CONCRETE, HARDENED AND MORTAR:

CALCIUM OXIDE AND SOLUBLE SILICA CONTENTS

Key words: Concrete, hardened
calcium oxide, soluble silica

concrete,

UDC 691.32
691.53
541.6

mortar,

SCOPE AND FIELD OF APPLICATION

This is a method for determining calcium oxide content and

soluble silica content of concrete. The results can be used to
estimate the cement content of concrete and sometimes the
type of cement. However, this estimation is outside the scope
of this method.
The described methods can also be used to determine the
calcium oxide content and soluble silica content of cement,
aggregate and supplement material.

Reagents
Ethanol, 99.5 %
Perchloric acid, HCIO4
Perchloric acid, HCIO 4 1+9
Dilute 100 ml conc. HCIO4 to 1000 ml
Triethanolamin. TEA, 10 %
Dilute 100 g TEA to 1000 ml
Potassium hydroxide, KOH (4 M)
Dissolve by stirring vigorously 255.3 g. KOH pellets in 700 ml
H2O

Note! Heat is released and there is a risk of splashes from the solution.
Use safety goggles. After cooling, dilute to 1000 ml and store
in a sealed plastic bottle.

EQUIPMENT

Sample preparation equipment:

Laboratory crusher
Laboratory mill/grinder
Ventilated oven, 105 5C
Balance, sensitivity 0,1 g
Sample divider
pH-meter

EDTA, 1.0 M, to be prepared from ampoule

EDTA-solution 0.025 M
Dilute 250 ml 0.1 M EDTA to 1000 ml. This solution should be
standardised against standard calcium solution at regular intervals.
Calcein indicator
Mix well 250 mg Calcein, 125 mg thymolphthalein and 25 g
NaCI.
Acetone

Chemical analysis
Balance, sensitivity 0,1 mg
De-ionised water 1)
Magnetic stirrer
Beakers, glass with spout, 150 ml, 250 ml
Volumetric flasks, 50 ml, 100 ml, 250 ml, 1000 ml
Pipettes class A
Filtration equipment
Filter paper, OOR
Burette
Photometer, 10 mm cuvette

1) Deionised water shall be used throughout the analysis.

Ammonium molybdate, 5 %
Dissolve 50 g Ammonium molybdate (NH 4) 6Mo 7O 2 x 4H 2O) in
H 2O and dilute to 1000 ml. Store the solution in a plastic bottle.
Standard silicon solution. Prepare 1000 ppm from a standard
ampoule and store in a plastic bottle.

PREPARATION OF SAMPLE

Crush a sample of at least 2 kg coarsely to a minimum grain

size of approximately 6 mm. Divide with a sample divider or by
equivalent means to about 100 g. Dry the sample obtained in
a drying cabinet (+105 5C)
C) until the weight loss during 24
h decreases to 0.1 % by weight. Grind the sample until at least
90 % of the sample passes a sieve of 1.125 mm. (K90 < 0.125).

Published by NORDTEST

Tekniikantie 12, FIN-02150 ESPOO FINLAND

ISSN 0283-7153

Proj. 983-91

Phone+35894554600

Fax+35894554272

www.nordtest.org

NORDTEST

METHOD

NT BUILD 437 2

Prepare a test solution as follows.

5.3

Preparation of test solution

1. Weigh about 1 gramme of the dried and powdered sample

to an accuracy of three decimal places (m) in a 250 ml
beaker.

Pipette an exact amount (V2) 5-20 ml test solution into a 100

ml volumetric flask. Add reagents (5.1). Dilute to the mark with
water and shake.

2. Moisten the sample with about 2 ml absolute ethanol.

3. Add 150 ml water and stir vigorously with a magnetic stirrer.

5.4

Determination

5. Allow the solution to settle.

Read the absorbance of the calibration solutions and the test

solution with the photometer after at least 5 minutes but within
60 minutes after preparation. Use a wave length of 412.5 nm.
The instrument is zeroed with the reagent blank.

6. Filter the solution through OR-filter in a 250 ml measuring

cylinder. Wash the filter carefully with water and dilute to
the mark with water.

Draw a calibration curve with the result of the three calibration

solutions and then determine the concentration of the test
solution with the help of the curve.

4. Slowly add about 5 ml concentrated HClO 4 directly into the

stirring centre and continue stirring for about 10 minutes.

Calculate the soluble silica content (SiO 2) from the expression:

DETERMINATION OF MASS OF SOLUBLE

CALCIUM

Pour 40-50 ml water into a 150 ml beaker. Pipette 10-25 ml

(V1) of the sample solution into the beaker. Add 10 ml TEAsolution (10 %), standardise pH to 12.5 with 5-10 ml KOH (4M)
and a pinch of calcein indicator. Titrate the solution with
EDTA-solution (0.025 m) whilst stirring with a magnetic stirrer
until the colour of the liquid changes to violet-green.
Calculate the calcium oxide content (CaO) from the expression:
CaO = 5.6079 a f M/m (% by weight)
where
a = volume of EDTA-solution used (ml)
v1 = volume of test solution
f = dilution factor, 250/V1
M = the concentration of the EDTA-solution (mol/1)
m = the mass of the analytical sample (g)
If 10 ml test solution is pipetted into the solution, the CaO
content can be calculated as:
CaO = 140.2.a.M/m

SiO 2 =

c x 10 -6 x f x 60.084 x 250 x 100

280.086 x m

0.05348 x c x f
m
(% by weight)

where
28.086 = molecular mass of Si
60.084 = molecular mass of SiO 2
V2
= volume of test solution (ml)
c
= the concentration of the test solution (ppm)
f
= dilution factor 100/V2
m
= the mass of the analytical sample (g)
If 10 ml test solution is pipetted the following equation is
obtained:
SiO 2 = 0.05348 c/m (% by weight)

EXPRESSION OF THE RESULTS

The calcium oxide content and the soluble silica content shall
be given in % by weight to the nearest 0.1 %.

REPORT

The final rest report shall include at least the following information.

DETERMINATION OF SOLUBLE SILICA

a) Name and address of the test laboratory

5.1

Reagents:

b) Date and identification of the report

10 ml HClO 4 1+9
10 ml acetone
15 ml ammonium molybdate, 5 %

c) Test method (number and title)

d) Any deviation from the method
e) Name and address of the customer
f)

5.2

Preparation of calibration

Prepare a standard silicon solution of 100 ppm by diluting a

standard silicon solution of 1000 ppm ten times with water.
Pipette 5, 10 and 20 ml standard silicon solution (100 ppm)
into each of the three 100 ml volumetric flasks. Furthermore,
prepare a reagent blank with only the above in a 100 ml
measuring flask. Add water into the volumetric flasks to the
mark and shake.

Name of the sample and method of sampling

g) Name of the producer if possible

h) Cement composition and age, if possible
i)

Shape, size and identification of the samples

j)

Test

results

k) Supplementary information of any significance for the

evaluation of the result
l)

Date of receipt and date of testing