomes a European Standard, 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.
This draft European Standard was established by CEN 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.
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.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice and
shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2014 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprEN 13194:2014 E
worldwide for CEN national Members.
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kSIST FprEN 13194:2014
FprEN 13194:2014 (E)
Contents Page
Foreword .4
Introduction .5
1 Scope .6
2 Normative references .6
3 Description .6
3.1 Identification .6
3.1.1 Chemical name .6
3.1.2 Synonym or common name .6
3.1.3 Relative molecular mass .6
3.1.4 Empirical formula.6
3.1.5 Chemical formula .7
3.1.6 CAS Registry Number .7
3.1.7 EINECS reference .7
3.2 Commercial form .7
3.3 Physical properties .7
3.3.1 Appearance .7
3.3.2 Density .7
3.3.3 Solubility in water .7
3.3.4 Vapour pressure (at 20 °C) .7
3.3.5 Boiling point at 100 kPa .7
3.3.6 Melting point .7
3.3.7 Specific heat .8
3.3.8 Viscosity, dynamic.8
3.3.9 Critical temperature (for gas) .8
3.3.10 Critical pressure (for gas) .8
3.3.11 Physical hardness .8
3.4 Chemical properties .8
4 Purity criteria .8
4.1 General .8
4.2 Composition of commercial product .8
4.3 Impurities and main by-products .8
4.4 Chemical parameters .9
5 Test methods .9
5.1 Sampling .9
5.1.1 Relevant Standards .9
5.1.2 Sampling from drums and bottles .9
5.1.3 Sampling from tanks and tankers . 10
5.2 Analysis . 10
5.2.1 Acetic acid (main product) . 10
5.2.2 Impurities . 11
5.2.3 Chemical parameters . 15
6 Labelling - Transportation - Storage . 17
6.1 Means of delivery . 17
6.2 Labelling according to the EU legislation . 17
6.3 Transportation regulations and labelling . 18
6.4 Marking . 19
2
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6.5 Storage . 19
6.5.1 General . 19
6.5.2 Long term stability . 19
6.5.3 Storage incompatibilities . 19
Annex A (informative) General information on acetic acid . 20
A.1 Origin . 20
A.1.1 Raw materials . 20
A.1.2 Manufacturing process . 20
A.2 Use . 20
A.2.1 Function. 20
A.2.2 Form in which it is used . 20
A.2.3 Treatment dose . 20
A.2.4 Means of application . 21
A.2.5 Secondary effects . 21
A.2.6 Removal of excess product . 21
Annex B (normative) General rules relating to safety . 22
B.1 Rules for safe handling and use . 22
B.2 Emergency procedures . 22
B.2.1 First aid . 22
B.2.2 Spillage . 22
B.2.3 Fire . 22
Bibliography . 23
3
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kSIST FprEN 13194:2014
FprEN 13194:2014 (E)
Foreword
This document (FprEN 13194:2014) has been prepared by Technical Committee CEN/TC 164 “Water supply”,
the secretariat of which is held by AFNOR.
This document is currently submitted to the Unique Acceptance Procedure.
This document will supersede EN 13194:2008.
Significant technical difference between this edition and EN 13194:2008 is as follows:
a) Deletion of reference to EU Directive 67/548/EEC of June 27, 1967 in order to take into account the latest
Regulation in force (see [3]).
b) clause 6.2 – updating of risk and safety labelling according to EU Regulation [3] and its latest Adaptations
to Technical Progress).
4
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kSIST FprEN 13194:2014
FprEN 13194:2014 (E)
Introduction
In respect of potential adverse effects on the quality of water intended for human consumption, caused by the
product covered by this European Standard:
a) this European Standard provides no information as to whether the product may be used without
restriction in any of the Member States of the EU or EFTA;
b) it should be noted that, while awaiting the adoption of verifiable European criteria, existing national
regulations concerning the use and/or the characteristics of this product remain in force.
NOTE Conformity with this European Standard does not confer or imply acceptance or approval of the product in any
of the Member States of the EU or EFTA. The use of the product covered by this European Standard is subject to
regulation or control by National Authorities.
5
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kSIST FprEN 13194:2014
FprEN 13194:2014 (E)
1 Scope
This European Standard is applicable to acetic acid used for treatment of water intended for human
consumption. It describes the characteristics of acetic acid and specifies the requirements and the
corresponding test methods for acetic acid. It gives information on its use in water treatment.*
2 Normative references
The following referenced documents are indispensable for the application 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.
EN 1233, Water quality - Determination of chromium - Atomic absorption spectrometric methods.
EN 1483, Water quality - Determination of mercury – Method using atomic absorption spectrometry.
EN 26595, Water quality - Determination of total arsenic - Silver diethyldithiocarbamate spectrophometric
method (ISO 6595).
EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987).
ISO 3165, Sampling of chemical products for industrial use — Safety in sampling.
ISO 3856-2, Paints and varnishes — Determination of "soluble" metal content — Part 2: Determination of
antimony content — Flame atomic absorption spectrometric method and Rhodamine B spectrophotometric
method.
ISO 6206, Chemical products for industrial use — Sampling — Vocabulary.
ISO 8288:1986, Water quality — Determination of cobalt, nickel, copper, zinc, cadmium and lead — Flame
atomic absorption spectrometric methods.
ISO 9965, Water quality — Determination of selenium — Atomic absorption spectrometric method (hydride
technique).
3 Description
3.1 Identification
3.1.1 Chemical name
Acetic acid, ethanoic acid.
3.1.2 Synonym or common name
Glacial acetic acid.
3.1.3 Relative molecular mass
60,05
3.1.4 Empirical formula
C H O
2 4 2
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3.1.5 Chemical formula
CH COOH
3
1)
3.1.6 CAS Registry Number
64-19-7
2)
3.1.7 EINECS reference
200-580-7
3.2 Commercial form
The product is available as colourless liquid.
3.3 Physical properties
3.3.1 Appearance
The product is colourless liquid at 20 °C.
3.3.2 Density
The density at 20 °C is given in Table 1.
Table 1 — Density
Concentration Density
mass fraction % g/ml
80 1,068 to 1,072
99,85 1,049 to 1,050
3.3.3 Solubility in water
Miscible.
3.3.4 Vapour pressure (at 20 °C)
1,57 kPa (for pure acetic acid)
3)
3.3.5 Boiling point at 100 kPa
118 °C (for pure acetic acid)
3.3.6 Melting point
16,2 °C (for pure acetic acid)
1)
Chemical Abstracts Service Registry Number.
2)
European Inventory of Existing Commercial Chemical Substances.
3)
100 kPa = 1 bar.
7
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3.3.7 Specific heat
2,047 kJ/(kg K) at 20 °C (for pure acetic acid)
3.3.8 Viscosity, dynamic
1,222 mPa.s at 20 °C (for pure acetic acid)
3.3.9 Critical temperature (for gas)
Not applicable.
3.3.10 Critical pressure (for gas)
Not applicable.
3.3.11 Physical hardness
Not applicable.
3.4 Chemical properties
Acetic acid is a weak acid.
4 Purity criteria
4.1 General
This European Standard specifies the minimum purity requirements for Acetic acid used for the treatment of
water intended for human consumption. Limits are given for impurities commonly present in the product.
Depending on the raw material and the manufacturing process other impurities may be present and, if so, this
shall be notified to the user and when necessary to relevant authorities.
Users of this product should check the national regulations in order to clarify whether it is of appropriate purity
for treatment of water intended for human consumption, taking into account raw water quality, required
dosage, contents of other impurities and additives used in the product not stated in the product standard.
Limits have been given for impurities and chemicals parameters where these are likely to be present in
significant quantities from the current production process and raw materials. If the production process or raw
materials leads to significant quantities of impurities, by-products or additives being present, this shall be
notified to the user.
4.2 Composition of commercial product
The product shall contain a minimum mass fraction of 80 percent acetic acid.
NOTE The commercial product may contain up to a mass fraction of 20% water.
4.3 Impurities and main by-products
The product shall conform to the requirements specified in Table 2.
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FprEN 13194:2014 (E)
Table 2 — Impurities
Impurity Limit in mg/kg of pure acetic acid
Formic acid max. 500
Acetaldehyde max. 50
4.4 Chemical parameters
NOTE For the purpose of this European Standard, "chemical parameters" are those defined in the EU Directive
98/83/EC of 3 November 1998 (see [2]).
The content of chemical parameters shall conform to the requirements specified in Table 3.
Table 3 — Chemical parameters
Limit in mg/kg
Parameter of pure acetic
acid
Arsenic (As) max. 0,5
Cadmium (Cd) max. 0,5
Chromium (Cr) max. 0,5
Mercury (Hg) max. 0,5
Nickel (Ni) max. 0,5
Lead (Pb) max. 0,5
Antimony (Sb) max. 0,5
Selenium (Se) max. 0,5
NOTE Cyanide does not exist in the acetic acid medium.
Pesticides and polycyclic aromatic hydrocarbons are not by-
products of the manufacturing process.
5 Test methods
5.1 Sampling
5.1.1 Relevant Standards
Observe the general recommendations of ISO 3165 and take account of ISO 6206.
5.1.2 Sampling from drums and bottles
5.1.2.1 General
5.1.2.1.1 Mix the contents of the container to be sampled by shaking the container, by rolling it or by
rocking it from side to side, taking care not to damage the container or spill any of the liquid.
5.1.2.1.2 If the design of the container is such (for example, a narrow-necked bottle) that it is impracticable
to use a sampling implement, take a sample by pouring after the contents have been thoroughly mixed.
Otherwise, proceed as described in 5.1.2.1.3.
5.1.2.1.3 Examine the surface of the liquid. If there are signs of surface contamination, take samples from
the surface as described in 5.1.2.2; otherwise, take samples as described in 5.1.2.3.
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5.1.2.2 Surface sampling
Take a sample using a suitable ladle. Lower the ladle into the liquid until the rim is just below the surface, so
that the surface layer runs into it. Withdraw the ladle just before it fills completely and allow any liquid adhering
to the ladle to drain off. If necessary, repeat this operation so that, when the other selected containers have
been sampled in a similar manner, the total volume of sample required for subsequent analysis is obtained.
5.1.2.3 Bottom sampling
Take a sample using an open sampling tube, or a bottom-valve sampling tube, suited to the size of container
and the viscosity of the liquid.
When using an open sampling tube, close it at the top and then lower the bottom end to the bottom of the
container. Open the tube and move it rapidly so that the bottom of the tube traverses the bottom of the
container before the tube is filled. Close the tube, withdraw it from the container and allow any liquid adhering
to the outside of the tube to drain off.
When using a bottom-valve sampling tube, close the valve before lowering the tube into the container and
then proceed in a similar manner to that when using an open sampling tube.
5.1.3 Sampling from tanks and tankers
From each access point, take samples as follows:
a) from the surface of the liquid, using a ladle as described in 5.1.2.2;
b) from the bottom of the tank or tanker, using a sampling tube as described in 5.1.2.3 or using a specially
designed bottom-sampling apparatus;
c) from one or more positions, depending on the overall depth, between the bottom and the surface using a
weighted sampling can.
5.2 Analysis
5.2.1 Acetic acid (main product)
5.2.1.1 Principle
An accurately weighed quantity of the sample is diluted with water and then titrated with a standard volumetric
sodium hydroxide solution using phenolphthalein as an indicator.
5.2.1.2 Reagents
All reagents shall be of a recognized analytical grade and the water used shall conform to grade 3 in
accordance with EN ISO 3696.
5.2.1.2.1 Sodium hydroxide solution c (NaOH) = 1,0 mol/l.
5.2.1.2.2 Phenolphthalein indicator solution, 5 g/l.
5.2.1.3 Apparatus
5.2.1.3.1 Ordinary laboratory apparatus and glassware.
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5.2.1.4 Procedure
Into a 100 ml conical flask accurately weigh 2,0 g of the sample and add 25 ml of water. Titrate with sodium
hydroxide solution (5.2.1.2.1) using phenolphthalein indicator (5.2.1.2.2) to a pink colouration which persists
for at least 15 s.
5.2.1.5 Expression of results
The concentration in mass fraction percent of acetic acid (C ) is given by the following formula:
1
V × c× 0,06005 × 100
C = (1)
1
m
o
where
V is the volume, in millilitres, of sodium hydroxide solution (5.2.1.2.1) used;
c is the concentration, in moles per litre, of sodium hydroxide solution (5.2.1.2.1);
is the mass in grams of acetic acid equivalent to 1 ml of sodium hydroxide
0,06005
solution c (NaOH) = 1,0 mol/l;
m
is the mass, in grams, of the test sample.
o
5.2.1.6 Repeatability limit
The absolute difference between two single test results, obtained under repeatability conditions, shall not be
greater than the repeatability limit value, r, as calculated from the following formula:
r = 0,05 z (2)
where
z is the mean of the two results, expressed in mass fraction %.
NOTE Repeatability conditions are conditions where mutually independent test results are obtained with the same
method on identical test material in the same laboratory by the same operator using the same equipment within short
intervals of time.
5.2.2 Impurities
5.2.2.1 Formic acid content (HCOOH)
5.2.2.1.1 Principle
A sample of acetic acid is introduced into a gas chromatograph containing a packed column and maintained at
135 °C. Butan-2-one is used as internal standard.
5.2.2.1.2 Reagents
All reagents shall be of a recognized analytical grade and the water used shall conform to grade 3 in
accordance with EN ISO 3696.
5.2.2.1.2.1 Acetic acid.
5.2.2.1.2.2 Carrier gas.
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Helium, gas chromatography grade.
5.2.2.1.2.3 Butan-2-one.
5.2.2.1.2.4 Formic acid.
5.2.2.1.3 Apparatus
Ordinary laboratory apparatus and glassware, together with the following:
5.2.2.1.3.1 Chromatograph
Use a gas chromatographic apparatus with typical set up described in the following subclauses.
NOTE Different instrumental parameters can be required for specific chromatographic apparatus.
5.2.2.1.3.2 Column oven
Air oven at 135 °C.
5.2.2.1.3.3 Gas controls
Carrier gas at 28 ml/min.
5.2.2.1.3.4 Injections
Direct on-column injector at 150 °C, 1 µl sample.
5.2.2.1.3.5 Column
A glass column of 2 m nominal length and an internal diameter of 3 mm. Packing Chromosorb
® 4)
101 (90/100 mesh) or equivalent.
NOTE Other columns may be used if they give similar results.
5.2.2.1.3.6 Flame ionisation detector, operating at 200 °C.
5.2.2.1.4 Procedure
5.2.2.1.4.1 Calibration
Prepare accurately four synthetic mixtures with formic acid (5.2.2.1.2.4) in the range of 10 mg/kg to 1 000
mg/kg in acetic acid (5.2.2.1.2.1).
Add accurately by weighting, butan-2-one (5.2.2.1.2.3) to give a final concentration of 500 mg/kg. Using the
purity of each component correct the mass of each mixture. Inject the samples into the gas chromatograph.
From the area and corrected masses calculate the area ratio and mass ratio of each component relative to
butan-2-one and plot on linear/linear graph paper the mass ratio on the y-axis and the area ratio on the x-axis.
The slope of the graph gives the response factor for the component relative to butan-2-one.
5.2.2.1.4.2 Determination
4) ®
Chromosorb 101 is the trade-name of a product supplied by Johns Manville. This information is given for the
convenience of users of this standard and does not constitute an endorsement by CEN of the product named. Equivalent
products may be used if they can be shown to lead to the same results.
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FprEN 13194:2014 (E)
Inject 1 μl of the test sample and adjust the amplification so that each peak obtained remains on the scale.
5.2.2.1.5 Expression of results
The formic acid content (C ) expressed in milligrams per kilogram of pure acetic acid is given by the following
2
formula:
(A × F )
100
x x
C = × (3)
2
A C
F 1
where
A is the peak area of formic acid;
x
F is the relative response factor of formic acid;
x
A is the sum of the peak areas multiplied by their relative response factors;
F
C is the concentration expressed in mass fraction percent of acetic acid (5.2.1.5).
1
5.2.2.1.6 Repeatability limit
The absolute difference between two single test results, obtained under repeatability conditions, shall not be
greater than the repeatability limit value, r, as calculated from the following formula:
r = 0,03 z (4)
where
z is the mean of the two results, expressed in milligrams per kilogram.
NOTE Repeatability conditions are conditions where mutually independent test results are obtained with the same
method on identical test material in the same laboratory by the same operator using the same equipment within short
intervals of time.
5.2.2.2 Aldehydes content (as CH CHO)
3
5.2.2.2.1 Principle
A sample of acetic acid is heated with an excess of sodium hydrogen sulfite solution, and the aldehydes react
to form addition compounds. The unreacted sodium hydrogen sulfite is titrated with a standard volumetric
iodine solution. The volume of disulfite used in the reaction is u
...
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