BS EN 933‑9:2022

BSI Standards Publication

Tests for geometrical properties of aggregates

Part 9: Assessment of fines — Methylene blue test

BS EN 933‑9:2022 BRITISH STANDARD

National foreword
This British Standard is the UK implementation of EN 933‑9:2022. It
supersedes BS EN 933‑9:2009+A1:2013, which is withdrawn.
The UK participation in its preparation was entrusted to Technical
Committee B/502/6, Test methods.
A list of organizations represented on this committee can be obtained on
request to its committee manager.
Contractual and legal considerations
This publication has been prepared in good faith, however no
representation, warranty, assurance or undertaking (express or
implied) is or will be made, and no responsibility or liability is or will be
accepted by BSI in relation to the adequacy, accuracy, completeness or
reasonableness of this publication. All and any such responsibility and
liability is expressly disclaimed to the full extent permitted by the law.
This publication is provided as is, and is to be used at the
recipient’s own risk.
The recipient is advised to consider seeking professional guidance with
respect to its use of this publication.
This publication is not intended to constitute a contract. Users are
responsible for its correct application.
© The British Standards Institution 2022
Published by BSI Standards Limited 2022
ISBN 978 0 539 04124 8
ICS 91.100.15
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 31 March 2022.

Amendments/corrigenda issued since publication

Date Text affected
 BS EN 933‑9:2022

EUROPEAN STANDARD EN 933-9

NORME EUROPÉENNE
EUROPÄISCHE NORM February 2022

ICS 91.100.15 Supersedes EN 933-9:2009+A1:2013

English Version

Tests for geometrical properties of aggregates - Part 9:

Assessment of fines - Methylene blue test
Essais pour déterminer les caractéristiques Prüfverfahren für geometrische Eigenschaften von
géométriques des granulats - Partie 9 : Qualification Gesteinskörnungen - Teil 9: Beurteilung von
des fines - Essais au bleu de méthylène Feinanteilen - Methylenblau-Verfahren

This European Standard was approved by CEN on 10 January 2022.

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, 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

© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 933-9:2022 E
worldwide for CEN national Members.
BS EN 933‑9:2022
EN 933-9:2022 (E)

Contents Page

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

1 Scope ........................................................................................................................................................ 5
2 Normative references........................................................................................................................ 5
3 Terms and definitions ....................................................................................................................... 5
4 Principle ................................................................................................................................................. 6
5 Reagents ................................................................................................................................................. 6
6 Apparatus .............................................................................................................................................. 7
7 Preparation of test portion.............................................................................................................. 8
7.1 General.................................................................................................................................................... 8
7.2 Preparation without pre-drying .................................................................................................... 8
7.3 Preparation with pre-drying .......................................................................................................... 9
8 Procedure .............................................................................................................................................. 9
8.1 Preparation of suspension .............................................................................................................. 9
8.2 Stain test ................................................................................................................................................. 9
Figure 1 — Flow chart of test procedure ............................................................................................... 11
9 Calculation and expression of results....................................................................................... 12
10 Test report.......................................................................................................................................... 12
10.1 Required data .................................................................................................................................... 12
10.2 Optional data ..................................................................................................................................... 13
Annex A (normative) Determination of the methylene blue value of the size 0/0,125 mm
fraction (MBF) .................................................................................................................................... 14
A.1 Procedure ........................................................................................................................................... 14
A.2 Calculation and expression of results....................................................................................... 14
A.3 Test report.......................................................................................................................................... 14
Annex B (normative) Preparation of 10 g/l methylene blue solution ..................................... 15
B.1 Procedure ........................................................................................................................................... 15
B.2 Storage ................................................................................................................................................. 16
Annex C (normative) Determination of the methylene blue value of kaolinite (MBK)....... 17
C.1 General................................................................................................................................................. 17
C.2 Procedure ........................................................................................................................................... 17
C.3 Calculation and expression of results....................................................................................... 17
Annex D (informative) Test of conformity in relation to a specified MB value ...................... 18
Annex E (informative) Example of a test data sheet ......................................................................... 19

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European foreword

This document (EN 933-9:2022) has been prepared by Technical Committee CEN/TC 154 “Aggregates”,
the secretariat of which is held by BSI.

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 August 2022, and conflicting national standards shall
be withdrawn at the latest by August 2022.

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.

This document supersedes EN 933-9:2009+A1:2013.

In comparison with the previous edition, the following technical modifications have been made:

a) Normative references has been extended with EN 933-2 which is referenced in 6.1.7 Test sieves;

b) Terms and definitions has been extended with the definition of laboratory sample;

c) Clause 6 Apparatus has been restructured into two subclauses (6.1 general and 6.2 special), due to
special apparatus (tinted glass bottle) used in former Annex C;

d) the test sieves in 6.1.7 are extended with 0,125 mm, which is used in normative Annex A;

e) the note in former Clause 6.4 about alternative types of mixers has been transformed to main text;

f) pre-drying temperature has been increased to (110 ± 5) °C for natural and manufactured
aggregates (Clause 7) and the clause has been divided into General, Preparation without pre-drying
and Preparation with pre-drying;

g) the procedure has been clarified with restructured text and an illustrating figure (Clause 8);

h) the Scope, the Terms and definitions and the Test report content have been adapted to the current
rules and the text has been clarified;

i) the order of annexes has been changed, to place the normative annexes first;

j) the note in former Annex D, containing recommendations about checking of MBK, has been
transformed to main text in a new Clause C.1 General;

k) Annex A and former Annexes C and D have been restructured;

l) the titles of Annex A and former Annex D have been shortened;

m) the row numbers in Annex E have been deleted.

This document forms part of a series of tests for geometrical properties of aggregates. Test methods for
other properties of aggregates are covered by the following European Standards:

— EN 932 (all parts), Tests for general properties of aggregates

— EN 1097 (all parts), Tests for mechanical and physical properties of aggregates

— EN 1367 (all parts), Tests for thermal and weathering properties of aggregates

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— EN 1744 (all parts), Tests for chemical properties of aggregates

— EN 13179 (all parts), Tests for filler aggregate used in bituminous mixtures

The other parts of EN 933 include:

— Part 1: Determination of particle size distribution — Sieving method

— Part 2: Determination of particle size distribution — Test sieves, nominal size of apertures

— Part 3: Determination of particle shape — Flakiness index

— Part 4: Determination of particle shape — Shape index

— Part 5: Determination of percentage of crushed and broken surfaces in coarse aggregate particles

— Part 6: Assessment of surface characteristics — Flow coefficient of aggregates

— Part 7: Determination of shell content — Percentage of shells in coarse aggregates

— Part 8: Assessment of fines — Sand equivalent test

— Part 10: Assessment of fines — Grading of filler aggregates (air jet sieving)

— Part 11: Classification test for the constituents of coarse recycled aggregate

Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.

According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: 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.

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1 Scope
This document specifies the reference method used for type testing and in cases of dispute, for the
determination of the methylene blue value of the size 0/2 mm fraction in fine aggregates or all-in
aggregates (MB). It also specifies the reference method for the determination of the methylene blue
value of the size 0/0,125 mm fraction (MBF) in normative Annex A. Other methods can be used for other
purposes, such as factory production control, provided that an appropriate working relationship with
the suitable reference method has been established.
Annex B specifies the preparation of 10 g/l methylene blue solution and Annex C specifies the
procedure for the determination of the methylene blue value of kaolinite (MBk). Annexes B and C are
normative.
A conformity check, adding a single quantity of dye solution equivalent to a specified limiting value and
which can be used as part of a production control process, is described in informative Annex D.
An example of a test data sheet is given in informative Annex E.
WARNING – The use of this part of EN 933 can involve hazardous materials, operations and equipment
(such as dust, noise and heavy lifts). It does not purport to address all of the safety or environmental
problems associated with its use. It is the responsibility of users of this document to take appropriate
measures to ensure the safety and health of personnel and the environment prior to application of the
standard, and fulfil statutory and regulatory requirements for this purpose.

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 932-2, Tests for general properties of aggregates - Part 2: Methods for reducing laboratory samples

EN 932-5, Tests for general properties of aggregates - Part 5: Common equipment and calibration

EN 933-2, Tests for geometrical properties of aggregates - Part 2: Determination of particle size
distribution - Test sieves, nominal size of apertures

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:
— ISO Online browsing platform: available at https://www.iso.org/obp/ui

— IEC Electropedia: available at https://www.electropedia.org/

3.1
laboratory sample
sample intended for laboratory testing

3.2
subsample
sample obtained by means of a sample reduction procedure

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3.3
test portion
d0/D0
sample used as a whole in a single test

3.4
fines
particle size fraction of an aggregate which passes the 0,063 mm sieve

3.5
particle size fraction
di/Di
fraction of an aggregate passing the larger (Di) of two sieves and retained on the smaller (di)

Note 1 to entry: The lower limit can be zero.

3.6
constant mass
mass determined after successive weighings at least 1 h apart not differing by more than 0,1 %

Note 1 to entry: In many cases constant mass can be achieved after a test portion has been dried for a pre-
determined period in a specified oven at (110 ± 5) °C. Test laboratories can determine the time required to achieve
constant mass for specific types and sizes of sample dependent upon the drying capacity of the oven used.

4 Principle
Increments of a methylene blue solution are added successively to a test portion suspended in water.
The adsorption of dye solution, by potential clay minerals in the test portion, is checked after each
addition of solution. This is done by carrying out a stain test on filter paper to detect the presence of
free dye, which indicates that adsorption is complete.
When the presence of free dye is confirmed, the methylene blue value (MB or MBF) is calculated and
expressed as grams of dye adsorbed per kilogram of the size fraction tested.
NOTE A conformity check, adding a single quantity of dye solution equivalent to a specified limiting value,
and which can be used as part of a production control process, is described in Annex D.

5 Reagents
5.1 Dye solution, solution of standard or technical quality methylene blue, (10,0 ± 0,1) g/l (see
Annex B). The solution shall not be used more than 28 days after preparation. It shall be stored in a dark
place.

5.2 Distilled or demineralized water.

5.3 Kaolinite, of known methylene blue value MBK (see Annex C).

NOTE Kaolinite of MBK value between 1 g and 2 g per 100 g of kaolinite is preferable in order to avoid
excessive use of dye.

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6 Apparatus
All apparatus, unless otherwise stated, shall conform to the general requirements of EN 932-5.
6.1 Apparatus for general purposes

6.1.1 Burette, pipette, micro pipette or bottle top dispenser, capable of delivering a volume of 5 ml
and 2 ml with an accuracy of 0,2 ml.

6.1.2 Filter paper, quantitative and ash-free (<0,010 %); 95 g/m2; thickness 0,20 mm; filtration
speed 75 s; pore size 8 µm.

6.1.3 Glass rod, length 300 mm; diameter 8 mm.

6.1.4 Impeller agitator, capable of controlled variable rotation rates up to (600 ± 60) r/min with
three or four impeller blades of (75 ± 10) mm diameter. Other types of mixers that have been shown to
produce the same results may be used.

6.1.5 Balance, accurate to 0,1 % of the mass of the test portion.

6.1.6 Timer.

6.1.7 Test sieves, 0,125 mm and 2 mm, with apertures as specified in EN 933-2, with guard sieve (if
necessary).

6.1.8 Sieve brush.

6.1.9 Beaker, glass or plastic, capacity of about 1 l or about 2 l.

6.1.10 Flask, glass, capacity of 1 l.

6.1.11 Ventilated oven, capable of maintaining a temperature of (110 ± 5) °C.

6.1.12 Thermometer, accurate to 1 °C.

6.1.13 Spatula.

6.1.14 Desiccator.

6.2 Special apparatus for the preparation of 10 g/l methylene blue solution (Annex B)

6.2.1 Tinted glass bottle.

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7 Preparation of test portion

7.1 General

The test portion shall consist of at least 200 g of particle size fraction 0/2 mm. It may be prepared using
pre-dried or not pre-dried material.
When testing a non-pre-dried material, a correction of the mass with respect to the water content is
necessary. Thus, the water content shall be determined in this case.
The preparation without pre-drying is described in 7.2 and the preparation with pre-drying is described
in 7.3.
All masses shall be determined to the nearest 1 g.
7.2 Preparation without pre-drying

Reduce the laboratory sample in accordance with EN 932-2 to produce two subsamples, each containing
at least 200 g of particle size fraction 0/2 mm.
NOTE 1 One subsample is aimed for determining the water content in order to calculate the dry mass M1 of the
test portion. In this way the test portion used for the MB determination is not exposed for any heating.

Sieve the subsamples on a 2 mm sieve, protected if necessary by a guard sieve, e.g. 4 mm, and using a
sieve brush to ensure effective separation and collection of all particles in the size 0/2 mm fraction.
Discard any particles retained on the 2 mm sieve.
Determine the water content W by weighing one of the sieved subsamples, M. Dry it to constant mass,
and weigh it again as M’. Calculate and record W according to Formula (1), and discard this subsample.

= 100 ×
W
( M − M ') (1)
M'
where
W is the water content, in percent (%);
M is the mass of the sieved subsample, in grams (g);
M’ is the mass of the sieved subsample dried to constant mass, in grams (g).

NOTE 2 The water content determination can be achieved by other means than drying in a ventilated oven,
such as drying in a microwave for example.

Take the second sieved subsample and, if necessary, achieve further reduction in accordance with EN
932-2. Sample reduction shall yield a test portion size which is larger than [200 ⨉ (1 + W/100)] g, but
not of an exact predetermined value.
Weigh the test portion as M0 and calculate M1 (dry mass), according to Formula (2):
M0
M1 = (2)
1 + (W /100)

where
M1 is the dry mass of the test portion, in grams (g);
M0 is the mass of the test portion, in grams (g);
W is the water content determined on the other subsample, in percent (%).

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7.3 Preparation with pre-drying

Reduce the laboratory sample in accordance with EN 932-2 to yield a test portion size which is larger
than the minimum, but not of an exact predetermined value.
Dry the sample to constant mass, at (110 ± 5) °C in the case of natural and manufactured aggregates,
and at less than 45 °C in the case of other type of aggregates.
Sieve the sample on a 2 mm sieve, protected if necessary by a guard sieve, e.g. 4 mm, and using a sieve
brush to ensure effective separation and collection of all particles in the size 0/2 mm fraction. Discard
any particles retained on the 2 mm sieve.
Weigh the obtained test portion as M1.

8 Procedure

8.1 Preparation of suspension

Place (500 ± 5) ml of distilled or demineralized water in the beaker (6.1.9) and add the test portion
while stirring well with the spatula (6.1.13).
Stir the dye solution (5.1) or alternatively mix it thoroughly. Fill the burette (6.1.1) with dye solution
and return the stock of dye solution to a dark place.
Set the agitator (6.1.4) to a speed of 600 r/min and position the impeller about 10 mm above the base
of the beaker. Switch on the agitator and start the timer (6.1.6), agitating the contents of the beaker for
5 min at (600 ± 60) r/min.
Reduce the speed of the agitator to (400 ± 40) r/min and agitate continuously for the remainder of the
test.
If insufficient fines are present in the test portion to obtain a halo (see 8.2), kaolinite shall be added
together with additional dye solution as follows:
— add to the beaker (30,0 ± 0,1) g of kaolinite (5.3), dried at (110 ± 5) °C to constant mass;

— add V´ ml of dye solution to the beaker, where V´ = 30 MBK, i.e. the volume of dye solution adsorbed
by 30 g of kaolinite.

8.2 Stain test

Place a filter paper (6.2) on top of an empty beaker, or some other suitable support, so that most of its
surface is not in contact with any solid or liquid.
Add a dose of 5 ml of dye solution into the beaker with the suspension and agitate at (400 ± 40) r/min
for at least 1 min.
Apply a drop of the dyed suspension on the filter paper (6.1.2) by means of the glass rod (6.1.3). The
stain formed on the filter paper is composed of a central deposit of material, of a generally solid blue
colour, surrounded by a colourless wet zone. The amount of drop applied shall be such that the diameter
of the deposit is between 8 mm and 12 mm. If this is not fulfilled, a new drop shall be applied.
The test result is said to be positive if, in the wet zone, a halo consisting of a light blue ring of about
1 mm is formed around the central deposit and persists for 5 min. This detects the presence of free dye,
which indicates that adsorption is complete.
If the halo does not appear after the addition of the initial 5 ml of dye solution, add a further 5 ml of dye
solution, continue agitating for 1 min, and carry out another stain test.

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If a halo still does not appear, continue agitating, making additions of dye and doing stain tests as
described until a halo is observed.
When the halo appears, continue agitating and confirm the test end-point by repeating the stain test at
1 min intervals for 5 min, without adding more dye solution.
NOTE The halo can disappear again because the clay minerals’ adsorption of the dye can take some time to
complete.

If the halo disappears during the first 4 min of the confirmation period; add a further 5 ml of dye
solution. If the halo disappears during the fifth minute, add only 2 ml of dye solution. In either case,
continue agitating and doing stain tests until a halo persists for 5 min, corresponding to six consecutive
stains starting from the addition of methylene blue (Figure 1).
Record the total volume of dye solution V1 added to produce a halo that persists for 5 min, to the nearest
1 ml.
Containers used in methylene blue tests shall be reserved specifically for that test. They shall be
cleansed thoroughly with water as soon as the test is completed and traces of any detergents used
should be removed by thorough rinsing.

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Figure 1 — Flow chart of test procedure

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9 Calculation and expression of results

The methylene blue value MB, expressed in grams of dye per kilogram of the size 0/2 mm fraction, is
given by Formula (3):
V1
MB
= × 10 (3)
M1

where
V1 is the total volume of dye solution injected, in millilitres (ml);
M1 is the mass of the test portion, in grams (g).

Record the MB to the nearest 0,1 g of dye per kilogram of the size 0/2 mm fraction.
If the test is carried out with the addition of kaolinite, the MB is given by Formula (4):
V1 − V'
MB
= × 10 (4)
M1

where
V’ is the volume of dye solution adsorbed by the kaolinite, in millilitres.

NOTE 1 The factor 10 in Formulae 3 and 4 converts the volume of dye solution used to the mass of dye adsorbed
per kilogram of the size fraction tested.

NOTE 2 An example of a test data sheet is given in Annex E.

10 Test report

10.1 Required data

The test report shall include the following information:

a) reference to this document, including its year of publication;

b) identification of the laboratory;

c) identification of the laboratory sample, including the origin;

d) date of test;

e) size fraction of the aggregate;

f) the method used to determine and calculate the result (Clauses 8 and 9 or Annex A);

g) MB value or MBF value, as applicable with significant digits;

h) pre-drying temperature (if pre-dried);

i) any deviations from the procedure;

j) any unusual features observed.

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10.2 Optional data

The test report can include the following information:

a) reference to the chosen sampling procedure;

b) sampling certificate, if available;

c) laboratory sample reception date if different from sampling date;

d) reference to the chosen sample reduction procedure;

e) mass of the test portion;

f) other influencing parameters.

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Annex A
(normative)

Determination of the methylene blue value of the size 0/0,125 mm fraction

(MBF)

A.1 Procedure
Prepare test portions as specified in Clause 7 and follow the test procedure in Clause 8, but with a test
portion mass M1 of (30,0 ± 0,1) g of the size 0/0,125 mm fraction.

A.2 Calculation and expression of results

Calculate the methylene blue value of the size 0/0,125 mm fraction in accordance with Formula (A.1):
V1
MB
= F × 10 (A.1)
M1

where
MBF is the methylene blue value, in grams of dye per kilogram of the size 0/0,125 mm
fraction (g/kg);
V1 is the total volume of dye solution added, in millilitres (ml);
M1 is the mass of the test portion, in grams (g).

Record the MBF value to the nearest 0,1 g of dye per kilogram of the size 0/0,125 mm fraction.

A.3 Test report

The test report shall include appropriate information in accordance with Clause 10.

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Annex B
(normative)

Preparation of 10 g/l methylene blue solution

B.1 Procedure
Use methylene blue; (C16H18ClN3S, nH2O (n = 2 to 3) purity ≥ 96 %).
Determine the water content W of the methylene blue powder as follows:
Weigh approximately 5 g of methylene blue powder and record the mass to the nearest 0,01 g as Mh.
Dry this powder at (100 ± 5) °C to constant mass. Cool in the desiccator, and then weigh immediately
after taking out of the desiccator. Record the dry mass to the nearest 0,01 g as Mg.
NOTE At temperatures above 105 °C, methylene blue powder can be modified.

Calculate and record the water content W, rounded to one decimal place, from Formula (B.1):
Mh − Mg
=W × 100 (B.1)
Mg

where
Mh is the mass of the methylene blue powder, in grams (g);
Mg is the mass of the dried methylene blue powder, in grams (g).

The water content shall be determined for the preparation of every new batch of dye solution.
Take a mass of methylene blue powder of ((100 + W)/10) g ± 0,01 g (equivalent to 10 g of dry powder).
Warm 500 ml to 700 ml of distilled or demineralized water in a beaker to a temperature close to, but
not exceeding, 40 °C.
Agitate the contents of the beaker while slowly pouring the methylene blue powder into the warm
water. Continue to agitate for 45 min, until complete dissolution of the powder, and then allow to cool
to 20 °C.
Pour into a flask of capacity 1 l, rinsing with distilled or demineralized water to ensure complete
transfer of all dye into the flask. Make sure that the flask and the water are at a temperature of
(20 ± 1) °C to conform with the calibration of the flask and add more distilled or demineralized water
to the 1 l graduation mark.
Shake the flask to ensure complete dissolution of the powder and pour into a conservation bottle in
tinted glass.
The following details shall be marked on the conservation bottle:
a) 10 g/l methylene blue solution;
b) date of preparation;
c) limit date of use.

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B.2 Storage
Methylene blue solution shall not be used more than 28 days after preparation. The stock of dye solution
shall be stored in a dark place.

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Annex C
(normative)

Determination of the methylene blue value of kaolinite (MBK)

C.1 General
A test on kaolinite of known MBK value shall be carried out at regular intervals to check the constancy
of results. This procedure shall also be used to check a new dye solution.

C.2 Procedure
Dry the kaolinite at (110 ± 5) °C to constant mass.
Weigh (30,0 ± 0,1) g of dry kaolinite and pour it into the beaker (6.9) together with 500 ml of
demineralized or distilled water.
Agitate for 5 min at (600 ± 60) r/min with the impeller about 10 mm above the base of the container
and subsequently agitate continuously at (400 ± 40) r/min for the remainder of this determination.
Add a dose of 5 ml of 10 g/l dye solution into the beaker and, after at least 1 min of agitating at
(400 ± 40) r/min, carry out a stain test on the filter paper (see 8.2).
If necessary, continue to add dye solution in 5 ml doses until a positive result as described in 8.2 is
obtained.
NOTE The test result is said to be positive if, in the wet zone, a halo consisting of a light blue ring of about
1 mm is formed around the central deposit and persists for 5 min.

If the light blue ring disappears, add further dye solution as described in 8.2 until the determination is
complete.
Record the total volume of dye solution V’ added to produce a halo that persists for 5 min, to the nearest
1 ml.

C.3 Calculation and expression of results

Calculate and record the methylene blue value of the kaolinite to the nearest 0,1 g of dye per 100 g of
kaolinite from Formula (C.1):
MBK = V´ / 30 (C.1)
where
V’ is the total volume of dye solution adsorbed, in millilitres (ml).

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Annex D
(informative)

Test of conformity in relation to a specified MB value

A check on conformity with a specified MB value can be carried out by making a single addition of dye
solution in the following manner.
If the specified MB value is MB1, the volume V2 of dye solution to be added at one time, is given by
Formula (D.1):
MB1 × M 1
=V2 + V' (D.1)
10
where
MB1 is the specified MB value, in grams of dye per kilogram of the size 0/2 mm fraction
(g/kg);
M1 is the mass of the test portion, in grams (g);
V´ is the volume of dye solution adsorbed by any added kaolinite, in millilitres (ml).

After preparation of a test portion in accordance with Clause 7, prepare the suspension using the test
portion, the water and, if necessary the kaolinite, all in accordance with 8.1, but including V2 ml of dye
solution.
Carry out the stain test after stirring the suspension for 8 min at (400 ± 40) r/min. If the stain test is
positive (see 8.2), the aggregates can be assumed to conform to the specification.
NOTE The test result is said to be positive if, in the wet zone, a halo consisting of a light blue ring of about
1 mm is formed around the central deposit and persists for 5 min.

If the stain test is negative, carry out the complete determination described in 8.2.

18
 BS EN 933‑9:2022
EN 933-9:2022 (E)

Annex E
(informative)

Example of a test data sheet

EN 933-9 Laboratory:
Date:
Identification of the sample:
Operator:

Dry mass of test portion 0/2 mm (to nearest gram), M1 M1 = g

Volume of solution adsorbed by kaolinite (if used), V´ V´ = ml

Total amount of dye solution added, V1 V1 = ml

MB value, expressed in grams of dye per kilogram of the size 0/2 mm MB =

fraction (see Clause 9)

19
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