INTERNATIONAL ISO

STANDARD 5794-1
Second edition
1994-12-15

Rubber compounding ingredients - Silica,

precipitated, hydrated -
Part 1:
Non-rubber tests

Ingrkdien ts de mklange du caoutchouc - Silices hydratees

prkcipit6es -
Partie 1: Essais SW Ie produit brut
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Reference number
ISO 5794-13 994(E)

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 ISO 5794-1:1994( E)

Foreword
ISO (the International Organization for Standardization) is a worldwide
federation of national Standards bodies (ISO member bodies). The work
of preparing International Standards is normally carried out through ISO
technical committees. Esch member body interested in a subject for
which a technical committee has been established 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. ISO
collaborates closely with the International Electrotechnical Commission
(IEC) on all matters of electrotechnical standardization.

Draft International Standards adopted by the technical committees are

circulated to the member bodies for voting. Publication as an International
Standard requires approval by at least 75 % of the member bodies casting
a vote.

International Standard ISO 5794-1 was prepared by Technical Committee

lSO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw ma-
terials (including latex) for use in the rubber industry.

This second edition cancels and replaces the first edition (ISO
5794-1 :1984), which has been technically revised.

ISO 5794 consists of the following Parts, under the general title Rubber
compounding ingredien ts - Silica, precipitated, hydrated

- Part 7: Non-rubber tests

- Part 2: Test recipe and determination of physical properties in rubber

Annexes A, B, C and D form an integral part of this part of ISO 5794. An-
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nex E is for information only.

0 ISO 1994
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced
or utilized in any form or by any means, electronie or mechanical, including photocopyrng and
microfilm, without Permission in writing from the publisher.
arg
International anization for Standa rdization
Case Postale 56 l CH-121 1 Geneve 20 l Switzerland
Printed in Switzerland

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 INTERNATIONAL STANDARD 0 ISO ISO 5794=1:1994(E)

Rubber compounding ingredients - Silica,

precipitated, hydrated -

Part 1:
Non-rubber tests

WARNING - Persons using this part of ISO 5794 should be familiar with normal laboratory
practice. This part of ISO 5794 does not purport to address all of the safety Problems, if any,
associated with its use. lt is the responsibility of the User to establish appropriate safety and health
practices and ensure compliance with any national regulatory conditions.

1 Scope ISO 787-8:1979, General methods of test for pig-

ments and extenders - Part 8: Determination of
This part of ISO 5794 specifies methods of test for matter soluble in water - Cold extraction method.
characterizing precipitated hydrated silica for use as a
rubber compounding ingredient. A definition is given. ISO 787-9: 1981, General methods of test for pig-
ments and extenders - Part 9: Determination of pH
ISO 5794-2 specifies methods of test for precipitated value of an aqueous Suspension.
hydrated silica in compounded rubber.
ISO 787-10:1993, General methods of test for pig-
ments and extenders - Part IO: Determination of
density - Pyknometer method.

ISO 787-18:1983, General methods of test for pig-

2 Normative references ments and extenders - Part 18: Determination of
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residue on sieve - Mechanical flushing procedure.

The following Standards contain provisions which,
through reference in this text, constitute provisions ISO 842: -‘1, Raw materials for paints and varnishes
of this part of ISO 5794. At the time of publication, the - Sampling.
editions indicated were valid. All Standards are subject
to revision, and Parties to agreements based on this ISO 3262: 1975, Extenders for paints.
part of ISO 5794 are encouraged to investigate the
possibility of applying the most recent editions of the ISO 4652-1: 1994, Rubber compounding ingredients
Standards indicated below. Members of IEC and ISO - Carbon black - Determination of specific surface
maintain registers of currently valid International area by nitrogen adsorption methods - Part 1:
Standards. Single-poin t procedures.

ISO 787-2:1981 I General methods of test for pig-

ments and extenders - Part 2: Determination of
matter volatile at 105 “C.

1) To be wblished. (Revision of ISO 842:1984)

1
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 ISO 5794-1: 1994(E) 0 ISO

3 Definition 4 Sampling

Sampling shall be carried out in accordance with

For the purposes of ISO 5794, the following definition ISO 842.
applies.
5 Methods of test

3.1 precipitated hydrated silica: Material com- The properties of precipitated hydrated silica shall be
posed of amorphous particles obtained from soluble determined by the methods of test referred to in
silicates by precipitation from aqueous Solution. table 1.

Table 1 - Methods of test

Property Method of test

Silica content of dried Sample, % (m/m) ISO 32621975, clause 17, except that in the expression of
results the denominator shall be mg, where q-, is the mass,
in grams, of the test Portion taken in subclause 11.2 of
ISO 3262:1975, not the mass of ignited residue obtained in
11.2

Colour ISO 3262:1975, clause 7

Residue on sieve (nominal aperture size 45 Pm):

- for silica in powder form ISO 3262:1975, clause 8
- for silica in other forms ISO 787-18

Matter volatile at 105 “C (loss on heating) ISO 787-2

(Use a test Portion of 2 g weighed to the nearest 0,l mg)

Loss on ignition at 1 000 “C of dried Sample ISO 3262:1975, clause 11

pl-l of slurry ISO 787-9

Water-soluble matter ISO 787-8

Total topper content, mg/kg See annex A

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Total manganese content, mg/kg See annex B

Total iron content, mg/kg See annex C

Specific surface area, m2/g See annex D

Density, Mg/m3 ISO 787-10

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 ISO 5794-1: 1994(E)

Annex A
(normative)

Determination of total topper content

A.l Principle turnings in a mixture of 10 cm3 of water and 5 cm3

of nitric acid (A.2.6) in a 100 cm3 beaker. Boil under
A test portion is digested with hydrofluoric acid and a fume hood to expel oxides of nitrogen. Cool, trans-
sulfuric acid and the Silicon is volatilized as Silicon fer to a 1 dm3 volumetric flask, make up to the mark
tetrafluoride. with water and mix.

Any metals in the digested test Portion are dissolved 1 cm3 of this Standard Solution contains 1 000 pg of
in hydrochloric acid, then the Solution is diluted and topper.
aspirated into the flame of an atomic absorption
spectrometer set at a wavelength of 324,7 nm. A.2.8 Copper, Standard Solution corresponding to
50 mg of Cu per cubic decimetre.
The method is applicable to the determination of
topper contents up to 125 mg/kg, and there is pro- Pipette 50,O cm3 of the 1 g/dm3 Standard topper sol-
Vision for extending the range to 1 250 mg/kg. ution (A.2.7) into a 1 dm3 volumetric flask, add 5 cm3
of nitric acid (A.2.6), make up to the mark with water
WARNING - All recognized health and safety and mix.
precautions shall be taken when performing this
method of analysis. 1 cm’ of this Standard Solution contains 50 pg of
topper.
A.2 Reagents and materials
A.2.9 Copper, Standard Solution corresponding to
All reagents shall be of recognized analytical grade. 10 mg of Cu per cubic decimetre.
The water used shall be distilled water or water of Pipette 50,O cm3 of the 50 mg/dm3 Standard topper
equivalent purity. Solution (A.2.8) into a 250 cm3 volumetric flask, add
1 cm3 of nitric acid (A.2.6), make up to the mark with
A.2.1 Acetylene, compressed-gas supply. water and mix.

A.2.2 Air, compressed-gas supply. 1 cm3 of this Standard Solution contains 10 pg of

topper.
A.2.3 Hydrochlorit acid, 10 % (m/m) Solution.
NOTE 1 Commercially available Standard topper sol-
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Dilute 20 cm3 of 35 % (4.) hydrochloric acid Solution utions may be used, if preferred, instead of A.2.7, A.2.8 and
= 1,18 Mg/m3) with 50 cm3 of water. A.2.9.
( e20

A.2.4 Hvdrofluoric acid, 40 % (rrtJm) Solution A.3 Apparatus

(e20 = 1.1’3 Mg/m3).
Usual laboratory equipment, plus the following:
A.2.5 Sulfuric acid, 98 % (dm) Solution
= 1,84 Mg/m3). A.3.1 Platinum dish, of capacity approximately
( Q20
35 cm3.
A.2.6 Nitrit acid, 68 % dm) Solution
= 1,42 Mg/m3). A.3.2 Atomic absorption spectrometer, fitted with
( e20
an airlacetylene burner.
A.2.7 Copper, Standard Solution corresponding to
1 g of Cu per cubic decimetre. A.3.3 Analytical balance, capable of weighing to
0,l mg.
Dissolve 1,000 g + 0,001 g of high-purity topper

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 ISO 5794-1:1994 Rubber compounding ingredients - Silica,
precipitated, hydrated - Part 1: Non-rubber tests
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