INTERNATIONAL ISO

STANDARD 1408
Third edition
1995-10-01

Rubber - Determination of carbon black

content - Pyrolytic and Chemical
degradation methods
iTeh STANDARD PREVIEW
(standards.iteh.ai)
Caoutchouc - Dosage du noir de carbone
mk thodes par ddgrada tion chimique
- Methode pyrolytique et

ISO 1408:1995
https://standards.iteh.ai/catalog/standards/sist/a7b0b4de-bc63-44f5-b9be-
67c26fa3ec00/iso-1408-1995

Reference number
ISO 1408: 1995(E)
ISO 1408:1995(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
(1EC) 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. iTeh STANDARD PREVIEW
International Standard ISO (standards.iteh.ai)
1408 was prepared by Technical Committee
ISO/TC 45, Rubber and rubber products.
ISO 1408:1995
This third edition cancelshttps://standards.iteh.ai/catalog/standards/sist/a7b0b4de-bc63-44f5-b9be-
and replaces the second edition
(ISO 1408:1987), of which it constitutes a minor revision.
67c26fa3ec00/iso-1408-1995

0 ISO 1995
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 photocopying and
microfilm, without Permission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-121 1 Geneve 20 l Switzerland
Printed in Switzerland
INTERNATIONAL STANDARD 0 ISO ISO 1408:1995(E)

Rubber - Determination of carbon black content -

Pyrolytic and Chemical degradation methods

WARNING - Persons using this international Standard should be familiar with normal laboratory
practice. This Standard 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 to ensure compliance with any national regulatory conditions.

1 Scope - fluorosilicone rubbers;

- chlorosulfonated polyethylenes containing less

iTeh STANDARD PREVIEW
1.1 This International Standard specifies a pyrolytic than 30 % (m/m) of chlorine.

and C) for the determination

(standards.iteh.ai)
method (A) and two Chemical degradation methods (B
of the carbon black con-
The precision of this method may be affected if min-
eral fillers, e.g. alumina or Calcium carbonate, are
tent of rubber.
ISO 1408:1995present which decompose or dehydrate, or form vol-
atile halides in the case of halogenated polymers, at
https://standards.iteh.ai/catalog/standards/sist/a7b0b4de-bc63-44f5-b9be-
the pyrolysis temperature.
67c26fa3ec00/iso-1408-1995
1.2 Method A is preferred and should be used for
the following polymers, except when certain com- The method cannot be used for either chloroprene
pounding materials such as lead and Cobalt salts, rubbers or butadiene-nitrile rubbers having an acrylic
graphitic carbon blacks, phenolic and other resins, acid nitrile content greater than 30 % (m/m).
bitumen, or cellulose, etc., which Cause the formation
of a carbonaceous residue during pyrolysis, are pre- 1.3 Method B is chiefly intended to be used with
sent: samples not amenable to the pyrolytic method A, al-
though it tan be used for all samples based on un-
- polyisoprene, natura1 or synthetic;
saturated rubbers except for isobutylene-isoprene
copolymers.
- polybutadiene;

- styrene-butadiene copolymers; 1.4 Method C is relatively hazardous and should be

used only for the analysis of samples based on
- butyl rubber; isobutylene-isoprene copolymers and ethylene-
propylene copolymers and related terpolymers when
- acrylate rubber; methods A and B fail.

- ethylene-propylene copolymer;
2 Normative references
- ethylene-propylene terpolymer;
The following Standards contain provisions which,
- polyethers; through reference in this text, constitute provisions
of this International Standard. At the time of publi-
- polyethylene-derived polymers; cation, the editions indicated were valid. All Standards
are subject to revision, and Parties to agreements
- Silicone rubbers; based on this International Standard are encouraged

1
ISO 1408:1995(E) 0 ISO

to investigate the possibility of applying the most re- Oxidation of the carbon black to carbon dioxide. The
cent editions of the Standards indicated below. residue is cooled and reweighed. The loss in mass
Members of IEC and ISO maintain registers of cur- represents the carbon black.
rently valid International Standards.
4 Method A
ISO 383: 1976, Laboratory glassware - Interchange-
able conical ground joints. WARNING - All recognized health and safety
precautions shall be in effect when carrying out
ISO 1407:1992, Rubber - Determination of solvent
this method. All evaporations shall be carried out
extrac t. in a fume cupboard (hood).

3 Principle 4.1 Reagents

3.1 Method A During the analysis, unless otherwise stated, use only
reagents of analytical reagent grade (or equivalent)
A weighed test piece of the rubber is extracted with and only distilled water or water of equivalent purity.
acetone and, if bitumen is present, with dichloro-
methane. The extracted rubber is pyrolized in a com- 4.1.1 Nitrogen, dry and free from Oxygen.
bustion boat at 850 “C in a stream of nitrogen. The
boat containing the non-volatile residue is cooled and NOTE 1 Commercial “Oxygen-free” nitrogen may require
further purification.
weighed.

The carbon black is then burnt off in air or Oxygen in 4.1.2 Oxygen or air, gaseous, dry.
a furnace at the same temperature. The boat and its
iTeh STANDARD
contents are cooled and reweighed. The loss in mass
represents the carbon black.
PREVIEW
4.1.3 Xylene, general laboratory grade.

(standards.iteh.ai)
4.1.4 Acetone.
3.2 Method B
4.1.5 Dichloromethane.
ISO 1408:1995
A weighed test piece of the rubber is extracted with
https://standards.iteh.ai/catalog/standards/sist/a7b0b4de-bc63-44f5-b9be-
4.1.6 Ethanol-toluene
acetone. The organic components are destroyed67c26fa3ec00/iso-1408-1995
by azeotrope (ETA).
Oxidation with nitric acid, the acid-soluble inorganic
Mix 7 volumes of absolute ethanol with 3 volumes of
components dissolving simultaneously in the nitric
toluene. Alternatively, mix 7 volumes of commercial-
acid. The residue, which consists of carbon black and
grade ethanol with 3 volumes of toluene and boil the
acid-insoluble mineral fillers is filtered, washed and
mixture with anhydrous Calcium Oxide (quicklime) un-
then dried to constant mass at 850 “C in a nitrogen
der reflux for 4 h. Then distil the azeotrope and collect
atmosphere to avoid Oxidation of the carbon black.
the fraction with a boiling range not exceeding 1 “C,
The weighed residue is reheated at the same tem- for use in the test.
perature (850 “C) (to avoid further Change in mass of
the inorganic matter) but this time in air so as to Cause 4.2 Apparatus
Oxidation of the carbon black to carbon dioxide. The
residue is cooled and reweighed. The loss in mass Ordinary laboratory apparatus, plus the following:
represents the carbon black.
4.2.1 Combustion boat, made of silica, of length
50 mm to 60 mm, with handle.
3.3 Method C

After swelling of a test piece by hot 4.2.2 Tube furnace assembly see figure 1, com-
p-dichlorobenzene, the organic matter is oxidized by prised of the following component Parts:
tert-butyl hydroperoxide. The undissolved carbon
black and mineral fillers are filtered, washed and then 4.2.2.1 Combustion tube, made of quartz or of
dried to constant mass at 850 “C in a nitrogen at- impervious aluminous porcelain, and fitted with
mosphere to avoid Oxidation of the carbon black. means for advancing and withdrawing the combustion
boat (4.2.1). The inside diameter shall be sufficient to
The weighed residue is reheated at the same tem- allow the combustion boat to enter the tube and
perature (850 “C) (to avoid further Change in mass of move easily through it. The tube shall be 30 cm longer
the inorganic matter) but this time in air so as to Cause than the tube furnace (4.2.2.2). One end of the tube

2
0 ISO ISO 1408:1995(E]

shall be provided with a gas-inlet System for nitrogen, 4.4.2 Weigh the test piece to the nearest 0,l mg
the opposite end with a suitable outlet System for the (mass m& Record this mass. Wrap the test piece in
vapours produced during the pyrolysis. filter Paper and extract with acetone (4.1.4) for 4 h or
until the solvent in contact with the test piece is
4.2.2.2 Horizontal-tube furnace, having an inside colourless. If bitumen is present in the compound,
diameter sufficiently large to allow the combustion extract with dichloromethane (4.1.5) for 4 h or until
tube (Lc.2.2.1) to enter the heated section of the fur- the solvent in contact with the test piece appears
nace. The furnace shall be electrically heated, colourless.
thermostatically maintained at 850 “C -+-25 “C and
fitted with a temperature-indicating device. Wncured coumpounds cannot be extracted with
dichloromethane. ETA (4.1.6) may be used instead of
acetone or dichloromethane.
4.2.2.3 Silica glass rod with hook, of length suf-
ficient to resch through the combustion tube NOTE 2 Extraction with dichloromethane is only necess-
(4.2.2.1) and inlet tube (4.2.2.4), and of diameter suf- at-y if materials not completely soluble in acetone, such as
ficient to make tight contact with the rubber tube in bitumen, are present.
the inlet tube.
Extraction tan be facilitated by comminuting the test
4.2.2.4 Inlet tube, with side tube for nitrogen supply piece before weighing. To do this, pass it through a
and with a short length of rubber tubing in which the mill with minimum clearance between the rolls.
silica glass rod (4.2.2.3) is held by an airtight joint but
tan slide in and out of the combustion tube (4.2.2.1). 4.4.3 Remove the extracted test piece from the filter
The tubing used for the gas-inlet System shall be Paper and dry in an oven maintained at
made of plasticized PVC or other material having a low 100 “C + 3 “C until the solvent is completely re-
permeability to Oxygen and water vapour. moved.
iTeh STANDARD PREVIEW
4.2.2.5 Vapour absorption equipment, consisting
for the connection of(standards.iteh.ai)
4.4.4 Quantitatively transfer the dried test piece to
of rubber tubing the outlet sys- the combustion boat (4.2.1) and place the boat in the
tem of the combustion tube (4.2.2.1) with a trap for combustion tube (4.2.2.1) near the nitrogen inlet sys-
readily condensable vapours, two gas-washing bottles ISO 1408:1995tem.
containing xylene (4.1.3),https://standards.iteh.ai/catalog/standards/sist/a7b0b4de-bc63-44f5-b9be-
and flowmeters and flow-
67c26fa3ec00/iso-1408-1995
controllers for nitrogen or Oxygen or air supplies. 4.4.5 Close the tube with the entry fitting and con-
nett to the nitrogen supply (4.1 .l). Introduce the
4.2.3 Suitable extraction apparatus, as specified combustion tube into the furnace (4.2.2.2) heated to
in ISO 1407. 850 “C + 25 “C but keep the boat in the cool part of
the combustion tube. Connect the opposite end of the
4.2.4 Desiccator. tube to the vapour absorption equipment (4.2.2.5).

4.2.5 Muffle furnace, electrically heated, thermo- 4.4.6 Pass nitrogen through the tube at about
statically controllable at 850 “C +- 25 “C. 200 cm3/min for 5 min or more to eliminate the air
contained in the combustion tube.
4.3 Sampling
4.4.7 Reduce the rate of nitrogen flow to about
Cut a test Sample of at least 1,5 g from the laboratory 100 cm3/min and move the boat slowly into the
Sample, preferably from more than one place, so that heated zone of the combustion tube over a period of
proper representation of the whole Sample is about 5 min.
achieved.
4.4.8 Leave the boat in the hot zone for a further
4.4 Procedure 5 min in Order to complete the pyrolysis.

4.4.1 Prepare the test Sample by passing the rubber 4.4.9 Withdraw the boat to the cold part of the tube
six times between the rolls of a laboratory mill set to and allow to cool for 10 min, while still maintaining
a nip not exceeding 0,5 mm. Cut from the sheet a the flow of nitrogen.
test piece having a mass of approximately Q,l g to
0,5 g. If it is not possible to pass the Sample through 4.4.10 Transfer the boat to the desiccator (4.2.4),
the mill, the Sample may be tut into pieces less than complete the cooling and weigh to the nearest
1 mm per side. 0,l mg (mass m,). Record this mass.

3
ISO 1408:1995(E) 0 ISO

4.4.11 Place the boat in the combustion tube again served with the use of acids and solvents. All
and close the tube; connect the inlet System of the operations shall be carried out in a properly ven-
tube to the Oxygen or air supply (4.1.2) and pass the tilated fume hood, and safety glasses shall be
gas through the tube at about 100 cm3/min. Move the worn during digestions, extractions and
boat to the heated zone and keep it there until all washings.
traces of carbon black have been removed.
5.1 Reagents
4.4.12 As an alternative to 4.4.11, heat the boat in
the muffle furnace (4.2.5) at 850 “C -+ 25 “C until all Reagents specified in 4.1, plus the following:
traces of carbon black have been removed.
5.1.1 Nitrit acid (p = 1,42 Mg/m3).
4.4.13 Transfer the boat to the desiccator and allow
to cool to room temperature. 5.1.2 Hydrochlorit acid solution.

Add 2 Parts by volume of concentrated hydrochloric

4.4.14 Weigh the boat to the nearest 0,l mg (mass
acid (p = 1 ,18 Mg/m3) to 98 Parts by volume of water.
9). Record this mass.

5.1.3 Chloroform.
4.4.15 Carry out the determination in duplicate.
5.1.4 Acetone-chloroform mixture, 1 + 1 (V/V).
4.5 Expression of results
5.1.5 Sodium hydroxide Solution, 250 g/dm3.
Calculate the carbon black content, as a percentage
by mass, from the formula 5.1.6 Sodium hydroxide Solution, 150 g/dm3.

m1-m2 XI00 iTeh STANDARD PREVIEW

mo 5.2 Apparatus
(standards.iteh.ai)
Apparatus specified in 4.2, plus the following:
ISO 1408:1995
mo is the mass, in grams, of the test piece
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5.2.1 Gooch crucible with a filtering layer of suit-
(see 4.4.2); 67c26fa3ec00/iso-1408-1995
able inert, thermally stable filter material in the bot-
is the mass, in grams, of the combustion tom, prepared as follows.
ml
boat and its contents after heating in ni-
Make a dispersion of the filter material in water, pour
trogen (see 4.4. IO);
some of the dispersion into the Gooch crucible, and
is the mass, in grams, of the combustion apply a moderate vacuum. When a thick layer covers
9
boat and its contents after combustion of the bottom of the crucible, press a ceramic disc hav-
the carbon black in Oxygen or air (see ing small holes on to the fibrous layer. Pour more
4.4.14). dispersion into the crucible until the disc is covered
with a homogeneous layer of fibres, and apply a
NOTES moderate vacuum. Before use, treat the crucible in
accordance with the procedures described in 5.3.5 to
3 The test piece may be taken from previously extracted 5.3.16 and then heat at 850 “C -+ 25 “C for 2 h.
material. In this case, a correction for solvent extract level
would normally be made to obtain Q. The tube furnace and ass ociated Systems (4.2.2) have
to be capable of acceptin g the Gooch cru cible.
4 Any matter volatile at 850 “C in the carbon black (as
purchased) will be lost during the pyrolysis in nitrogen. The
final result for the mass percentage of carbon black will 5.3 Procedure
therefore be low by this amount. In cases where the carbon
black type and origin are known, a suitable correction tan 5.3.1 Weigh a test piece of about 0,3 g to 0,5 g of
be made. thinly sheeted Sample to the nearest 0,l mg (mass
q). Record this mass. Extract and dry the test piece
5 Method B in accordance with 4.4.2 and 4.4.3.

WARNING - Because of possible health and 5.3.2 Quantitatively transfer the dried test piece to
safety hazards inherent in this method, recog- a 100 cm3 beaker containing about 10 cm3 of nitric
nized health and safety precautions shall be ob- acid (5.1 .l); cover with a watch-glass.
0 ISO ISO 1408:1995(E)

5.3.3 The Oxidation reaction usually Starts after a 5.3.10 Wash the insoluble matter in the beaker with
few minutes at room temperature. If it does not, three portions of 10 cm’ of chloroform (5.1.3), filtering
warm the beaker gently on a boiling water bath until the washings through the Gooch crucible and main-
the reaction Starts. Complete the first step of the re- taining the greater part of the insoluble matter in the
action at room temperature with occasional heating bea ker.
on the boiling water bath, if necessary.
WARNING - Under basic conditions, mixtures of
5.3.4 Make up to 50 cm3 by washing the Walls of chloroform and acetone may explode. Thoroughly
the beaker with nitric acid (5.1 .l) and complete the wash out the filter flask with acetone and then
oxidative reaction by heating the beaker on the boiling water before proceeding to 5.3.11.
water bath for 2 h with occasional stirring. The
Oxidation is complete when no bubbling or foam is 5.3.11 Add to the beaker 25 cm3 of 250 g/dm3
observed on the surface of the liquid. sodium hydroxide solution (5.1.5) and heat on a boiling
water bath for 30 min with occasional stirring.
NOTE 5 Heating times and conditions mentioned in 5.3.3
and 5.3.4 must be adhered to strictly. Insufficient Oxidation
will Cause the carbon black to be overestimated, owing to 5.3.12 Dilute with 35 cm’ of warm water and filter
the presence of unoxidized polymer. Prolonged heating, on the mixture through the Gooch crucible, quantitatively
the other hand, will Cause loss of carbon black by Oxidation transferring the insoluble matter into the crucible.
to carbon dioxide, as in the determination of styrene content
by nitration (ISO 5478:1990, Rubber - Determination of
styrene content - Nitration method), where more vigorous 5.3.13 Wash the beaker and the Gooch crucible with
heating conditions are used to partially or completely re- three portions of 10 cm3 of 150 g/dm3 sodium hy-
move carbon black. Such Poss of carbon black is particularly droxide Solution (5.1.6).
likely to occur with carbon blacks of fine particle size.
iTeh STANDARD 5.3.14
5.3.5 Filter the warm Solution through the Gooch
PREVIEW Complete the quantitative transfer of the in-
(standards.iteh.ai)
soluble matter into the Gooch crucible by washing the
crucible (5.2.1) with the aid of a moderate vacuum,
beaker and the crucible with hydrochloric acid Solution
maintaining the greater part of the insoluble residue
in the beaker. (5.1.2).
ISO 1408:1995
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5.3.6 Wash the residue in the beaker three times 5.3.15 Wash the Gooch crucible with 10 cm3 of
67c26fa3ec00/iso-1408-1995
with three portions of 10 cm3 of warm nitric acid acetone (4.1.4).
(5.1.1) filtering the washings through the Gooch
crucible and maintaining the greatest patt of the in-
5.3.16 Dry the Gooch crucible at 850 “C +- 25 “C in
soluble matter in the beaker.
a nitrogen atmosphere using the tube furnace and
5.3.7 Discard the filtrate and wash the filter flask associated apparatus (4,2.2). Cool in the desiccator
thoroughly with water to remove all traces of nitric (4.2.4) and weigh to the nearest 0,l mg (mass m,).
acid. Record this mass.

WARNING - Nitrit acid and acetone may react 5.3.17 Disconnect the nitrogen flow to the tube fur-
and Cause an explosion nace and replace it with air or Oxygen (4.1.2). Heat the
Gooch crucible again at 850 “C + 25 “C until all traces
5.3.8 Wash the insoluble matter in the beaker three sf carbon black have disappeared. Cool the Gooch
times with three portions of 10 cm3 of acetone crucible in the desiccator and weigh to the nearest
(4.1.4), filtering the washings through the Gooch 0,l mg (mass mJ Record this mass.
crucible and maintaining the greater part of the in-
soluble matter in the beaker.
5.3.18 lt is essential to check the experimental pro-
cedure by first carrying out the complete procedure
5.3.9 Wash the insoluble matter in the beaker three
on a Sample containing a known amount of a similar
times with three portions of 10 cm3 of acetone-
grade of carbon black.
chloroform mixture (5.1.4) filtering the washings
through the Gooch crucible and maintaining the
greater part of the insoluble matter in the beaker. 5.3.19 Carry out the determination in duplicate.

5
ISO 1408:1995(E) 0 ISO

5.4 Expression of results 6.2.1 Flat-bottomed flask, capacity 150 cm3, with
conical ground-glass joint, 34/35, female, complying
Calculate the carbon black content, as a percentage with the requirements of ISO 383.
by mass, from the formula
6.2.2 Air condenser, with conical ground-glass joint,
ml - m2
x 100 34/35, female, complying with the requirements of
mo
ISO 383.
where
6.2.3 Water-cooled condenser, length 250 mm,
mo is the mass, in grams, of the test piece with conical ground-glass joint, 34/35, male, comply-
(see 5.3.1);
ing with the requirements of ISO 383.
is the mass, in grams, of the Gooch
crucible and its contents after drying at 6.2.4 Hotplate, capable of being maintained at
850 “C in nitrogen (see 5.3.16); 200 “C.

% is the mass, in grams, of the Gooch

6.2.5 Gooch crucible with a filtering layer, pre-
crucible and its contents after heating at
pared as specified in 5.2 but treated in accordance
850 “C in air or Oxygen (see 5.3.17).
with the procedures described in 6.3.7 to 6.3.15 and
NOTE 6 Any matter volatile at 850 “C in the carbon black then heated at 850 “C -+ 25 “C for 2 h.
(as purchased) will be los-t during the pyrolysis in nitrogen.
The final result for the mass percentage of carbon black will
therefore be low by this amount. In cases where the carbon 6.3 Procedure
black type and origin are known, a suitable correction tan
be made. iTeh STANDARD PREVIEW
6.3.1 Weigh a test piece of about 0,3 g to 0,5 g of
thinly sheeted Sample to the nearest 0,l mg (mass
6 Method C (standards.iteh.ai)
q). Record this mass. Place the test piece in a flask
containing 20 g of dichlorobenzene (6.1 .l).
WARNING - Because of possible health and ISO 1408:1995
safety hazards inherent in https://standards.iteh.ai/catalog/standards/sist/a7b0b4de-bc63-44f5-b9be-
this method, recog- 6.3.2 Reflux the mixture gently (to avoid charring) in
nized health and safety precautions shall be67c26fa3ec00/iso-1408-1995
ob- an efficient fume cupboard (hood) using the air
served with the use of Peroxides and solvents. All condenser (6.2.2) for 30 min to 60 min.
operations shall be carried out in a properly ven-
tilated fume hood, and safety glasses shall be NOTE 7 It may be beneficial to stir the mixture, while
worn during digestions, extractions and refluxing, to minimize the possibility of charring. This tan
conveniently be done by using a PTFE-coated stirring bar
washings.
and a magnetic stirrer.

6.1 Reagents 6.3.3 After allowing the mixture produced in 6.3.2 to

cool to 80 “C to 90 “C, replace the air condenser with
Reagents specified in 4.1 and 5.1, plus the following:
the water-cooled condenser (6.2.3) and add 5 cm3 of
tert--butyI hydroperoxide Solution (6.1.2).
6.1 .l 1,4=Dichlorobenzene (pdichlorobenzene) or
1.2.dichlorobenzene (odichlorobenzene).
6.3.4 Reflux the mixture gently in the fume cup-
6.1.2 tert-Butyl hydroperoxide Solution, 60 % board (hood) for 30 min to 60 min, then cool to 50 “C
to 60 “C.
minimum purity. The remaining 40 % is commonly
water or di-tert-butyl peroxide or te&utanoI.
6.3.5 Add, through the condenser, 100 cm3 to
This solution is stable for several months, if stored in 150 cm3 of toluene (6.1.3).
a cool place.
6.3.6 Allow the Solution to stand for 1 h to 2 h. At
6.1.3 Toluene. the end of this period, the insoluble matter has to be
settled on the bottom of the flask and the Solution has
6.2 Apparatus to be clear. If the Solution is no% clear after standing
for 2 h, repeat the determination, increasing the times
Apparatus specified in 4.2 and 5.2, plus the following: specified in 6.3.2 and 6.3.4.

6
0 ISO ISO 1408:1995(E)

6.3.7 Filter through the Gooch crucible (6.2.5) under 64. Expression of results
moderate vacuum, and wash the flask three times
with three portions of 10 cm3 of toluene (6.1.3), fil- Calculate the carbon black content, as a percentage
tering the washings through the Gooch crucible. If any by mass, from the formula
Problem occurs with the filtration, repeat the deter-
mination, but use acetone (4.1.4) instead of toluene ml - m2
x 100
(6.1.3) in 6.3.5 and 6.3.7. Check that the filtrate is free mo
from carbon black, then discard the filtrate.
where
6.3.8 Wash the flask three times with three portions is the mass, in grams, of the test piece
mo
of 10 cm3 of acetone (4.1.4), filtering the washings (see 6.3.1);
through the Gooch crucible.
m1 is the mass, in grams, of the Gooch
6.3.9 Discard the filtrate and wash the filter flask crucible and its contents after drying at
with water. 850 “C in nitrogen (see 6.3.14);

WARNING - Nitrit acid and acetone may react m, is the mass, in grams, of the Gooch
and Cause an explosion crucible and its contents after heating at
850 “C in air or Oxygen (see 6.3.15).
6.3.10 Wash the flask and the Gooch crucible three
times with three portions of 10 cm3 of warm nitric NOTE 8 Any matter volatile at 850 “C in the carbon black
acid (5.1 .l). (as purchased) will be lost during the pyrolysis in nitrogen.
The final result for the mass percentage of carbon black will
therefore be low by this amount. In cases where the carbon
6.3.11 Wash the flask and the Gooch crucible with black type and origin are known, a suitable correction tan
the hydrochloric acid solution (5.1.2) and complete the
iTeh STANDARD PREVIEW
quantitative transfer of the insoluble matter to the
be made.

Gooch crucible. (standards.iteh.ai)

6.3.12 Discard the filtrate and wash the filter flask
with water.
ISO 1408:1995
https://standards.iteh.ai/catalog/standards/sist/a7b0b4de-bc63-44f5-b9be-
7 Test report
67c26fa3ec00/iso-1408-1995
6.3.13 Wash the Gooch crucible with 10 cm3 of
acetone (4.1.4).
The test report shall include the following particulars:
6.3.14 Dry the Gooch crucible at 850 “C -+ 25 “C in
a) a reference to this International Standard;
a nitrogen atmosphere, using the tube furnace and
associated apparatus (4.2.2). Allow to cool in the b) all details necessary for complete identification of
desiccator (4.2.4) and weigh to the nearest 0,l mg the Sample;
(mass m-,). Record this mass.
c) the method used (method A, B or C);
6.3.15 Disconnect the nitrogen flow to the tube fur-
nace and replace it with air or Oxygen (4.1.2). Heat the d) the mean of the two results and the units in which
Gooch crucible again at 850 “C -+ 25 “C until all traces they are expressed;
of carbon black have disappeared. Allow the Gooch
crucible to cool in the desiccator and weigh to the e) any unusual features noted during the determi-
nearest 0,l mg (mass q). nation;

6.3.16 lt is essential to check the experimental pro- f) any Operation not included in this International
cedure by first carrying out the complete procedure Standard or in the International Standards to
on a Sample containing a known amount of a similar which reference is made, as well as any Operation
grade of carbon black. regarded as optional;

6.3.17 Carry out the determination in duplicate. 9) the date of the test.