Bitumen and bituminous binders - Determination of acid number of bitumen - Potentiometric method

This document describes a method for the determination of the free acidic constituents present in bitumen, conventionally known as acid number.
WARNING - The use of this document may involve hazardous materials, operations and equipment. This document does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this document to establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use.

Bitumen und bitumenhaltige Bindemittel - Bestimmung der Säurezahl von Bitumen - Potentiometrisches Verfahren

Dieses Dokument beschreibt ein Verfahren zur Bestimmung der in Bitumen enthaltenen freien sauren Bestandteile, gemeinhin als Säurezahl bekannt.
WARNUNG - Die Anwendung dieses Dokuments kann gefährliche Substanzen, Arbeitsgänge und Ausrüstung einschließen. Dieses Dokument erhebt nicht den Anspruch, auf alle Sicherheitsprobleme hinzuweisen, die mit seiner Anwendung verbunden sind. Es liegt in der Verantwortung des Anwenders dieses Dokuments, geeignete Sicherheits- und Gesundheitsschutzmaßnahmen vorzusehen und im Vorfeld die Anwendbarkeit von einschränkenden Vorschriften zu klären.

Bitumes et liants bitumineux - Détermination de l'indice d'acide d’un bitume - Méthode potentiométrique

Le présent document prescrit une méthode de détermination des constituants acides libres présents dans un bitume, conventionnellement désignés sous le terme « indice d’acide ».
AVERTISSEMENT - L'utilisation de ce document implique l'intervention de produits, d'opérations et d'équipements à caractère dangereux. Le présent document n'est pas censé aborder tous les problèmes de sécurité concernés par son usage. Il est de la responsabilité de l'utilisateur de ce document de consulter et d'établir des règles de sécurité et d'hygiène appropriées et de déterminer l'applicabilité des restrictions réglementaires avant utilisation.

Bitumen in bitumenska veziva - Določevanje kislinskega števila bitumna - Potenciometrijska metoda

General Information

Status
Published
Public Enquiry End Date
19-Apr-2020
Publication Date
14-Sep-2020
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
28-Jul-2020
Due Date
02-Oct-2020
Completion Date
15-Sep-2020

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SLOVENSKI STANDARD
SIST-TS CEN/TS 17482:2020
01-oktober-2020
Bitumen in bitumenska veziva - Določevanje kislinskega števila bitumna -
Potenciometrijska metoda
Bitumen and bituminous binders - Determination of acid number of bitumen -
Potentiometric method
Bitumen und bitumenhaltige Bindemittel - Bestimmung der Säurezahl von Bitumen -
Potentiometrisches Verfahren

Bitumes et liants bitumineux - Détermination de l'indice d'acide d’un bitume - Méthode

potentiométrique
Ta slovenski standard je istoveten z: CEN/TS 17482:2020
ICS:
75.140 Voski, bitumni in drugi naftni Waxes, bituminous materials
proizvodi and other petroleum products
91.100.50 Veziva. Tesnilni materiali Binders. Sealing materials
SIST-TS CEN/TS 17482:2020 en,fr,de

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

---------------------- Page: 1 ----------------------
SIST-TS CEN/TS 17482:2020
---------------------- Page: 2 ----------------------
SIST-TS CEN/TS 17482:2020
CEN/TS 17482
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
July 2020
TECHNISCHE SPEZIFIKATION
ICS 75.140; 91.100.50
English Version
Bitumen and bituminous binders - Determination of acid
number of bitumen - Potentiometric method

Bitumes et liants bitumineux - Détermination de Bitumen und bitumenhaltige Bindemittel -

l'indice d'acide d'un bitume - Méthode Bestimmung der Säurezahl von Bitumen -
potentiométrique Potentiometrisches Verfahren

This Technical Specification (CEN/TS) was approved by CEN on 1 June 2020 for provisional application.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to

submit their comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS

available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in

parallel to the CEN/TS) until the final decision about the possible conversion of the CEN/TS into an EN is reached.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, 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: Rue de la Science 23, B-1040 Brussels

© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 17482:2020 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST-TS CEN/TS 17482:2020
CEN/TS 17482:2020 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

1 Scope .................................................................................................................................................................... 4

2 Normative references .................................................................................................................................... 4

3 Terms and definitions ................................................................................................................................... 4

4 Principle ............................................................................................................................................................. 4

5 Products and reagents ................................................................................................................................... 4

6 Apparatus ........................................................................................................................................................... 5

7 Sampling ............................................................................................................................................................. 5

8 General instructions....................................................................................................................................... 6

8.1 Preparation of the potentiometry apparatus and electrodes ......................................................... 6

8.2 Titration of the solution of alcoholic potassium hydroxide and blank test ............................... 6

8.3 Operating procedure ..................................................................................................................................... 6

9 Operating procedure ..................................................................................................................................... 6

9.1 Titration of the solution of alcoholic potassium hydroxide and blank test ............................... 6

9.2 Titration of the bitumen ............................................................................................................................... 7

10 Calculations ....................................................................................................................................................... 8

11 Expression of results ...................................................................................................................................... 8

12 Precision ............................................................................................................................................................. 9

12.1 Repeatability ..................................................................................................................................................... 9

12.2 Reproducibility ................................................................................................................................................ 9

13 Test report ......................................................................................................................................................... 9

Annex A (informative) Method for using a manual titration apparatus ................................................. 10

A.1 General ............................................................................................................................................................. 10

A.2 Operating procedure .................................................................................................................................. 10

Bibliography ................................................................................................................................................................. 13

---------------------- Page: 4 ----------------------
SIST-TS CEN/TS 17482:2020
CEN/TS 17482:2020 (E)
European foreword

This document (CEN/TS 17482:2020) has been prepared by Technical Committee CEN/TC 336

“Bituminous binders”, the secretariat of which is held by AFNOR.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

According to the CEN/CENELEC Internal Regulations, the national standards organisations of the

following countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria,

Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,

Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of

North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United

Kingdom.
---------------------- Page: 5 ----------------------
SIST-TS CEN/TS 17482:2020
CEN/TS 17482:2020 (E)
1 Scope

This document describes a method for the determination of the free acidic constituents present in

bitumen, conventionally known as acid number.

WARNING — The use of this document may involve hazardous materials, operations and equipment. This

document does not purport to address all of the safety problems associated with its use. It is the

responsibility of the user of this document to establish appropriate safety and health practices and to

determine the applicability of regulatory limitations prior to use.
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.

EN 58, Bitumen and bituminous binders — Sampling bituminous binders
EN 12594, Bitumen and bituminous binders — Preparation of test samples
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:

— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
3.1
acid number

number of milligrams of potassium hydroxide necessary for the neutralization of the free acids contained

in one gram of bitumen
3.2
equivalence point

stage of the titration procedure at which the added volume (equivalent volume) of titration reagent has

allowed to neutralize the acid compounds of the test sample

Note 1 to entry: In potentiometric titrations, this point corresponds to the inflexion point of the potential curve.

4 Principle

The bitumen is dissolved in a solvent-alcohol mixture. The acidic constituents are titrated using a solution

of alcoholic potassium hydroxide. The titration is monitored by potentiometry.
5 Products and reagents
5.1 General
Only use reagents of a quality recognized for analysis.
5.2 Potassium hydroxide RP (analytical grade), in pellets.
5.3 Propan-2-ol (isopropanol) RP (analytical grade).
---------------------- Page: 6 ----------------------
SIST-TS CEN/TS 17482:2020
CEN/TS 17482:2020 (E)
5.4 Solvent RP (analytical grade), xylene or methyl benzene (toluene).
5.5 Benzoic acid RP (analytical grade).
5.6 Solution of alcoholic potassium hydroxide, 0,1 mol/L.

Dissolve (6,0 ± 0,2) g of potassium hydroxide pellets (5.2) in 1 L of pure propan-2-ol (5.3).

A ready-for-use, off-the-shelf solution can also be used. Only a titration certificate coming from an

authorized supplier can avoid the titration procedure (9.1). The alcoholic potassium hydroxide solution

shall be kept in brown glass containers and stored in the dark.
6 Apparatus
6.1 General
Usual laboratory equipment, together with the following.
6.2 Balance of adequate capacity for weight with precision of ± 1 mg.
6.3 Potentiometry apparatus, for automatic or manual titration:

— apparatus for automatic titration, including a titration device with sensitivity of at least 2 mV,

equipped with an automatic dosage unit with a capacity of 5 mL to 20 mL. Most of these pieces of

equipment offer a program for potentiometric detection with dynamic equivalence point titration. It

means that increment is slowed down near the equivalence point;

— apparatus for manual titration, including a potentiometer with a sensitivity of at least 2 mV and a

burette with a pointed spout.

The equipment shall allow titration steps to be performed at an accuracy of at least ± 0,05 mL in volume.

6.4 Glass combination electrode – Ag/AgCl.

6.4.1 A pH glass electrode for non-aqueous media and a reference electrode of Ag/AgCl (kept in its

inner reference electrolyte).

6.4.2 Combined pH electrode for non-aqueous media instead of the two electrodes cell of 6.4.1.

6.5 Glass beakers, or any glass titration container, specific for the automatic potentiometric titration

device (6.3).

The volume of beakers shall be appropriate for immersing the membrane of electrodes into the tested

solution and shall allow increasing this volume during titration.

The level of solution in the beaker shall be below the filling hole of the electrodes but has to be high

enough to prevent the stirring bar (if it is necessary to use it) from hitting the membranes if the electrodes

have to be close to the bottom of the beaker.
6.6 Magnetic stirrer, with polytetrafluoroethylene (PTFE)-coated bar.
7 Sampling

Take the sample in accordance with EN 58. Prepare the test samples in accordance with EN 12594.

---------------------- Page: 7 ----------------------
SIST-TS CEN/TS 17482:2020
CEN/TS 17482:2020 (E)
8 General instructions
8.1 Preparation of the potentiometry apparatus and electrodes
The titration device shall be prepared following manufacturer instructions.

Special attention shall be paid to the storing and maintenance of the electrodes:

— before using, the inner body shall be filled with the electrolyte. If necessary, refill and let the electrode

to rest for at least o
...

SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 17482:2020
01-april-2020
Bitumen in bitumenska veziva - Določevanje kislinskega števila bitumna -
Potenciometrijska metoda
Bitumen and bituminous binders - Determination of acid number of bitumen -
Potentiometric method
Bitumen und bitumenhaltige Bindemittel - Bestimmung der Säurezahl von Bitumen -
Potentiometrisches Verfahren

Bitumes et liants bitumineux - Détermination de l'indice d'acide d’un bitume - Méthode

potentiométrique
Ta slovenski standard je istoveten z: FprCEN/TS 17482
ICS:
75.140 Voski, bitumni in drugi naftni Waxes, bituminous materials
proizvodi and other petroleum products
91.100.50 Veziva. Tesnilni materiali Binders. Sealing materials
kSIST-TS FprCEN/TS 17482:2020 en,fr,de

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

---------------------- Page: 1 ----------------------
kSIST-TS FprCEN/TS 17482:2020
---------------------- Page: 2 ----------------------
kSIST-TS FprCEN/TS 17482:2020
FINAL DRAFT
TECHNICAL SPECIFICATION
FprCEN/TS 17482
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2020
ICS 75.140; 91.100.50
English Version
Bitumen and bituminous binders - Determination of acid
number of bitumen - Potentiometric method

Bitumes et liants bitumineux - Détermination de Bitumen und bitumenhaltige Bindemittel -

l'indice d'acide d'un bitume - Méthode Bestimmung der Säurezahl von Bitumen -
potentiométrique Potentiometrisches Verfahren

This draft Technical Specification is submitted to CEN members for Vote. It has been drawn up by the Technical Committee

CEN/TC 336.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, 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 Technical Specification. It is distributed for review and comments. It is subject to change

without notice and shall not be referred to as a Technical Specification.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprCEN/TS 17482:2020 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
kSIST-TS FprCEN/TS 17482:2020
FprCEN/TS 17482:2020 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

1 Scope .................................................................................................................................................................... 4

2 Normative references .................................................................................................................................... 4

3 Terms and definitions ................................................................................................................................... 4

4 Principle ............................................................................................................................................................. 4

5 Products and reagents ................................................................................................................................... 4

6 Apparatus ........................................................................................................................................................... 5

7 Sampling ............................................................................................................................................................. 5

8 General instructions....................................................................................................................................... 6

8.1 Preparation of the potentiometry apparatus and electrodes ......................................................... 6

8.2 Titration of the solution of alcoholic potassium hydroxide and blank test ............................... 6

8.3 Operating procedure ..................................................................................................................................... 6

9 Operating procedure ..................................................................................................................................... 6

9.1 Titration of the solution of alcoholic potassium hydroxide and blank test ............................... 6

9.2 Titration of the bitumen ............................................................................................................................... 7

10 Calculations ....................................................................................................................................................... 8

11 Expression of results ...................................................................................................................................... 8

12 Precision ............................................................................................................................................................. 8

12.1 Repeatability ..................................................................................................................................................... 8

12.2 Reproducibility ................................................................................................................................................ 9

13 Test report ......................................................................................................................................................... 9

Annex A (informative) Method for using a manual titration apparatus ................................................. 10

A.1 General ............................................................................................................................................................. 10

A.2 Operating procedure .................................................................................................................................. 10

Bibliography ................................................................................................................................................................. 13

---------------------- Page: 4 ----------------------
kSIST-TS FprCEN/TS 17482:2020
FprCEN/TS 17482:2020 (E)
European foreword

This document (FprCEN/TS 17482:2020) has been prepared by Technical Committee CEN/TC 336

“Bituminous binders”, the secretariat of which is held by AFNOR.
This document is currently submitted to the Vote on TS.
---------------------- Page: 5 ----------------------
kSIST-TS FprCEN/TS 17482:2020
FprCEN/TS 17482:2020 (E)
1 Scope

This document describes a method for the determination of the free acidic constituents present in

bitumen, conventionally known as acid number.

WARNING — The use of this document may involve hazardous materials, operations and equipment. This

document does not purport to address all of the safety problems associated with its use. It is the

responsibility of the user of this document to establish appropriate safety and health practices and to

determine the applicability of regulatory limitations prior to use.
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.

EN 58, Bitumen and bituminous binders — Sampling bituminous binders
EN 12594, Bitumen and bituminous binders — Preparation of test samples
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:

— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at http://www.iso.org/obp
3.1
acid number

number of milligrams of potassium hydroxide necessary for the neutralization of the free acids contained

in one gram of bitumen
3.2
equivalence point

stage of the titration procedure at which the added volume (equivalent volume) of titration reagent has

allowed to neutralize the acid compounds of the test sample

Note 1 to entry: In potentiometric titrations, this point corresponds to the inflexion point of the potential curve.

4 Principle

The bitumen is dissolved in a solvent-alcohol mixture. The acidic constituents are titrated using a solution

of alcoholic potassium hydroxide. The titration is monitored by potentiometry.
5 Products and reagents
5.1 General
Only use reagents of a quality recognized for analysis.
5.2 Potassium hydroxide RP (analytical grade), in pellets.
5.3 Propan-2-ol (isopropanol) RP (analytical grade).
---------------------- Page: 6 ----------------------
kSIST-TS FprCEN/TS 17482:2020
FprCEN/TS 17482:2020 (E)
5.4 Solvent RP (analytical grade), xylene or methyl benzene (toluene).
5.5 Benzoic acid RP (analytical grade).
5.6 Solution of alcoholic potassium hydroxide, 0,1 mol/L.

Dissolve (6 ± 0,2) g of potassium hydroxide pellets (5.2) in 1 L of pure propan-2-ol (5.3).

A ready-for-use, off-the-shelf solution can also be used. Only a titration certificate coming from an

authorized supplier can avoid the titration procedure (9.1). The alcoholic potassium hydroxide solution

shall be kept in brown glass containers and stored in the dark.
6 Apparatus
6.1 General
Usual laboratory equipment, together with the following.
6.2 Balance of adequate capacity for weight with precision of ± 1 mg.
6.3 Potentiometry apparatus, for automatic or manual titration:

— apparatus for automatic titration, including a titration device with sensitivity of at least 2 mV,

equipped with an automatic dosage unit with a capacity of 5 mL to 20 mL. Most of these pieces of

equipment offer a program for potentiometric detection with dynamic equivalence point titration. It

means that increment is slowed down near the equivalence point;

— apparatus for manual titration, including a potentiometer with a sensitivity of at least 2 mV and a

burette with a pointed spout.

The equipment shall allow titration steps to be performed at an accuracy of at least ± 0,05 mL in volume.

6.4 Glass combination electrode – Ag/AgCl.

6.4.1 A pH glass electrode for non-aqueous media and a reference electrode of Ag/AgCl (kept in its

inner reference electrolyte).

6.4.2 Combined pH electrode for non-aqueous media instead of the two electrodes cell of 6.4.1.

6.5 Glass beakers, or any glass titration container, specific for the automatic potentiometric titration

device (6.3).

The volume of beakers shall be appropriate for immersing the membrane of electrodes into the tested

solution and shall allow increasing this volume during titration.

The level of solution in the beaker shall be below the filling hole of the electrodes but has to be high

enough to prevent the stirring bar (if it is necessary to use it) from hitting the membranes if the electrodes

have to be close to the bottom of the beaker.
6.6 Magnetic stirrer, with polytetrafluoroethylene (PTFE)-coated bar.
7 Sampling

Take the sample in accordance with EN 58. Prepare the test samples in accordance with EN 12594.

---------------------- Page: 7 ----------------------
kSIST-TS FprCEN/TS 17482:2020
FprCEN/TS 17482:2020 (E)
8 General instructions
8.1 Preparation of the potentiometry apparatus and electrodes
The titration device shall be prepared following manufacturer instructions.

Special attention shall be paid to the storing and maintenance of the electrodes:

— before using, the inner body shall be filled with the electrolyte. If necessary, refill and let the electrode

to rest for at least one hour immersed in the reference electrolyte;

— before each titration, let the electrode to rest for at least 5 min immersed in the reference electrolyte;

— when the test is finished, the electrodes shall be cleaned with the solvent (5.4), then rinsed with

water, and finally stored according to the recommendations of the supplier.
8.2 Titration of the solution of alcoholic potassium hydroxide and blank test
The soluti
...

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