BS EN 12592:2014
BS 2000-47:2014
BSI Standards Publication
Bitumen and bituminous
binders — Determination of
solubility
BS EN 12592:2014
BRITISH STANDARD
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It supersedes BS EN 12592:2007 which is withdrawn.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
Date
Text affected
EN 12592
EUROPEAN STANDARD
NORME EUROPÉENNE
EUROPÄISCHE NORM
November 2014
ICS 75.140; 91.100.50
Supersedes EN 12592:2007
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
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
worldwide for CEN national Members.
Ref. No. EN 12592:2014 E
BS EN 12592:2014
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
8.1
8.2
8.3
Procedure ...............................................................................................................................................5
Test conditions ......................................................................................................................................5
Preparation of crucible ..........................................................................................................................6
Test method............................................................................................................................................6
9
Calculation ..............................................................................................................................................6
10
Expression of results ............................................................................................................................7
11
11.1
11.2
Precision .................................................................................................................................................7
Repeatability...........................................................................................................................................7
Reproducibility .......................................................................................................................................7
12
Test report ..............................................................................................................................................7
Bibliography ........................................................................................................................................................9
2
BS EN 12592:2014
EN 12592:2014 (E)
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.
3
BS EN 12592:2014
EN 12592:2014 (E)
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
4
Toluene, conforming to ISO 5272.
BS EN 12592:2014
EN 12592:2014 (E)
5.2
6
Xylene, conforming to ISO 5280.
Apparatus
Usual laboratory apparatus and glassware, together with the following:
6.1
Filtering apparatus
NOTE
6.1.1
Assembled as illustrated in Figure 1. Details of the component parts are as given in 6.1.1 to 6.1.5.
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
7
Balance, accurate to 0,2 mg and readable to 0,1 mg.
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
8.1
Procedure
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.
5
BS EN 12592:2014
EN 12592:2014 (E)
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 (xi) or the mass percentage of soluble matter
(xs), of the sample in the solvent as follows:

x i =  mA
 × 100
m
B

(1)

 × 100
xs = 100 −  mA


m
B

(2)
where
xi
6
is the percentage of insoluble matter, in percent;
BS EN 12592:2014
EN 12592:2014 (E)
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.
7
BS EN 12592:2014
EN 12592:2014 (E)
Key
1
sintered glass crucible
2
rubber tubing
3
filter tube
4
polychloroprene stopper
5
filter flask
Figure 1 — Filtering apparatus assembly
8
BS EN 12592:2014
EN 12592:2014 (E)
Bibliography
[1]
ASTM D2042-01, Standard Test Method for Solubility of Asphalt Materials in Trichloroethylene
9
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