Plastics - Determination of the tendency of compounds and products based on vinyl chloride homopolymers and copolymers to evolve hydrogen chloride and any other acidic products at elevated temperatures - Part 3: Conductometric method (ISO 182-3:1993)

The principle of the method is maintaining a test portion of the PVC at an agreed temperature in a nitrogen gas stream, absorbing the hydrogen chloride evolved in a given amount of demineralized water, and potentiometrically determining the amount of hydrogen chloride evolved in relation to the recorded change in conductivity of the water. The method is recommended for compounded PVC materials and products only, although it can be used for polymers in powder form under appropriate conditions.

Kunststoffe - Bestimmung der Neigung von Formmassen und Erzeugnissen auf der Basis von Vinyl-chlorid-Homopolymeren und -Copolymeren, bei erhöhten Temperaturen Chlorwasserstoff und andere saure Produkte abzugeben - Teil 3: Leitfähigkeitsverfahren (ISO 182-3:1993)

Dieser Teil von ISO 182 legt ein Verfahren zur Bestimmung der thermischen Stabilität bei erhöhter Temperatur von Formmassen und Erzeugnissen fest, die auf der Grundlage von Vinylchlorid-Homopolymeren und -Copolymeren (im folgenden Text abgekürzt als PVC) hergestellt sind und die zum Chlorwasserstoffverlust neigen (Entwicklung von Chlorwasserstoff). Das Verfahren kann zur Qualitätskontrolle während der Herstellung und Umwandlung von PVC-Formmassen angewendet werden.

Plastiques - Détermination de la tendance des compositions à base d'homopolymères et copolymères du chlorure de vinyle à dégager du chlorure d'hydrogène et éventuellement d'autres produits acides à températures élevées - Partie 3: Méthode conductimétrique (ISO 182-3:1993)

Polimerni materiali - Ugotavljanje tendence zmesi in proizvodov na osnovi homo- in kopolimerov vinilklorida, da pri povišanih temperaturah sproščajo klorovodik ali druge kisle produkte - 3. del: Konduktometrijska metoda (ISO 182-3:1993)

General Information

Status
Withdrawn
Publication Date
19-Sep-2000
Withdrawal Date
12-Dec-2023
Technical Committee
Drafting Committee
Current Stage

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SLOVENSKI STANDARD
01-junij-2001
3ROLPHUQLPDWHULDOL8JRWDYOMDQMHWHQGHQFH]PHVLLQSURL]YRGRYQDRVQRYLKRPR
LQNRSROLPHURYYLQLONORULGDGDSULSRYLãDQLKWHPSHUDWXUDKVSURãþDMRNORURYRGLNDOL
GUXJHNLVOHSURGXNWHGHO.RQGXNWRPHWULMVNDPHWRGD ,62
Plastics - Determination of the tendency of compounds and products based on vinyl
chloride homopolymers and copolymers to evolve hydrogen chloride and any other acidic
products at elevated temperatures - Part 3: Conductometric method (ISO 182-3:1993)
Kunststoffe - Bestimmung der Neigung von Formmassen und Erzeugnissen auf der
Basis von Vinyl-chlorid-Homopolymeren und -Copolymeren, bei erhöhten Temperaturen
Chlorwasserstoff
und andere saure Produkte abzugeben - Teil 3: Leitfähigkeitsverfahren (ISO 182-3:1993)
Plastiques - Détermination de la tendance des compositions a base d'homopolymeres et
copolymeres du chlorure de vinyle a dégager du chlorure d'hydrogene et éventuellement
d'autres produits acides a températures élevées - Partie 3: Méthode conductimétrique
(ISO 182-3:1993)
Ta slovenski standard je istoveten z: EN ISO 182-3:2000
ICS:
83.080.20 Plastomeri Thermoplastic materials
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

INTERNATIONAL IS0
STANDARD 182-3
First edition
1993-04-01
Plastics - Determination of the tendency
of compounds and products based on vinyl
chloride homopolymers and copolymers to
evolve hydrogen chloride and any other
acidic products at elevated
temperatures -
Part 3:
Conductometric method
Plas tiques - 06termination de la tendance des compositions 2 base
d ’homopolym&es et copolym&res du chlorure de vinyle ;i dkgager du
chlorure d ’hydrogkne et 6ventuellement d ’autres produits acides 9
temperatures 6lev6es -
Par-tie 3: Mkthode conductim&rique
Reference number
IS0 182-3:1993(E)
IS0 182=3:1993(E)
Foreword
IS0 (the International Organization for Standardization) is a worldwide
federation of national standards bodies (IS0 member bodies). The work
of preparing International Standards is normally carried out through IS0
technical committees. Each 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. IS0
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 IS0 182-3 was prepared by Technical Committee
lSO/TC 61, Plastics, Sub-Committee SC 6, Ageing, chemical and environ-
mental resistance.
Together with the three other parts of IS0 182, it cancels and replaces IS0
Recommendation R 182:1970, of which the four parts of IS0 182 consti-
tute a technical revision.
IS0 182 consists of the following parts, under the general title
Plastics - Determination of the tendency of compounds and products
based on vinyl chloride homopolymers and copolymers to evolve hydrogen
chloride and any other acidic products at elevated temperatures:
- Part 1: Congo red method
- Part 2: pH method
- Part 3: Conductometric method
- Part 4: Po tentiometric method
Annexes A, B and C of this part of IS0 182 are for information only.
0 IS0 1993
All rights resewed. No part of this publication may be reproduced or utilized in any form or
by any means, electronic or mechanical, including photocopying and microfilm, without per-
mission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-1211 Geneve 20 l Switzerland
Printed in Switzerland
ii
INTERNATIONAL STANDARD IS0 182=3:1993(E)
Plastics - Determination of the tendency of
compounds and products based on vinyl chloride
homopolymers and copolymers to evolve hydrogen
chloride and any other acidic products at elevated
temperatures -
Part 3: -
Conductometric method
WARNING - The use of this part of IS0 182 may involve hazardous materials, operations and
equipment. This part of IS0 182 does not purport to address all of the safety problems associated
with its use. It is the responsibility of the user of this part of IS0 182 to establish appropriate safety
and health practices and determine the applicability of regulatory limitations prior to use.
compounds in the form of dry blends, since such
1 Scope
materials may not be sufficiently homogeneous.
1.1 This part of IS0 182 specifies a method for the
1.4 PVC compounds and products may evolve other
determination of the thermal stability at elevated
in addition to hydrogen
decomposition products,
temperature of compounds and products based on
chloride, at elevated temperatures. A limited number
vinyl chloride homopolymers and copolymers (in the
of these decomposition products may affect the con-
following text abbreviated as PVC) which undergo
ductivity of water when they are absorbed into it.
dehydrochlorination (the evolution of hydrogen chlor-
Compensation for this effect is not within the scope
de).
of this part of IS0 182, and therefore care is necess-
ary in attempting to compare results for dissimilar
compounds and products. In this case a method suit-
1.2 The method may be used as a quality control
able for the determination of chloride ion (Cl-) in the
test during manufacture and conversion of PVC com-
absorbing solution shall be used (see IS0 182-4).
pounds. It may also be used for the characterization
of PVC compounds and products, especially with re-
1.5 The method may also be applied to other plas-
gard to the effectiveness of their heat-stabilizing sys-
tics materials which can evolve hydrogen chloride or
tems.
other hydrogen halides when heated under the con-
It is suitable for coloured PVC compounds and prod-
ditions prescribed by the relevant specifications, or as
ucts where a discolouration test under the action of agreed upon between the interested parties.
heat may be unsatisfactory.
2 Normative references
1.3 The method is recommended for compounded
PVC materials and products only, although it can be The following standards contain provisions which,
through reference in this text, constitute provisions
used for polymers in powder form under appropriate
conditions, to be agreed upon between the interested of this part of IS0 182. At the time of publication, the
parties. The method is not recommended for PVC editions indicated were valid. All standards are subject
IS0 182=3:1993(E)
to revision, and parties to agreements based on this
5.1 Pure nitrogen, containing less than 6 ppm oxy-
part of IS0 182 are encouraged to investigate the
gen and less than 0,l ppm carbon dioxide by volume.
possibility of applying the most recent editions of the
The purity shall be such that when the gas is passed
standards indicated below. Members of IEC and IS0
through demineralized water (see 5.3) for 1 h at a rate
maintain registers of currently valid International
of 7,2 I/h + 0,l I/h, the conductivity of the water re-
Standards.
mains unchanged.
The gas shall be dried by passing it through a suitable
IS0 182-4:1993, Plastics - Determination of the
drying agent, and the flow-rate through the
tendency of compounds and products based on vinyl
dehydrochlorination cell adjusted by means of a nee-
chloride homopoiymers and copolymers to evolve hy-
dle valve and measured using a suitable flowmeter.
drogen chloride and any other acidic products at ele-
va ted temperatures - Part 4:
Po ten tiome tric
method. 5.2 Hydrochloric
acid, aqueous solution,
c(HCI) = 0,l mol/l.
IS0 565:1990, Test sieves - Metal wire cloth, per-
forated metal plate and electroformed sheet - Nom-
5.3 Demineralized water, with a pH of 4,0 + 0,l
inal sizes of openings.
and a conductivity not greater than 40 j&cm, ad-
justed by the addition of 0,l mol/l hydrochloric acid.
IS0 4793: 1980, Laboratory sintered (fritted) filters -
Porosity grading, classification and designation.
6 Apparatus
IS0 6353-2: 1983, Reagents for chemical analysis -
The general arrangement of the apparatus is shown
Part 2: Specifications - First series.
in figure 1. The figure shows a re-usable
dehydrochlorination cell A. This cell may be replaced
3 Definition
by a disposable cell B.
For the purposes of this part of IS0 182, the following
6.1 Dehydrochlorination cells.
definition applies.
Cell A (re-usable), with shape and dimensions
6.1.1
3.1 stability time, ts: Time, measured by reference
as shown in figure2.
to a predetermined change in the conductivity of ab-
sorbing demineralized water, required for a certain
A recommended procedure for cleaning the cell is
amount of hydrogen chloride to be evolved when a
given in annex A.
prescribed mass of PVC compound or product is
maintained at an elevated temperature under the test
6.1.2 Cell B (disposable),
with shape and dimen-
conditions specified in this part of IS0 182.
sions as shown in figure3.
4 Principle NOTE 1 Other types of cell may be employed if it has
been proved that the results obtained are equivalent to
those obtained with one of the cells described in 6.1 .I and
A test portion of the PVC compound or product is
6.1.2.
maintained at an agreed temperature in a nitrogen gas
stream and the hydrogen chloride evolved is absorbed
in a given amount of demineralized water. The 6.2 Test portion holder, for use with cell A. The
amount of hydrogen chloride evolved is determined in test portion is supported on a porous sintered-glass
relation to the recorded change in conductivity of the disc (grade P 100, IS0 4793), 10 mm in diameter.
water.
To prevent blocking of the porous disc, it is advisable
to place a thin, soft layer of glass wool between it and
5 Reagents
the test portion.
During the test, use only reagents of recognized ana- A recommended procedure for cleaning the disc sup-
lytical grade in accordance with IS0 6353-2. port is given in annex A.

IS0 182=3:1993(E)
1 N2 cylinder
9 Thermometer (scale division 0,l"C)
2 Purification train 10 Silicone oil
3 Ball flowmeter 11 Magnetic stirrer
4 Electronic temperature controller (scale division 0,l"C) 12 Absorbing solution
5 Temperaturesensor
13 Measuring electrode(s)
6 Heating bath
14 Conductancemeter
7 PVCtestportion
15 Recorder
8 Dehydrochlorination cell
Figure 1 - General arrangement of apparatus

IS0 182-3:1993(E)
Dimersions in millimetres
I
I
Spurs
17 coils
Sintered-glass disc,
10 mm diameter (removable)
Figure 2 - Cell A (re-usable) for dehydrochlorination of PVC samples

IS0 182=3:1993(E)
6.6 Thermometer, with a scale suitable for reading
the heating bath temperature in the range 170 “C to
Dimensions in millimetres
210 “C and with a scale division of 0,l “C.
@ int. 6
L.
6.7 Balance, with a scale division of 1 mg.
6.8 Measurement cell.
A suitable measurement cell is shown in figure6. If
the diameters of the measurement electrode and the
U-tube (wall
feed tube for the gases from decomposition of the
thickness I)
test portion are sufficiently small, a 300 ml
Erlenmeyer flask is a suitable alternative measure-
ment cell.
A recommended procedure for cleaning the cell is
given in annex A.
6.9 Magnetic stirrer, capable of providing gentle
agitation within the measurement cell.
6.10 Conductance meter, with a conductivity probe
Figure 3 - Cell B (disposable) for
constant of 1 cm- ‘, giving direct readings in @cm,
dehydrochlorination of PVC samples
and preferably equipped with an automatic tempera-
ture compensating device and an output for a chart
recorder.
NOTE 2 Graphite electrodes have been shown to operate
in a more trouble-free manner than platinized platinum
electrodes.
6.3 Glass connection tube, for use with cell A,
having dimensions as shown in figure4. The con-
6.11 Stopclock, or other suitable timing device, if
nection tube is secured to cell A by two springs fixed
not included in the recorder.
to hooks on the ground-glass joints. The tube shall be
provided with an insulating jacket.
6.12 Flowmeter, for example a rotameter, or other
suitable device capable of measuring a gas flow-rate
within the range 120 cm3/min + 4 cm3/min.
6.4 Expansion joints and cell connections, for use
with cell B. Cell B is connected to the apparatus
7 Preparation of test samples
through flexible polytetrafluoroethylene (PTFE) and
silicone rubber tubes. Special joints allow for thermal
The measured stability times ts depend to some ex-
expansion. The complete joint arrangement is shown
tent on the surface area of the prepared test portions
in figure 5.
as well as on their thermal history. Any cutting or
grinding of a material necessary to produce the test
portions shall be conducted in a uniform manner,
avoiding heating of the material.
NOTE 3 Cryogenic grinding is recommended.
6.5 Oil bath, with a capacity of at least 10 I. The
bath shall be capable of operating in the temperature
range 170 “C to 210 “C and of maintaining the test
7.1 PVC plastisols
temperature with an accuracy of + 0,l “C.
-
The bath shall be designed so that the temperature
Spread these materials on glass plates and gel them
distribution is even throughout, and shall have a ther- in an oven at an agreed temperature so that sheets
mal capacity sufficient to avoid temperature change 0,5 mm thick are formed. Cut these sheets into
when the dehydrochlorination cell is immersed in it.
squares approximately 2 mm on a side.
IS0 182=3:1993(E)
Dimensions in millimetres
Y
@ ext. 4
@ int. 2
a
a) Glass tube for use with cell A
b) PTFE tubing for use with cell B
...

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