Bsi bs en 12592 2014 (bs 2000 47 2014)

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 2015 and conflicting national

BSI Standards Publication

BS EN 12592:2014

BS 2000-47:2014

Bitumen and bituminous binders — Determination of solubility

National foreword

This British Standard is the UK implementation of EN 12592:2014

It supersedes BS EN 12592:2007 which is withdrawn

The UK participation in its preparation was entrusted to Technical Committee PTI/13, Petroleum Testing and Terminology

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 2014

Published by BSI Standards Limited 2014 ISBN 978 0 580 77112 5

ICS 75.140; 91.100.50

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 2014

BS 2000 Series

Energy Institute, under the brand of IP, publishes and sells all Parts of BS 2000, and all BS EN and BS ISO petroleum test methods that would be part of BS 2000, both in its annual publication “IP Standard Test Methods for analysis and testing

of petroleum and related products, and British Standard 2000 Parts” and individually

Amendments/corrigenda issued since publication

EUROPEAN STANDARD

NORME EUROPÉENNE

EUROPÄISCHE NORM

EN 12592

November 2014

English Version

Bitumen and bituminous binders - Determination of solubility

Bitumes et liants bitumineux - Détermination de la solubilité Bitumen und bitumenhaltige Bindemittel - Bestimmung der

Löslichkeit

This European Standard was approved by CEN on 16 August 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

C O M I T É E U R O P É E N D E N O R M A L I S A T I O N

E U R O P Ä I S C H E S K O M I T E E F Ü R N O R M U N G

CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2014 CEN All rights of exploitation in any form and by any means reserved

worldwide for CEN national Members

Ref No EN 12592:2014 E

Contents Page

Foreword 3

1 Scope 4

2 Normative references 4

3 Terms and definitions 4

4 Principle 4

5 Reagents and materials 4

6 Apparatus 5

7 Sampling 5

8 Procedure 5

8.1 Test conditions 5

8.2 Preparation of crucible 6

8.3 Test method 6

9 Calculation 6

10 Expression of results 7

11 Precision 7

11.1 Repeatability 7

11.2 Reproducibility 7

12 Test report 7

Bibliography 9

BS EN 12592:2014

EN 12592:2014 (E)

3

Foreword

This document (EN 12592:2014) has been prepared by Technical Committee CEN/TC 336 “Bituminous binders”, 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 May 2015 and conflicting national standards shall be withdrawn at the latest by May 2015

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 12592:2007

In comparison with EN 12592:2007, the following significant changes have been made:

— changed/added wording of the Warning in the Scope;

— the function of the powdered glass (subclause 6.1.2) as filter aid has been highlighted in the standard;

— preparation of the test sample according to EN 12594 in subclause 8.3 has been added

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

1 Scope

This European Standard specifies a method for determining the degree of solubility of bituminous binders having little or no mineral matter other than recovered bituminous binders from asphalt mixes, in a specific solvent Toluene is used as the solvent for reference tests

NOTE Bituminous binders will have varying solubility in different solvents

WARNING — Use of this European Standard can involve hazardous materials, operations and equipment This European Standard does not purport to address all of the safety problems associated with its use It is the responsibility of the user of this European Standard to identify the hazards and assess the risks involved in performing this test method and to implement sufficient control measures

to protect individual operators (and the environment) This includes appropriate safety and health practices and determination of the applicability of regulatory limitations prior to use

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 58, Bitumen and bituminous binders — Sampling bituminous binders

EN 1425, Bitumen and bituminous binders — Characterization of perceptible properties

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

ISO 4793, Laboratory sintered (fritted) filters — Porosity grading, classification and designation

ISO 5272, Toluene for industrial use — Specifications

ISO 5280, Xylene for industrial use — Specification

3 Terms and definitions

For the purposes of this document, the following term and definition apply

3.1

solubility

portion of material that is soluble in a specific solvent

4 Principle

A sample of bituminous binder is dissolved in a solvent The solution is filtered through a layer of powdered glass in a sintered crucible The insoluble material is then washed, dried, and weighed

5 Reagents and materials

Examples of specific solvents are given in 5.1 and 5.2

5.1 Toluene, conforming to ISO 5272

BS EN 12592:2014

EN 12592:2014 (E)

5

5.2 Xylene, conforming to ISO 5280

6 Apparatus

Usual laboratory apparatus and glassware, together with the following:

6.1 Filtering apparatus

NOTE Assembled as illustrated in Figure 1 Details of the component parts are as given in 6.1.1 to 6.1.5

6.1.1 Sintered glass crucible, porosity P4 (see ISO 4793), effective diameter approximately 30 mm

6.1.2 Powdered glass, borosilicate glass powder, particle diameter approximately between 50 µm and

80 µm The powdered glass functions as filter aid

The granulometry of powdered glass may evolve over time It is recommended to check the granulometry prior to using the powdered glass, if used

Instead of powdered glass, glass fibre or Whatman filter grade 934 or equivalent may also be used However, the use of powdered glass is the reference method When using glass wool or filter as filter aid, a Gooch crucible may also be used

6.1.3 Filter flask, 250 ml or 500 ml, heavy-wall, with a side tube

6.1.4 Filter tube, 40 mm to 42 mm inside diameter

6.1.5 Rubber tubing or adaptor, for holding the crucible on the filter tube

Other suitable assemblies permitting vacuum filtration with a crucible can be used

6.2 Oven, capable of maintaining a temperature, T, of 15 °C to 25 °C above the boiling temperature of the

selected solvent

6.3 Balance, accurate to 0,2 mg and readable to 0,1 mg

7 Sampling

Take the test sample in accordance with EN 58, taking all necessary safety precautions and ensuring that the test sample is representative of the laboratory sample from which it is taken Ensure that the laboratory sample is homogenous and not contaminated (see EN 1425) If the sample contains water, heat a representative portion of between 100 g and 200 g at a temperature not exceeding 130 °C stirring constantly until the binder ceases to foam

8 Procedure

8.1 Test conditions

Normally the temperature at which the test is run is not critical and may be performed at the laboratory air temperature For reference tests, the flask with the sample in solution shall be placed in a water bath maintained at (25 ± 2) °C for 1 h before filtering

Crystallized paraffins may disturb the analysis of the samples with high wax content To avoid this, use the higher test temperature of 40 °C

8.2 Preparation of crucible

Weigh (3,0 ± 0,1) g of clean dried powdered glass into the crucible Place the crucible in the filter tube (6.1.4) Wash the powdered glass (6.1.2) with a small portion of the selected solvent (see Clause 5) and filter carefully into the flask with or without vacuum, as necessary Repeat the washing process several times Place the

crucible on a heater or steam bath for 30 min before placing in the oven (6.2) at the temperature T (see 6.2)

for at least 20 min Remove the crucible from the filter tube and cool in a desiccator for 25 min to 35 min and determine the mass to the nearest 0,1 mg Repeat the drying and weighing until constant mass is obtained, i.e the difference between the two weights shall not exceed 0,5 mg

8.3 Test method

Prepare the test sample according to EN 12594 in order to homogenize it and transfer (2 ± 1) g of the dry sample, if necessary, using a warmed knife, into a suitable weighed container, e.g Erlenmeyer flask

Determine the mass of the container and sample to the nearest 1 mg Add 100 ml of the selected solvent to the container in small portions with continuous agitation until all lumps disappear and no undissolved sample adheres to the container For reference testing stopper or cover the container and set aside for at least 15 min (see 8.1)

Place the previously prepared and weighed crucible in the filter tube (6.1.4) Wet the powdered glass with a small portion of solvent and filter the solution carefully into the flask through the powdered glass of the crucible with or without vacuum as necessary If the insoluble matter is appreciable, retain as much of it as possible in the container until the solution has drained through the filter aid Wash the container with a small amount of solvent and, using a stream of solvent from a wash bottle, transfer all insoluble matter to the crucible If necessary use a glass rod to remove any insoluble matter adhering to the container and transfer it into the crucible Thoroughly rinse the glass rod and container and transfer it with the crucible

Wash the insoluble matter in the crucible with solvent until the filtrate flows substantially colourless, then apply strong vacuum to remove the remaining solvent or place the crucible into a vacuum desiccator Remove the crucible from the tube or desiccator, wash the bottom free of any dissolved matter, and place the crucible on a

heater or a steam bath for 30 min Place in an oven at the temperature T (see 6.2) for at least 20 min

Remove the crucible from the filter tube and cool in a desiccator for 25 min to 35 min and determine the mass

to the nearest 0,1 mg Repeat the drying and weighing until constant mass is obtained, i.e the difference between the two weights is not more than 0,5 mg

Repeat the determinations, making at least two valid determinations Two solubility determinations shall be considered valid if they do not differ by more than 0,2 % mass

9 Calculation

Calculate either the total mass percentage of insoluble matter (x i) or the mass percentage of soluble matter

(x s), of the sample in the solvent as follows:

100

B

A











= m m

















−

B

A

where

xi is the percentage of insoluble matter, in percent;

BS EN 12592:2014

EN 12592:2014 (E)

7

xs is the percentage of soluble matter, in percent;

mA is the mass of insoluble material, in grams;

mB is the mass of the dry sample, in grams

10 Expression of results

Express the solubility as the percentage of mass of soluble material xs, to the nearest 0,05 %, as the mean of the two valid determinations

11 Precision

11.1 Repeatability

The difference between two test results, obtained by the same operator with the same apparatus under constant operating conditions on identical test material would, in the long run, in the normal and correct operation of the test method, exceed 0,10 % absolute in only one case in twenty

11.2 Reproducibility

The difference between two single and independent results obtained by different operators working in different laboratories on identical test material would, in the long run, in the normal and correct operation of the test method, exceed 0,15 % absolute in only one case in twenty

These precision data are not automatically applicable to modified bitumen, and for modified bitumen, they should only be used for guidance until criteria data are available

12 Test report

The test report shall contain at least the following information:

a) type and complete identification of the sample under test;

b) reference to this European Standard;

c) solvent used;

d) results obtained (see Clause 10);

e) any deviation, by agreement or otherwise, from the procedure specified;

f) date of the test;

g) type of filtrating medium (glass powder, glass fibre, filter) used

Key

3 filter tube

5 filter flask

Figure 1 — Filtering apparatus assembly

BS EN 12592:2014

EN 12592:2014 (E)

9

Bibliography

[1] ASTM D2042-01, Standard Test Method for Solubility of Asphalt Materials in Trichloroethylene

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