malaysian standard

MALAYSIAN
STANDARD
MS ISO 1628-6:2008
PLASTICS - DETERMINATION OF VISCOSITY
NUMBER AND LIMITING VISCOSITY NUMBER PART 6: METHYL METHACRYLATE POLYMERS
(ISO 1628-6:1990, IDT)
ISO 1628-6:1990 is endorsed as Malaysian Standard with the
reference number MS ISO 1628-6:2008.
ICS: 83.080.20
Descriptors: viscosity, polymers, capillary viscometers, methyl methacrylate polymers
© Copyright 2008
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© STANDARDS MALAYSIA 2008 – All rights reserved
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© STANDARDS MALAYSIA 2008 – All rights reserved
MS ISO 1628-6:2008
CONTENTS
Page
Committee representation.....................................................................................................
ii
National foreword ..................................................................................................................
iii
1
Scope .......................................................................................................................
1
2
Normative references...............................................................................................
1
3
Definitions and units.................................................................................................
1
4
Principle ...................................................................................................................
1
5
Measurements .........................................................................................................
1
6
Apparatus.................................................................................................................
2
7
Solvent and test solution..........................................................................................
2
8
Temperature of measurement .................................................................................
2
9
Procedure ................................................................................................................
2
10
Expression of results................................................................................................
3
11
Test report................................................................................................................
3
Annexes
A
Calibration of the viscometer ...................................................................................
4
B
Determination of the limiting viscosity number ........................................................
6
C
Bibliography .............................................................................................................
6
© STANDARDS MALAYSIA 2008 – All rights reserved
i
MS ISO 1628-6:2008
Committee representation
The Plastics and Plastics Products Industry Standards Committee (ISC J) under whose authority this Malaysian
Standard was adopted, comprises representatives from the following organisations:
Department of Standards Malaysia
Federation of Malaysian Manufacturers
Jabatan Kerja Raya Malaysia
Malaysian Association of Standards Users
Malaysian Institute of Chemistry
Malaysian Petrochemical Association
Malaysian Plastics Manufacturers Association
Malaysian Rubber Board
Ministry of Domestic Trade and Consumers Affairs
Ministry of Health Malaysia
Ministry of International Trade and Industry Malaysia
Plastics and Rubber Institute of Malaysia
SIRIM Berhad (Advanced Polymer and Composites Programme)
SIRIM QAS International Sdn Bhd
The Institution of Engineers, Malaysia
Universiti Kebangsaan Malaysia
Universiti Sains Malaysia
Universiti Teknologi Malaysia
The Technical Committee on General and Raw Materials for Plastics which recommends adoption of the ISO
Standard consists of representatives from the following organisations:
Federation of Malaysian Manufacturers (Hercules Sdn Bhd)
Malaysian Petrochemical Association (Dow Chemical (Malaysia) Sdn Bhd)
Malaysian Plastics Manufacturers Association (Industrial Resins (Malaysia) Berhad)
Petronas Polymer Technology Centre
SIRIM Berhad (Advanced Polymer and Composites Programme)
SIRIM Berhad (Secretariat)
SIRIM QAS International Sdn Bhd (Civil and Construction Section)
Universiti Malaya
Vinyl Chloride (Malaysia) Sdn Bhd
ii
© STANDARDS MALAYSIA 2008 – All rights reserved
MS ISO 1628-6:2008
NATIONAL FOREWORD
The adoption of the ISO Standard as a Malaysian Standard was recommended by the
Technical Committee on General and Raw Materials for Plastics under the authority of the
Plastics and Plastics Products Industry Standards Committee.
This Malaysian Standard 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). However, for the
purposes of this Malaysian Standard, the following apply:
a)
in the source text, “this International Standard” should read “this Malaysian Standard”;
b)
the comma which is used as a decimal sign (if any), to read as a point; and
c)
reference(s) to International Standard(s) should be replaced by equivalent Malaysian
Standard(s) as follows:
Referenced International Standard
Corresponding Malaysian Standard
ISO 1628-1:1984, Plastics - Determination of
the viscosity of polymers in dilute solution
using capillary viscometers - Part 1: General
Principles
MS
ISO
1628-1:2004,
Plastics
Determination of the viscosity of polymers in
dilute solution using capillary viscometers Part 1: General Principles
Compliance with a Malaysian Standard does not of itself confer immunity from legal
obligations.
NOTE. IDT on the front cover indicates an identical standard i.e. a standard where the technical content, structure,
and wording (or is an identical translation) of a Malaysian Standard is exactly the same as in an International
Standard or is identical in technical content and structure although it may contain the minimal editorial changes
specified in clause 4.2 of ISO/IEC Guide 21-1.
© STANDARDS MALAYSIA 2008 – All rights reserved
iii
INTERNATIONAL
STANDARD
.
ISO
1628-6.
First edition
1990-02-01
Plastics - Determination
of viscosity
and limiting viscosity number -
number
Part 6:
Methyl methacrylate polymers
Hastiques - Dt2termination de l’indice de viscosittS et de l’indice limite de
viscositb Partie 6: Polymkres de mbhacrylate
de m&h yle
Reference number
ISO 1628-6 : 1990 (El
ISOl628-6:199O(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of
national Standards bodies (ISO member bedies). 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 approval before their acceptance as International Standards by
the ISO Council. They are approved in accordance with ISO procedures requiring at
least 75 % approval by the member bodies voting.
International Standard ISO 1628-6 was prepared by Technical Committee ISO/TC 61,
Plastics.
lt cancels and replaces International Standard ISO 1233 : 1975, of which it constitutes
a technical revision.
ISO 1628 consists of the following Parts, under the general title Plastics - Determination of viscosity number and limiting viscosity number 1):
-
Part 1: General conditions
-
Part 2: Polyfvinyl chloride) resins
-
Part 3: Polyeth ylenes and polyprop ylenes
-
Part 4: Polycarbonate (PC) moulding and extrusion materials
-
Part 5: Poly(alkylene tereph thala tes)
-
Part 6: Methyl methacrylate polymers
Annexes A and B form an integral part of this part of ISO 1628. Annex C is for information only.
1) The general title of ISO 1628-1 is Guide/i.es for the Standardkation of methods for the determination of viscosity number and limiting viscosity number of polymers in dilute solution.
0 ISO 1990
All rights reserved. No patt 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-1211 Geneve 20 l Switzerland
Printed in Switzerland
ii
INTERNATIONAL
Plastics
viscosity
-
STANDARD
ISO 1628-6 : 1990 (E)
Determination
number -
Part 6:
Methyl methacrylate
of viscosity
number
and limiting
Polymers
1 Scope
3
This patt of ISO 1628 specifies the conditions to be used for the
determination of the viscosity number of methyl methacrylate
polymer moulding and extrusion materials in dilute solution.
For the purposes of this part of ISO 1628, the following
definition applies, in addition to those in clause 3 of
ISO 1628-1 : 1984.
lt applies to methyl methacrylate (MMA)
copolymers, and mixtures of the two with
(mlm) of MMA and up to 20 % (mlm)
with and without additives, as defined in
homopolymers and
a minimum of 80 %
of other monomers,
ISO 8257-1.
Definitions
viscosity
number,
V.N. = -
1
C
and units
V. N. :
r - f-70
( VO >
. . . (1)
where
NOTE - The dilute-Solution viscosity of Polymers tan be also expressed as a limiting viscosity number [VI (sec annex 6).
V. N.
is the viscosity number, in millilitres per gram;
q is the dynamic
millipascal seconds;
2
Normative
references
The following Standards contain provisions which, through
reference in this text, constitute provisions of this part of
ISO 1628. At the time of publication, the editions indicated
were valid. All Standards are subject to revision, and Parties to
agreements based on this part of ISO 1628 are encouraged to
investigate the possibility of applying the most recent editions
of the Standards indicated below. Members of IEC and ISO
maintain registers of currently valid International Standards.
viscosity
of the test
Solution,
in
q. is the dynamic viscosity of the solvent, in millipascal
seconds;
c is the concentration,
the Solution.
in grams per millilitre, of polymer in
NOTE - If the solvent and Solution densities eo and Q are substantially
equal, q in equation (1) may be replaced by v and ylo by vo, where v and
v. are the kinematic viscosities, in Square millimetres per second, of the
solution and the solvent, respectively (sec clause IO).
ISO 1628-1 : 1984, Guidelines for the standardization
of
methods for the determination of viscosity number and limiting
viscosity number of Polymers in dilute Solution - Part 7:
General conditions.
4
IS 0 3105 : 1976, Glass capillary kinema tic
Specifica tion and Opera ting instructions.
Calculation of the viscosity number and the limiting viscosity
number from the above measurements and the known concentration of the Solution.
viscometers
-
ISO 4793 : 1980, Laboratory sintered (fritted) filters - Porosity
grading, classifica tion and designa tion.
ISO 8257-1: 1987,
(PMMA) moulding
na tion.
Plastics Polyfmethyl
and extrusion materials -
methacrylate)
Part 1: Desig-
Principle
Determination of the efflux time at 25 OC + 0,05 OC of a solvent and of a polymer Solution, having a specified concentration, in that solvent.
5
Measurements
The data needed to calculate the function defined in clause 3
are obtained by means of a capillary tube viscometer, as
explained in clause 4 of ISO 1628-1 : 1984.
1
ISO 1628-6 : 1990 (E)
The efflux time of a liquid is related to its viscosity
Poiseuille-Hagenbach-Couette
equation :
= !!- = k(t - At) = kt - -A
t
e
V
k
is the viscometer
second squared;
constant,
by the
. . .
in Square millimetres
7.1
Per
Chloroform,
recognized analytical grade, stabilized with less
than 1 % (V/ V) of ethanol, kept in a brown bottle and stored in
the dark.
(Hagenbach
Q is the density, in grams per cubic centimetre,
liquid;
of the
A
is a kinetic energy correction Parameter, as defined in
ISO 1628-1.
NOTE - The kinetic energy correction At becomes insignificant if it is
less than 0,2 % of t. For Ubbelohde type OC apparatus, At tan be
neglected if the efflux time t is greater than 270 s; for micro-Ubbelohde
type MI apparatus, At tan be neglected if f is greater than 70 s.
6
Apparatus
(see also ISO 1628-1 : 1984, clause 5)
6.1 Capillary viscometer : suspended-level 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
micro-Ubbelohde
type MI viscometer,
with a capillary
diameter of 040 mm and measuring bulb of volume 0,75 ml.
The calibration of the viscometer used shall be checked by the
method specified in annex A.
6.2 Timing device, with an accuracy of 0,l s for the
Ubbelohde type OC viscometer and 0,02 s for the type MI
viscometer .
65.
Balance,
2
Shaking
of 100 ml capacity, fitted
accurate to 0,l mg.
6.6 Sintered-glass
diameter of 40 Fm
ISO 4793).
6.7
flask,
filter funnel, with a maximum pore
(porosity grade P 40 as defined in
machine.
Solvent
Sample
lt is important that the Sample is representative of the material
to be tested.
7.3
Test
solution
concentration
The Solution concentration
Solution.
7.4
Preparation
be 2,6 g of polymer per litre of
of the test
solution
Weigh, to the nearest 0,l mg, 0,26 g + 0,005 g of the Sample
into the volumetric flask (6.4). Add 50 ml of chloroform (7.1)
and dissolve the Sample completely with shaking. Then make
up to the mark with chloroform at 20 OC + 1 OC and Shake
once more briefly.
With polymers containing viscosity-increasing additives requiring modifications to the Solution preparation process, such
modifications shall be agreed upon by the interested Parties.
For materials containing Pigments and/or special additives, the
quantity weighed into the volumetric flask shall be increased so
that the test Solution contains 0,26 g of MMA homopolymers
and copolymers per 100 ml.
8
Temperature
of measurement
The temperature of measurement shall be 25 OC ?I 0,05 OC.
9
6.3 Thermostatic
bath, capable of being maintained at a
temperature of 25 OC + 0,05 OC.
6.4 One mark volumetric
with a ground-glass stopper.
(sec also
(2)
7.2
correction
Solvent and test solution
ISO 1628-1 : 1984, clause 6)
t is the efflux time, in seconds;
At .is the kinetic
energy
correction), in seconds;
7
Procedure
(see also 1628-1 : 1984, clause 8)
Using the sintered-glass filter (6.6), introduce the chloroform
solvent or the test Solution directly into the tube of the
viscometer .
Determine the efflux times of the solvent and the test Solution
at 25 OC + 0,05 OC in three to five passages through the same
viscometer. If the maximum differente between the efflux
times exceeds 0,2 s for a Ubbelohde type OC viscometer 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.
The above procedure may be suitably modified if a viscometer
other than the Ubbelohde as described in ISO 3105 is used.
ISO 1628-6 : 1990 (EI
10
Expression
of resuks (sec also ISO 1628-1 : 1984,
clause 9)
Calculate the viscosity number V.N., expressed in millilitres per
gram, by means of the following equation (this equation is in
accordance with ISO 1628-1, but includes the kinetic energy
correction, which is necessary in Order to obtain accurate
results with the viscometer sizes specified) :
t,
is the arithmetic mean of the values obtained for the
efflux time, in seconds, of the solvent;
c is the concentration,
the test Solution;
At
At,
expressed in grams per millilitre, of
is the kinetic energy correction for t (see annex A);
is the kinetic energy correction for t0 (see annex A).
The equation for the viscosity number given in ISO 1628-1:
V.N. = +(;-
l)=f(t;+;;O
- 1)
lmm (9)
VN = t _ t,
. .
. . . (4)
tOc
v
vO
is the viscosity of the test Solution;
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.
is the viscosity of the solvent;
t is the arithmetic mean of the values obtained for the
efflux time, in seconds, of the test Solution;
11 Test report
See ISO 1628-1 : 1984, clause 10.
3
ISO 1628-6 : 1990 (EI
Annex A
(normative)
Calibration
of the viscometer
A.l
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 U bbelohde viscometers because of minor
irregularities in the capillary. lt 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
k =- ’
. . . (A.1)
where v for n-undecane at 25 OC is 1,467 5 mm2/s.
NOTE - The density Q of n-undecane at 25 OC is 0,736 5 g/ml.
Kinetic energy corrections
At, and At
The energy correction tan be neglected if it is less than 0,2 %
of the efflux time.
The Ubbelohde type OC viscometer camplies with this requirement if the efflux time is greater than 270 s (ASTM
viscometer) .
Measure the efflux time of each Standard liquid in three to five
passages and determine the kinetic energy correction Atsi for
each liquid using the equation
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 :
(recognized
V25oc
@25OC
2. Trichloroethylene
analytical grade)
4
0,314 2 mm2ls
= 1,316 3 g/ml
=
(recognized
vBoc = 0,369 3 mm2/s
@25OC = 1,455 5 g/ml
. . . (A.2)
where
t SI*
is the efflux time, in seconds, of the ith Standard liquid;
is the kinema tic viscos Iity, in
vi
second, of the ith Standard liquid;
k
is the viscometer
second squared.
constant,
millimetres
Per
in Square millimetres
Per
Linear interpolation, using the following equations, between
the two efflux times ts, and te for the Standard liquids i = 1
and i = 2 (see figure A. 1) gives the kinematic energy correction
At, for the efflux time t, of the solvent (chloroform) :
At,=
42=
The micro-Ubbelohde type MI viscometer camplies if the efflux
time is greater than 70 s.
1. Dichloromethane
analytical grade)
v250c = 0,525 7 mm2/s
@25OC = 1,614 4 g/ml
Atsi = tsi - 2
Using n-undecane of recognized analytical grade at 25 OC,
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:
A.3
3. Tetrachloroethylene
(recognized analytical grade)
At,, - K,, (y-)
At,1
1
- At,
--
t sl
. . . (A.3)
At,,
- At,
1
-- 1
1
h2
t SI
t0
=-------
. . .
(A.4)
In the same manner, linear interpolation, using the following
equations, between tB and ta gives At for the efflux time t of
the test Solution:
At=Atd-K23(&-+)
FD=
At,
1
-k2
. . . (A-5)
- At,
1
h3
=
At,
- At
1
1
--P
h2
t
. . . (A-6)
hl
Ata
Ah
At
Afs3
111
fs- f&
Figure A.1 -
Kinetic
11
5 G
Reciprocal of
eff lux time
energy correction as a function
of efflux time
of the reciprocal
5
ISO 1628-6 I 1990 (i,
Annex B
(normative)
Determination
of the limiting
The limiting viscosity number [VI 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 [Zl :
viscosity
number
where
y~ is the dynamic viscosity, in millipascal seconds, of the
Solution;
Q is the dynamic viscosity, in millipascal seconds, of the
solvent;
[q] = f-f]
. . . (B.l)
csol;,i,n~
IS the concentration
of polymer, in grams per millilitre of
Annex C
(informative)
Bibliography
Hl
BAUER, H., and MEERENDER, G., Precise viscosity measurements of Newtonian liquids with v < 1 mm%
suitable Standards. Rheologica Acta 23: 514-521 (1984).
M
BILLMEYER,F.W., Jr., Journal of Polymer Science 4: 83 (1949).
UDC 678.744.335 : 532.13.08
Descriptors
: plastics,
Price based on 6 pages
6
polymers,
methylmethacrylate,
tests, physical tests, determination,
viscosity,
viscosity index.
for the selection of
Acknowledgements
Members of Technical Committee on General and Raw Materials for Plastics
Mr Ahmad Khairuddin Sha’aban (Chairman)
Dow Chemical (Malaysia) Sdn Bhd
Ms Noraslina Mat Zain (Secretary)
SIRIM Berhad
Mr Chu Tam Sang
Federation of Malaysian Manufacturers
Mr Umat Lokman Ahmad Johari
Petronas Polymer Technology Centre
Ms Zarina Rasmin
SIRIM Berhad (Advanced Polymer and
Composites Programme)
Ms Kamaliah Ahmad
SIRIM QAS International Sdn Bhd (Civil and
Construction Section)
Mr Mohd Helmee Mat Jenan
Vinyl Chloride (Malaysia) Sdn Bhd
© STANDARDS MALAYSIA 2008 – All rights reserved