.

STANDARDIZATION AND QUALIFICATION OF FINES

IN AGGREGATES IN FRANCE

A. MALDONADO1 , S. ORSETTf, C. TOURENQ3

Abstract:

The qualification of fines included in a sand is necessary for the engineer who wishes to
forecast the characteristics of the manufactured concrete. The authors present two french
methods concerning successively the pollutions by clay and sulfate depending on the origin of
the materials.

. Introduction

The qualification of fines in a sand or a material O/D is a necessity. The civil engineer generally
wishes to adapt the quality of the components of a concrete to the quality of the finished
structure. Depending on their origin, fines consist of materials which react in the presence of
water and modify the properties of the produced concrete.

The problem for the engineer is thus to identify and to control the amount of fines, which may
be regarded as contamination in the materials used, with the aim of not wasting resources
which are becoming raiein certain regions. -

Charg de Mission auprs du Directeur Technique Geotechnique - Directeur de Recherche

Laboratoire Central des Ponts et Chausses (LCPC)
58 boulevard Lefebvre
75732 PARIS CEDEX 15- France
T1. :33(1)4043 50 00 - Fax: 33 (1) 40 43 54 98
Thdsard
Laboratoire Central des Ponts et Chausses de Paris
3 chargd de Mission auprs du Directeur Technique Geotechnique
L Laboratoire Central des Ponts et Chausses de Paris
 We shall be considering below:

- the problems encountered with natural sands:

* the sand equivalent test generally used to quantify clayey fines in a sand,
associated with the methylene blue test,

- the problems raised by gypsum in demolition concrete:

* the method under study which will allow fast determination of calcium
sulfates in recycled materials.

I- Mechanical strength of composite materials and cleanliness of fines

When using natural materials, civil engineers have generally been able to note the influence of
clay on the mechanical properties of produced concrete.

.
Percentcge of /lies c,idmecho'c/sfrength

The variation in the tensile strength of a composite material as a function of the percentage of
clayey or non-clayey fines is illustrated in figure 1.

The following may be noted:

- when the fines come from the crushing or grinding of unweathered natural rock,
tensile strength increases initially with the percentage of fines. It then decreases and loses
- 10-0/6 of its value when the proportion of flnesreaches 20

- on the other hand, when the fines are made up of kaolinite or montmorillonite, the
drop in strength is very fast. Less than 5 % fines is sufficient to cause a drop of 10 % in
strength. The higher the specific surface of the fines, the faster the loss of strength.

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Materials Crushed rock Kaolinite Montmorillonite

Total specific surface of 1 to 5 in 45 m/g 800 m2/g

fines

Percentage causing a drop of 18 6 2

10% in strength

Table 1: Percentage of fines and specific surface

1-2 Ths qu/iifiti /P5/$

France uses the sand equivalent (SE) test imported from the United States about 40 years ago.
The test consists in measuring, after suitable preparation, the ratio between the heights of the
sediment H2 and the sediment overlaid with a clayey flocculate of a sand sample (H1)
(figure-2).

.
E5= 100-

This test affords a very good idea of clay contamination. When the amount of clay is less than
3 %, the SE is higher than or equal to 70, corresponding to specifications intended for sand
used in hydraulic concrete.

The value of the SE however depends qualitatively and quantitatively on the fines content.
Fines from unweathered rocks cause the value of the SE to drop in the same manner as a small
amount of clayey fines. For example, a sample containing 5 % kaolinite yields an SE value of
42. This value is reached with 14 % fines coming from rock.

This small discrimination on the nature of contamination is a drawback in the optimum

management of natural resources. Thus, depending on the adopted specification thresholds (SE
= 70, 60, or 50), some supplies may be unjustifiably rejected (figure 3).

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/-J Ifethy/ene IVue test

It is thus important to be able to discriminate more precisely between fine particles having
different physico-chemical properties. How can clayey particles be differentiated from non-
clayey particles in a sand supply?

After fairly long studies, special efforts were made in France to make better use of the
methylene blue test.

The principle of this test is as follows: methylene blue fixes on the surface of particles by
absorption. The higher the specific surface of a sample, the mare methylene blue will be
required to "cover" the particles that it contains (table 1).

Figure 4 shows to what extent methylene blue is sensitive to the presence of clay and in
particular montmorillonite. A few percent of montmorillonite adsorbs several grams of blue.

Ii French,00sition ii the quo'/iTi'ctibii of 1117es

The foregoing observations explain why French engineers have chosen to combine the use of
the SE and the methylene blue test in natural resource management.

The SE is always carried out on sands and materials O/D to be acceptance tested. If the value
of the SE found is lower than the required specification, this may be due to:

- the presence of rock fines smaller than 15 or 10 p.m which do not affect the strength
of the concrete,

- a few percent of clay which, within a certain limit, also has no effect on strength.

The methylene blue test is then carried out. It will shed light on the poor value of the SE:
- the blue value is low because fines are not clayey or only slightly clayey and the
material can be used,

- the blue value is high (> 1) and the fines are clayey and the material must not be used.

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 The methylene blue test is easy to conduct. It is carried out on sand with its fines. It consists in
placing, in a beaker, enough sand to have more than 30 g of fines (:!^ 0.063 mm) to which is
added 500 ml of water, followed by stirring.

After a settlement period, a medicinal solution of methylene blue (10 g/l) is injected, this is
stirred, and a drop is taken and placed on a white filter paper. The stain is produced by the
deposit of colored materials (adsorbed methylene blue) surrounded by a colorless water halo.

Methylene blue is again added until the halo has a persistent blue color. The sample is then
saturated by the methylene blue. The amount of blue consumed is then noted and referred t
the weight of fines or sand introduced into the flask.

The blue value is expressed in grains of blue per kilogram of sand or fines.

The methylene blue test is covered by a French standard and repeatability and reproducibility
tests have been carried out (table 2). This can be accomplished by means of a turbidimeter, in
which case the method is clearly more precise.

1^1 Type of test

Methylene blue stain test (new
Repeatability Reproducibility
0.3 0.5
specification 1 to 2 g/100 g of fines)
SE (specification 50 to 70) 4 7

Table 2: Variances concerning qualification tests for fines and sands

II- Influence ofplasler on the sJveig of hydrcu/i 6i,c/er treotec' cab' untrectea' mofethls
- cose of o'emo/i7i'n concrete

The demolition of industrial or private buildings, but also of civil engineering structures, has
been increasing substantially owing to the age of structures or to new environmental concerns.

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The tonnage of waste or rubble from demolition is increasing not only in France but
throughout Europe. The amounts are acknowledged to represent from 20 to 25 million metric
tons, which may appear trivial compared with the 400 million metric tons of natural aggregates
extracted each year. These aggregates coming from demolition products are concentrated in
urban areas, where dumps are difficult to set up but also where needs are greatest.

Environmental constraints are responsible for growing demand aimed at allowing the re-use of
these materials. This being so, such materials compete with natural aggregates. It is thus
indispensable to find applications for them. In accomplishing this, it is important to ensure the
protection of the environment and proper resource management.

The recycling of such materials in roadbuilding or, still extremely rare, in concrete
construction, raises problems owing to the gypsum fraction (coming from plaster) which forms
an integral part of certain batches of rubble likely to reach the recycling sites.

The dissolution of gypsum in the indurated matrix after construction leads to the formation of
expansive minerals of the ettringite or thaumasite type which cause swelling responsible for
deformations and deterioration considered to be unacceptable. Water plays a primary role in
these disorders resulting from sulfate attack.

Considerable bibliographic and investigatory work was undertaken, considering the subject
from various viewpoints (technical, economic, legal, in terms of standards, pathological,
experimental).

To deal with the problems mentioned, the objectives of the work were as follows:

- working out of an inexpensive chemical method for fast sulfate analysis and detection
suited to worksite conditions,

- determination of the sulfate threshold as of which the disorders will appear, and this
according to the fields of application and re-use conditions,

- working out of a fast, simple and inexpensive method for determining the behavior of
the material,

- proposing solutions for inhibiting the appearance of disorders; knowledge of these

inhibiting mechanisms is important for understanding the reaction mechanisms.

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These objectives were approached and developed essentially on the basis of specific cases and
through the experimental preparation of mixes contaminated with gypsum as concerns the
experimental part.

I/-i. The su//cle on'si. mefhoo'

Conventional sulfate analysis reference methods require time (3 days). They are also costly
(from $100 to $360 for an analysis).

A need was thus felt for the development of a fast, simple and low-cost sulfate determination
method easily applicable in a worksite laboratory.

A spectro-photometric method was experimented. Sulfate content is based on the

measurement of the optical density of the BaSO4 precipitate which is formed in the analysis
tube between gypsum and the filters incorporated in the photometer guaranteeing good
measurement accuracy. Determinations are carried out on samples having a known sulfate
content.

The determination protocol includes:

- leaching of gypsum with hot water and agitation (15 mm.),

- fast filtration (3 mm.),
- a rest period (190 mm.),
- determination (15 s), the result is expressed in mg/l.

The use of the photometer does not require any particular technical knowledge.

The first results are encouraging but call for additional experimentation by means of inter-
laboratory tests.

The advantage of the method in addition to measurement accuracy, is that it takes very little
account of the stable sulfates of cement that do not participate in the swelling reactions. From
this viewpoint, the reference methods penalize this type of material.
.

// The ehcvt'r test'

The determination of the acceptability thresholds for CaSO4, 2H20 plaster content (or sulfate
content) in aggregates coming from demolition products, corresponding to limits that
guarantee good structural durability, is based on the preparation, study and monitoring of
reference specimens or micro-specimens to obtain a quicker result.

The tests were validated by a comparison of results obtained using conventional methods and
those provided by micro-specimens.
On completion of the work, a table of the used of recycled aggregates according to their
gypsum content may be proposed.

Conclusion
All the tests mentioned above are or will form the subject of work within the framework of
European standardization. The European Technical Committee TC 154 which is responsible
for this work includes two subgroups in charge of:
- drafting standard specifications relative to the different uses of aggregates (mortars,
concrete, untreated granular materials, etc.),
- drafting test standards (sampling, geometry, mechanical properties, etc.).

These work groups have the job of choosing the important properties of materials to be set
forth in the specifications.
While some tests have already been covered by draft standards, work is advancing slower in
the field of utilization standards because the technical cultures of the various countries are
different.
On the other hand, as concerns the qualification of fines, the rejection and hence the non-use of
certain good materials makes little sense economically and the proposed tests seek to limit this.

Contacts at the Laboratoire Central des Ponts et Chaussdes:

- Main Maldonado: Sand production process

- Stphane Orsetti: Sulfate identification,
- Claude Tourenq : Methylene blue test.

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ALTER G.R. : <<The methylene blue test for bentonite liner quality controb> - 1983 - Geot.
Test. Journ. - Vol. 6 n 3 pp. 128-132.

- BENSTED J. : <<Application of the methylene blue test to cement raw materials>> - 1985 -
Journ. Techn. Biotechnol. 35A pp. 181-184.

- HIGGS N.B. <Preminiraly studies of methylene blue adsorption as a method of evaluating

degrable smectite bearing concrete aggregate sands>> - 1986 - Cement and Concrete Res. -
Vol. 16 pp. 525-534.

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 mechanical
strength
(concrete)

R-1

S 2 5 10 20
% clays or non-clayey fines

Figure 1 : Influence of percentage of fines on the tensile strength of a composite

.
flow of water +
flocculating agent

wate fines +
flocculating flocculate
clays
fines-fc

MMW hi
SE

fir sand h2

ck

I]
Figure 2 : Principle of the sand equivalent

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S Es

5 10 15 20
% clays ornon-clayey fines

. Figure 3: Influence of percentage of fines on the SE value

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blue value
g/1 kg sand
(spot)

401 2 4 6 8
% clays or non-clayey fines

Figure 4 : Amount of methylene blue needed to cover samples of different kinds