Download as pdf or txt
Download as pdf or txt
You are on page 1of 12

BRITISH STANDARD BS 2782-7:

Method
732F:1991
ISO 1628-6:
1990

Methods of testing

Plastics —
Part 7: Rheological properties —

Method 732F: Determination of


viscosity number of methyl
methacrylate polymers

IMPORTANT NOTE. Before reading this method it is essential to read


BS 2782-0, Introduction, issued separately.
BS 2782-7:Method 732F:1991

Committees responsible for this


British Standard

The preparation of this British Standard was entrusted by the Plastics and
Rubber Standards Policy Committee (PRM/-) to Technical Committee PRM/21,
upon which the following bodies were represented:

British Plastics Federation


British Steel Industry
British Telecommunications plc
British Textile Confederation
Department of Trade and Industry (National Physical Laboratory)
EEA (the Association of Electronics, Telecommunications and Business
Equipment Industries)
Electrical and Electronic Insulation Association (BEAMA Ltd.)
Electrical Installation Equipment Manufacturers’ Association (BEAMA Ltd.)
GAMBICA (BEAMA Ltd.)
Ministry of Defence
Packaging and Industrial Films Association
PIRA
Plastic Industrial Containers Association
Plastics and Rubber Institute
RAPRA Technology Ltd.
Standards Association of Australia
Yarsley Technical Centre Ltd.

This British Standard, having


been prepared under the
direction of the Plastics and
Rubber Standards Policy
Committee, was published
under the authority of the
Standards Board and comes
into effect on Amendments issued since publication
28 June 1991

© BSI 12-1999 Amd. No. Date Comments

The following BSI references


relate to the work on this
standard:
Committee reference PRM/21
Draft for comment 87/38634 DC

ISBN 0 580 19774 3


BS 2782-7:Method 732F:1991

Contents

Page
Committees responsible Inside front cover
National foreword ii
1 Scope 1
2 Normative references 1
3 Definitions and units 1
4 Principle 1
5 Measurements 1
6 Apparatus 1
7 Solvent and test solution 2
8 Temperature of measurement 2
9 Procedure 2
10 Expression of results 2
11 Test report 3
Annex A (normative) Calibration of the viscometer 4
Annex B (normative) Determination of the limiting viscosity number 5
Annex C (informative) Bibliography 5
Figure A.1 — Kinetic energy correction as a function of the
reciprocal of efflux time 5
Publication(s) referred to Inside back cover

© BSI 12-1999 i
BS 2782-7:Method 732F:1991

National foreword

This British Standard has been prepared under the direction of the Plastics and
Rubber Standards Policy Committee and is identical with ISO 1628-6:1990
“Plastics — Determination of viscosity number and limiting viscosity number —
Part 6: Methyl methacrylate polymers”, published by the International
Organization for Standardization (ISO).
Cross-references
International Standard Corresponding British Standard
ISO 1628-1:1984 BS 2782 Methods of testing plastics
Method 732A:1991 Determination of viscosity
number: general conditions
(Identical)
ISO 4793:1980 BS 1752:1983 Specification for laboratory sintered or
fritted filters including porosity grading
(Identical)
The Technical Committee has reviewed the provisions of ISO 3105:1976 and
ISO 8257-1:1987, to which reference is made in the text, and has decided that
they are acceptable for use in conjunction with this standard.
WARNING NOTE. This British Standard, which is identical with ISO 1628-6,
does not necessarily detail all the precautions necessary to meet the requirements
of the Health and Safety at Work etc. Act 1974. Attention should be paid to any
appropriate safety precautions and the method should be operated only by
trained personnel.
A British Standard does not purport to include all the necessary provisions of a
contract. Users of British Standards are responsible for their correct application.
Compliance with a British Standard does not of itself confer immunity
from legal obligations.

Summary of pages
This document comprises a front cover, an inside front cover, pages i and ii,
pages 1 to 6, an inside back cover and a back cover.
This standard has been updated (see copyright date) and may have had
amendments incorporated. This will be indicated in the amendment table on the
inside front cover.

ii © BSI 12-1999
BS 2782-7:Method 732F:1991

1 Scope c is the concentration, in grams per millilitre, of


polymer in the solution.
This part of ISO 1628 specifies the conditions to be
NOTE If the solvent and solution densities Õ0 and Õ are
used for the determination of the viscosity number substantially equal, ½ in equation (1) may be replaced by É and ½0
of methyl methacrylate polymer moulding and by É0, where É and É0 are the kinematic viscosities, in square
extrusion materials in dilute solution. millimetres per second, of the solution and the solvent,
respectively (see clause 10).
It applies to methyl methacrylate (MMA)
homopolymers and copolymers, and mixtures of the 4 Principle
two with a minimum of 80 % (m/m) of MMA and up
to 20 % (m/m) of other monomers, with and without Determination of the efflux time at 25 °C ± 0,05 °C
additives, as defined in ISO 8257-1. of a solvent and of a polymer solution, having a
NOTE The dilute-solution viscosity of polymers can be also
specified concentration, in that solvent.
expressed as a limiting viscosity number [½] (see Annex B). Calculation of the viscosity number and the limiting
viscosity number from the above measurements and
2 Normative references the known concentration of the solution.
The following standards contain provisions which,
through reference in this text, constitute provisions 5 Measurements
of this part of ISO 1628. At the time of publication, The data needed to calculate the function defined in
the editions indicated were valid. All standards are clause 3 are obtained by means of a capillary tube
subject to revision, and parties to agreements based viscometer, as explained in clause 4 of
on this part of ISO 1628 are encouraged to ISO 1628-1:1984.
investigate the possibility of applying the most
The efflux time of a liquid is related to its viscosity
recent editions of the standards indicated below.
by the Poiseuille-Hagenbach-Couette equation:
Members of IEC and ISO maintain registers of
currently valid International Standards.
. . . (2)
ISO 1628-1:1984, Guidelines for the standardization
of methods for the determination of viscosity number
and limiting viscosity number of polymers in dilute where
solution — Part 1: General conditions. k is the viscometer constant, in square
ISO 3105:1976, Glass capillary kinematic millimetres per second squared;
viscometers — Specification and operating t is the efflux time, in seconds;
instructions.
%t is the kinetic energy correction (Hagenbach
ISO 4793:1980, Laboratory sintered (fritted) correction), in seconds;
filters — Porosity grading, classification and
Õ is the density, in grams per cubic centimetre,
designation.
of the liquid;
ISO 8257-1:1987, Plastics — Poly(methyl
A is a kinetic energy correction parameter, as
methacrylate) (PMMA) moulding and extrusion
defined in ISO 1628-1.
materials — Part 1: Designation.
NOTE The kinetic energy correction %t becomes insignificant if
it is less than 0,2 % of t. For Ubbelohde type OC apparatus, %t
3 Definitions and units can be neglected if the efflux time t is greater than 270 s; for
micro-Ubbelohde type MI apparatus, %t can be neglected if t is
For the purposes of this part of ISO 1628, the greater than 70 s.
following definition applies, in addition to those in
clause 3 of ISO 1628-1:1984. 6 Apparatus (see also ISO 1628-1:1984,
viscosity number, V.N. clause 5)
6.1 Capillary viscometer: suspended-level
. . . (1) Ubbelohde type OC apparatus with a capillary
diameter of 0,36 mm and measuring bulb of
volume 2 ml, in accordance with ISO 3105, or
where micro-Ubbelohde type MI viscometer, with a
V.N. is the viscosity number, in millilitres per capillary diameter of 0,40 mm and measuring bulb
gram; of volume 0,75 ml.
½ is the dynamic viscosity of the test solution, Any viscometer listed in ISO 3105 may be used,
in millipascal seconds; provided it gives results equivalent to those
½0 is the dynamic viscosity of the solvent, in obtained with the specified viscometers, which shall
millipascal seconds; be used in the event of a dispute.

© BSI 12-1999 1
BS 2782-7:Method 732F:1991

The calibration of the viscometer used shall be 8 Temperature of measurement


checked by the method specified in Annex A.
The temperature of measurement shall
6.2 Timing device, with an accuracy of 0,1 s for the be 25 °C ± 0,05 °C.
Ubbelohde type OC viscometer and 0,02 s for the
type MI viscometer. 9 Procedure (see also 1628-1:1984,
6.3 Thermostatic bath, capable of being maintained clause 8)
at a temperature of 25 °C ± 0,05 °C.
Using the sintered-glass filter (6.6), introduce the
6.4 One mark volumetric flask, of 100 ml capacity, chloroform solvent or the test solution directly into
fitted with a ground-glass stopper. the tube of the viscometer.
6.5 Balance, accurate to 0,1 mg. Determine the efflux times of the solvent and the
6.6 Sintered-glass filter funnel, with a maximum test solution at 25 °C ± 0,05 °C in three to five
pore diameter of 40 4m (porosity grade P 40 as passages through the same viscometer. If the
defined in ISO 4793). maximum difference between the efflux times
exceeds 0,2 s for a Ubbelohde type OC viscometer
6.7 Shaking machine or 0,03 s for a type MI viscometer, repeat the test
with the same test solution after cleaning the
viscometer with the solvent and drying it.
7 Solvent and test solution (see also The above procedure may be suitably modified if a
ISO 1628-1:1984, clause 6) viscometer other than the Ubbelohde as described in
7.1 Solvent ISO 3105 is used.
Chloroform, recognized analytical grade, 10 Expression of results (see also
stabilized with less than 1 % (V/V) of ethanol, kept ISO 1628-1:1984, clause 9)
in a brown bottle and stored in the dark.
Calculate the viscosity number V.N., expressed in
7.2 Sample
millilitres per gram, by means of the following
It is important that the sample is representative of equation (this equation is in accordance with
the material to be tested. ISO 1628-1, but includes the kinetic energy
7.3 Test solution concentration correction, which is necessary in order to obtain
accurate results with the viscometer sizes specified):
The solution concentration shall be 2,6 g of polymer
per litre of solution.
. . . (3)
7.4 Preparation of the test solution
Weigh, to the nearest 0,1 mg, 0,26 g ± 0,005 g of the
sample into the volumetric flask (6.4). Add 50 ml of where
chloroform (7.1) and dissolve the sample completely É is the viscosity of the test solution;
with shaking. Then make up to the mark with É0 is the viscosity of the solvent;
chloroform at 20 °C ± 1 °C and shake once more
briefly. t is the arithmetic mean of the values obtained
for the efflux time, in seconds, of the test
With polymers containing viscosity-increasing
solution;
additives requiring modifications to the solution
preparation process, such modifications shall be t0 is the arithmetic mean of the values obtained
agreed upon by the interested parties. for the efflux time, in seconds, of the solvent;
For materials containing pigments and/or special c is the concentration, expressed in grams per
additives, the quantity weighed into the volumetric millilitre, of the test solution;
flask shall be increased so that the test solution %t is the kinetic energy correction for t
contains 0,26 g of MMA homopolymers and (see Annex A);
copolymers per 100 ml. %t0 is the kinetic energy correction for t0
(see Annex A).

2 © BSI 12-1999
BS 2782-7:Method 732F:1991

The equation for the viscosity number given in


ISO 1628-1:
t–t
V.N. = ------------0- . . . (4)
t 0c

may be used to give results of similar accuracy if a


viscometer with a smaller capillary diameter is used
so that the kinetic energy correction is less
than 0,2 % of the efflux time.

11 Test report
See ISO 1628-1:1984, clause 10.

© BSI 12-1999 3
BS 2782-7:Method 732F:1991

Annex A (normative)
Calibration of the viscometer
A.1 Experience has shown that the required high accuracy of the viscosity number determination of MMA
homopolymer and copolymer solutions cannot always be achieved with commercially available Ubbelohde
viscometers because of minor irregularities in the capillary. It is therefore advisable to check the accuracy
of the viscometer by means of calibrating liquids whose kinematic viscosity[1] is known.
A.2 Viscometer constant k
Using n-undecane of recognized analytical grade at 25 °C, make three to five passages with the same
viscometer and determine the mean efflux time t in accordance with ISO 3105:1976, clause 5. Calculate the
viscometer constant k from the equation:

k = É-- . . . (A.1)
t

where É for n-undecane at 25 °C is 1,467 5 mm2/s.


NOTE The density Õ of n-undecane at 25 °C is 0,736 5 g/ml.
A.3 Kinetic energy corrections %t0 and %t
The energy correction can be neglected if it is less than 0,2 % of the efflux time.
The Ubbelohde type OC viscometer complies with this requirement if the efflux time is greater than 270 s
(ASTM viscometer).
The micro-Ubbelohde type MI viscometer complies if the efflux time is greater than 70 s.
If the efflux time is less than specified above, a kinetic energy correction shall be made for the viscometer,
using the following low-viscosity liquids as standards:
1. Dichloromethane (recognized
analytical grade) É25°C = 0,314 2 mm2/s
Õ25°C = 1,316 3 g/ml
2. Trichloroethylene (recognized
analytical grade) É25°C = 0,369 3 mm2/s
Õ25°C = 1,455 5 g/ml
3. Tetrachloroethylene (recognized
analytical grade) É25°C = 0,525 7 mm2/s
Õ25°C = 1,614 4 g/ml
Measure the efflux time of each standard liquid in three to five passages and determine the kinetic energy
correction %tsi for each liquid using the equation
É
%t si = t si – -----i . . . (A.2)
k
where
tsi is the efflux time, in seconds, of the ith standard liquid;
Éi is the kinematic viscosity, in square millimetres per second, of the ith standard liquid;
k is the viscometer constant, in square millimetres per second squared.
Linear interpolation, using the following equations, between the two efflux times ts1 and ts2 for the standard
liquids i = 1 and i = 2 (see Figure A.1) gives the kinematic energy correction %t0 for the efflux time t0 of the
solvent (chloroform):

. . . (A.3)

. . . (A.4)

4 © BSI 12-1999
BS 2782-7:Method 732F:1991

In the same manner, linear interpolation, using the following equations, between ts2 and ts3 gives %t for the
efflux time t of the test solution:

. . . (A.5)

. . . (A.6)

Figure A.1 — Kinetic energy correction as a function of the reciprocal of efflux time

Annex B (normative)
Determination of the limiting viscosity number
The limiting viscosity number [½] for methyl methacrylate polymer solutions may be calculated, in
millilitres per gram, from values obtained at a single concentration by use of the following equation[2]:

. . . (B.1)

where
½ is the dynamic viscosity, in millipascal seconds, of the solution;
½0 is the dynamic viscosity, in millipascal seconds, of the solvent;
c is the concentration of polymer, in grams per millilitre of solution.

Annex C (informative)
Bibliography
[1] BAUER, H., and MEERLENDER, G., Precise viscosity measurements of Newtonian liquids
with É < 1 mm2/s for the selection of suitable standards. Rheologica Acta 23: 514–521 (1984).
[2] BILLMEYER, F.W., Jr., Journal of Polymer Science 4: 83 (1949).

© BSI 12-1999 5
6 blank
BS 2782-7:Method 732F:1991

Publication(s) referred to

See national foreword.

© BSI 12-1999
BS 2782-7:
Method
732F:1991 BSI — British Standards Institution
ISO 1628-6:
BSI is the independent national body responsible for preparing
1990 British Standards. It presents the UK view on standards in Europe and at the
international level. It is incorporated by Royal Charter.

Revisions

British Standards are updated by amendment or revision. Users of


British Standards should make sure that they possess the latest amendments or
editions.

It is the constant aim of BSI to improve the quality of our products and services.
We would be grateful if anyone finding an inaccuracy or ambiguity while using
this British Standard would inform the Secretary of the technical committee
responsible, the identity of which can be found on the inside front cover.
Tel: 020 8996 9000. Fax: 020 8996 7400.

BSI offers members an individual updating service called PLUS which ensures
that subscribers automatically receive the latest editions of standards.

Buying standards

Orders for all BSI, international and foreign standards publications should be
addressed to Customer Services. Tel: 020 8996 9001. Fax: 020 8996 7001.

In response to orders for international standards, it is BSI policy to supply the


BSI implementation of those that have been published as British Standards,
unless otherwise requested.

Information on standards

BSI provides a wide range of information on national, European and


international standards through its Library and its Technical Help to Exporters
Service. Various BSI electronic information services are also available which give
details on all its products and services. Contact the Information Centre.
Tel: 020 8996 7111. Fax: 020 8996 7048.

Subscribing members of BSI are kept up to date with standards developments


and receive substantial discounts on the purchase price of standards. For details
of these and other benefits contact Membership Administration.
Tel: 020 8996 7002. Fax: 020 8996 7001.

Copyright

Copyright subsists in all BSI publications. BSI also holds the copyright, in the
UK, of the publications of the international standardization bodies. Except as
permitted under the Copyright, Designs and Patents Act 1988 no extract may be
reproduced, stored in a retrieval system or transmitted in any form or by any
means – electronic, photocopying, recording or otherwise – without prior written
permission from BSI.

This does not preclude the free use, in the course of implementing the standard,
of necessary details such as symbols, and size, type or grade designations. If these
details are to be used for any other purpose than implementation then the prior
written permission of BSI must be obtained.

If permission is granted, the terms may include royalty payments or a licensing


agreement. Details and advice can be obtained from the Copyright Manager.
BSI Tel: 020 8996 7070.
389 Chiswick High Road
London
W4 4AL

You might also like