BS/EN 12592-2014 pdf download.Bitumen and bituminous binders – Determination of solubility.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are indispensable foi 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 (frEtted) filters — Porosity grading, classification and designation
ISO 5272. Toiuene for industnal 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.
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 .1 and 5.2.
5.1 Toluene, conforming to ISO 5272.
6.1.2 Powdered glass. borosilicate glass powder, partide diameter approximately between 50 pm and
80 pm. 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 oi 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 ponion 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 mm before placing in the oven (6.2) at the temperature T (see 6.2) for at least 20 mm. Remove the crucible from the filter tube and cool In a desiccator for 25 mm to 3.5 mm and determine the mass to the nearest 0.1 mg. Repeat the drying and weighing until constant mass is obtained, Le. 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 mm (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 mm. Place in an oven at the temperature T (see 6.2) for at least 20 mm. Remove the crucible from the filter tube and cool in a desiccator for 25 mm to 35 mm 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.BS/EN 12592-2014 pdf download.