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Sodium and potas s ium s ilicates for indus trial use -

Determination of s ilica content - Titrimetric method

F irst edition - 1972-06-15

iTeh STANDARD PREVIEW
(standards.iteh.ai)
ISO 2124:1972
https://standards.iteh.ai/catalog/standards/sist/0077116a-814d-49f4-bf93-
9ff6e3925a54/iso-2124-1972

-LLI UDC 661.31/.32 : 546.284-31 Ref. No. IS0 2124-1972 (E)

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Descriptors : chemical analysis, determination of content, potassium silicates, silicon dioxide, sodium silicates, volumetric analysis.
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Price based on 2 pages
IS0 (the International Organization for Standardization) is a worldwide federation
of national standards institutes (IS0 Member Bodies). The work of developing
International Standards is carried out through IS0 Technical Committees. Every
Member Body interested in a subject for which a Technical Committee has been set
up has the right to be represented on that Committee. International organizations,
governmental and non-governmental, in liaison with ISO, also take part in the work.

Draft International Standards adopted by the Technical Committees are circulated

to the Member Bodies for approval before their acceptance as International
Standards by the IS0 Council.

International Standard
ISO/TC 47, Chemistry.
iTeh
IS0 2124 STANDARD
was drawn up by Technical PREVIEW
Committee

It was approved in March

(standards.iteh.ai)
1971 by the Member Bodies of the following countries:
ISO 2124:1972
Austria India South Africa, Rep. of
https://standards.iteh.ai/catalog/standards/sist/0077116a-814d-49f4-bf93-
Ireland Spain
Belgium
Chile Israel
9ff6e3925a54/iso-2124-1972
Switzerland *
Czechoslovakia Italy Thailand
Egypt, Arab Rep. of Netherlands Turkey
France New Zealand United Kingdom
Germany Poland U.S.A.
Hungary Portugal U.S.S.R.

No Member Body expressed disapproval of the document.

0 International Organization for Standardization, 1972 l

Printed in Switzerland
INTERNATIONAL STANDARD ’ IS0 2124-1972 (E)

Sodium and potassium silicates for industrial use -

Determination of silica content - Titrimetric method

1 SCOPE AND FIELD OF APPLICATION 5.2 Ethanol, approximately 95 % ) which may be

denatured with ether.
This International Standard specifies a simple and rapid
titrimetric method for the determination of the silica content
5.3 Ethanol, approximately 50 % ) which may be
of sodium and potassium silicates for industrial use.
denatured with ether.

2 REFERENCES 5.4 Hydrochloric acid, N standard volumetric solution.

lSO/R 645, Statistical vocabulary and symbols - First approximately 0.1 N solution.
5.5 Hydrochloric acid,
series of terms and symbols - Part 1 : Statistical vocab-
ulary.
5.6 Sodium hydroxide, N standard volumetric solution.
IS0 2122, Sodium and potassium silicates for industrial
use - Preparation of solution of products not easily
iTeh STANDARD5.7PREVIEW
Methyl red, 1 g/l solution
soluble in boiling water and determination of matter insol-
in 95 % (V/V) ethanol.

uble in water. (At present at the stage of Draft).

(standards.iteh.ai)
6 APPARATUS
3 PRINCIPLE ISO 2124:1972 Ordinary laboratory apparatus and
Neutralization https://standards.iteh.ai/catalog/standards/sist/0077116a-814d-49f4-bf93-
of the alkalinity of a test portion, pre-
viously dissolved, with methyl red as indicator. 9ff6e3925a54/iso-2124-1972
6.1 Burette, 25 ml, graduated in 0.05 ml.

Addition of sodium fluoride, which reacts with the silicic

acid, forming an equivalent quantity of sodium hydroxide. 7 PROCEDURE
Addition of a measured volume of standard volumetric
hydrochloric acid solution in excess, followed by ethanoi. 7.1 Test portion
Filtration of the silicic compound thus obtained, which is Weigh, to the nearest 0.1 mg, a quantity of laboratory
insoluble under these conditions. sample corresponding to 2.0 + 0.3 g of Si02. I

Titration of the excess of acid in the filtrate with standard

NOTE - In the case of products not easily soluble, use an
volumetric sodium hydroxide solution with methyl red as equivalent quantity of the solution prepared according to the
indicator. method described in IS0 2122.

4 REACTIONS 7.2 Blank test

HzSi03 + 6 NaF + Hz0 - NaaSiF6 -t 4 NaOH Place in a 250 ml conical flask, 70 ml of water, 5.00 ml of
the sodium hydroxide solution (5.6) and 0.30 ml of the
NaOH -I- HCI -NaCl -l- HZO. methyl red solution (5.7). Add, by means of a graduated
pipette, approximately 4.5 ml of the hydrochloric acid
solution (5.4) and neutralize with the hydrochloric acid
5 REAGENTS solution (5.5) until the colour of the indicator turns from
yellow to red. Then add 5 f 0.1 g of the sodium fluoride
Distilled water or water of equivalent purity shall be used (5.1) to the solution thus neutralized. Stir to aid dissolution
sh the test. of this product, then add a precisely measured volume ( V3)
of the hydrochloric acid solution (5.4) corresponding to an
5.1 Sodium fluoride, anhydrous, heated at 600 “C and excess of about 5 ml after the colour change to red.
cooled in a desiccator.

1
602124-1972(E)

Then add 50 ml of the ethanol (5.2), stir for about 1 min, w 1 - 2 V2) - w, - 2 Vg)] x 0.015 02 x 2gx ‘g
transfer quantitatively to a 200 ml one-mark volumetric
flask, dilute to the mark with ethanol (5.3) and mix. Filter
a little more than 100 ml on a folded, dry, close grained =[(V1 -2 Vz)-(V3 -2 V,)]X y
filter, discarding the first few millilitres. Take 100.0 ml of
the filtrate and place in a 250 ml conical flask; add 0.30 ml where
of the methyl red solution (5.7) andtitrate the excess of
acid with the sodium hydroxide solution (5.6), contained VI is the volume, in millilitres, of the hydrochloric acid
in the burette (6.1), until the colour changes from red to solution (5.4) added for the determination (7.3);
yellow.
v2 is the volume, in millilitres, of the sodium hydroxide
7.3 Determination solution (5.6) used for the back titration in the determi-
nation;
Place the test portion (7.1) in a 250 ml one-mark volu-
metric flask, if necessary dissolving it in water, dilute to the V3 is the volume, in millilitres, of the hydrochloric acid
mark and mix. solution (5.4) added for the blank test (7.2);
Take 50.0 ml of this dilute solution immediately and place
in a 250 ml conical flask. Add 0.30 ml of the methyl red V4 is the volume, in m illilitres, of th e sodi urn hydrox ide
solution (5.7). Neutralize with the hydrochloric acid solution solution (5. 6) used for the back titration in the blank test;
(5.4) the total alkalinity less about 1 mg equivalent (if
necessary, carry out a preliminary titration of this alkalinity
on another 50 ml sample) and neutralize with hydrochloric 0.015 02 is the mass, in grams, of Si02 correspond-
acid solution (5.5) until the colour of the indicator changes ing to 1 ml of the hydrochloric acid solution (5.4);
from yellow to red. Then add to the neutralized product
iTeh STANDARD PREVIEW
5 -+ 0 . 1 g of thesodium fluoride (5.1). Stir to aid dissolution
of this product and then add a precisely measured volume
173 is the mass, in grams, of the test portion.

(VI ) of the hydrochloric

(standards.iteh.ai)
acid solution (5.4) corresponding
to an excess of about 5 ml after the colour changes to
8.2 Repeatability1 )
red. Add 50 ml of the ethanol (5.2), stir for about 1 min, The results obtained by this method are exact to Ifr 0.3 % in
transfer to a 200 ml one-mark volumetric flask, dilute ISO to 2124:1972
absolute value.
the mark with the ethanol (5.3)https://standards.iteh.ai/catalog/standards/sist/0077116a-814d-49f4-bf93-
and mix.
9ff6e3925a54/iso-2124-1972
9 TEST REPORT
Filter a little more than 100 ml on a folded, dry, close
grained filter, discarding the first few millilitres. Take The test report shall include the following particulars :
1’00.0 ml of the filtrate and place in a 250 ml conical
flask; add 0.30 ml of the methyl red solution (5.7) and
a) the reference of the method used;
titrate the excess of acid with the sodium hydroxide W the results and the method of expression used;
solution (5.6) contained in the burette (6.1) until the colour
changes from red to yellow. c) any unusual features noted during the determina-
tion;

8 EXPRESSION OF RESULTS
d any operation not included in this International
Standard 8 or regarded as optional.

8.1 Formula for calculation 1) repeatability : Closeness of agreement between successive re-
sults obtained with the same method on identical test material and
Silica content is given, as a percentage by mass, by the under the same conditions (same operator, same apparatus, same
formula : laboratory and same time). (Definition taken from ISO/R 645.)