Polyamide Viscosity Standard
Polyamide Viscosity Standard
STANDARD 307
Third edition
1994-09-01
(standards.iteh.ai)
ISO 307:1994
https://standards.iteh.ai/catalog/standards/sist/db4de2f9-82fd-4cdb-bf83-
4e15806c3328/iso-307-1994
Reference number
ISO 307: 1994(E)
ISO 307:1994(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.
0 ISO 1994
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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
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Printed in Switzerland
ii
INTERNATIONAL STANDARD 0 ISO ISO 307:1994(E)
This International Standard specifies a method for the ISO 599: 1985, Plastics - Polyamide homopolymers
determination of the viscosity number of dilute sol- - Determination of matter extractable by boiling
utions of polyamides in certain specified solvents. methanol.
The method is applicable to the polyamides desig- ISO 960: 1988, Plastics - Polyamides (PA) - Deter-
nated PA 6, PA 66, PA 69, PA 610, PA 612, PA 11, mina tion 0 f wa ter content.
iTeh STANDARDISOPREVIEW
PA 12 and PA MXD6 as defined in ISO 1874-1, as
well as to copolyamides and other polyamides that are 1042:1983, Laboratory glassware - One-mark
(standards.iteh.ai)
soluble in one of the specified solvents under the
specified conditions.
volume tric flasks.
The determination of the viscosity number of a ISO 3451-4:1986, Plastics - Determination of ash -
Polyamide provides a measure of the relative mol- Part 4: Polyamides.
ecular mass of the polymer.
ISO 6427:1992, Plastics - Determination of matter
extractable by organic solvents (conventional meth-
2 Normative references Ods).
The following Standards contain provisions which, ASTM D 789:1986, Standard test methods for deter-
through reference in this text, constitute provisions mination of relative viscosity, melting Point, and
of this International Standard. At the time of publi- moisture tonten t o f Polyamide (PA).
cation, the editions indicated were valid. All Standards
are subject to revision, and Parties to agreements
based on this International Standard are encouraged 3 Definitions
to investigate the possibility of applying the most re-
cent editions of the Standards indicated below. For the purposes of this International Standard, the
Members of IEC and ISO maintain registers of cur- definitions given in ISO 1628-1 and the following de-
rently valid International Standards. finition apply.
3.1 viscosity number (of a polymer): The value 5.1.3 m-Cresol, meeting the following specifi-
given by the formula cations:
WARNING - Avoid contact with the skin and 6.2 Balance, accurate to 0,l mg.
inhalation of any vapours of the solvents and
cleaning liquids. 6.3 Volumetric flask, capacity 50 ml, complying
with the requirements of ISO 1042, fitted with a
ground-glass stopper.
5.1 Solvents
64. Shaking apparatus or magnetic stirrer.
5.1.1 Sulfuric acid, 96 % (m/m) + 0,15 % Im/m) sol-
ution. 6.5 Sintered-glass filter, with a pore size between
40 Pm and 100 Pm (grade P IOO), or stainless-steel
For the determination of the concentration of com- sieve, with apertures of about 0,075 mm*.
mercial sulfuric acid (95 % to 97 %) and adjustment
to 96,0 %, see annex A. 6.6 Viscometer, of the suspended-level Ubbelohde
type, complying with the requirements of ISO 3105.
5.1.2 Formic acid, 90 % (m/m) + 0,15 % (m/an) sol- The essential dimensions of the viscometer are
ution. shown in figure 1. For use with the formic acid sol-
ution (5.1.2), the inside diameter of the capillary shall
The solvent shall be stored in a brown glass bottle. Its be 0,58 mm -+ 2 % (complying with the requirements
concentration shall be checked at least evev of size No. 1 of ISO 3105). For use with the sulfuric
2 weeks. lt shall not contain more than 0,2 % acetic acid Solution (5.1 .l) or mcresol (5.1.3), the inside di-
acid or methyl formate. ameter of the capillary shall be 1,03 mm +- 2 %
2
0 ISO ISO 307:1994(E)
(complying with the requirements of size No. 2 of vent to be used, i.e. that it does not form particles of
ISO 3105). w 1.
Other types of viscometer listed in ISO 3105 may be The fraction of polymer modifier and other additives
used, provided that the results are equivalent to those that are insoluble in hydrochloric acid is determined
of the Ubbelohde viscometers specified above. How- from the hydrolysis residue (this method will form the
ever, in cases of dispute, an Ubbelohde viscometer subject of a future International Standard) and the
shall be used. correct amount of Polyamide Sample to be weighed
out is calculated using equation 8.2.
6.7 Thermostatic bath, capable of being main-
NOTE 1 Experience indicates that the usual polymer
tained at 25 “C -+ 0,05 “C. modifiers for polyamides, e.g. ethylene copolymers and EP
rubber, are so finely dispersed in the Solution of the Sample
6.8 Stop-watch, accurate to 0,l s. that the Solution viscosity is practically unaffected, provided
that the Solution is free from gel particles.
Table 1 - Determination of additives in Polyamide samples in Order to be able to calculate the correct
test Portion size
Additives
Property determined Test method Remarks See subclause
determinable
Extractable-matter ISO 6427; ISO 599 Low-molecular-weight Extract Sample before 7.2
content fractions measurement (thus
no correction necess-
Plasticizers at-y to size of test por-
tion)
Stabilizers
Slip agents
Organic flame-
retardants
Ash (no Oxide conver- ISO 3451-4 ISO 307:1994 If necessary, increase
Glass fibres 7.5
sion) https://standards.iteh.ai/catalog/standards/sist/db4de2f9-82fd-4cdb-bf83-
size of test Portion
Silicates
4e15806c3328/iso-307-1994
Inorganic flame-
retardants
8 Calculation of mass of test Portion ww3 is the content of other materials (for
example other polymers such as
polyolefins, or additives, such as flame-
8.1 Polyamides with extractable matter retardants), expressed as a percentage
content not greater than 2,00 % (m/m) by mass, determined by appropriate
methods.
Calculate the mass mc, in milligrams, of the test por-
tion as follows: The corrections for w(%),, Wo and Wo need
250 only be applied if they exceed 0,5 % (dm) each.
mc =
, w(%), + w(%)* + w(%>3
(standards.iteh.ai)
Polyamide depends on the solvent used. After each determination,
with the solvent, then
drain the viscometer, rinse
with water, followed by
Three different solvents are described in this Inter- acetone (5.2.2) and dry as described above.
national Standard: sulfuric acid Solution (5.1.1), formic ISO 307:1994
https://standards.iteh.ai/catalog/standards/sist/db4de2f9-82fd-4cdb-bf83-
acid Solution (5.1.2) and m-cresol (5.1.3). The flow However, if the next Solution to be measured is of a
times of the solvents shall be determined at least 4e15806c3328/iso-307-1994Polyamide of the Same type and of a similar viscosity,
once each day that they are used (see 10.3). If the it is permissible to drain the viscometer, wash it with
flow time of a solvent differs by more than 1 % from the Solution to be measured, and then fill it with this
the initial value at the time of preparation, the solvent Solution.
shall be discarded and fresh solvent prepared.
10.2 Preparation of test Solution
The solvent or solvents to be used for a particular
Polyamide are specified below. Weigh, to the nearest 0,2 mg, a test Portion of
(m, & 5) mg, where m, is the mass calculated in ac-
9.2 For PA 6, PA 66, PA 69, PA 610, PA MXD6 and cordante with clause 8, working rapidly to minimize
corresponding copolyamides, the sulfuric acid or moisture pick-up by the polymer. If the weighing
formic acid Solution shall be used as solvent, unless takes more than 2 min, reject the material and begin
these polyamides contain additives that liberate gases another weighing.
in acidic solvents, in which case m-cresol shall be
used as the solvent. Transfer the test Portion to the 50 ml volumetric flask
(6.3) and add about 40 ml of the solvent selected in
NOTE 4 Graphs for interconversion of the viscosity num- accordance with clause 9. Close the flask and Shake,
bers determined in sulfuric acid and in formic acid as solvent or stir with the magnetic stirrer (6.4), the contents
are presented in figure2. The reliability of the conversion is until the polymer has dissolved. This may take from
discussed in 13.1. approximately 0,5 h to several hours, depending on
the type of Polyamide and the particle size of the test
9.3 For PA 612 and corresponding copolyamides, Portion. When the sulfuric acid or formic acid Solution
the sulfuric acid Solution or m-cresol shall be used as is used as the solvent, the temperature shall not ex-
solvent. ceed 30 “C. When m-cresol is used as the solvent,
the temperature may be raised to 95 “C to 100 “C. If,
NOT ‘E 5 Graph s for interconversion of the v iscosity num- in the latter case, dissolution takes more than 2 h, this
bers deter mined in these two solvents are presented in shall be reported.
ISO 307:1994(E) 0 ISO
When dissolution is complete, cool the Solution to With each polyamide Sample, carry out at least two
approximately 25 “C, dilute to the mark with the sol- determinations of the viscosity number, each time
vent and mix weil. The temperature of the Solution using a fresh solution, until two successive values
during dilution shall lie between 23 “C and 27 “C. If meet the repeatability requirement corresponding to
the magnetic stirrer (6.4) is used, remove it from the the solvent used (see clause 12). Report the mean
Solution before dilution and rinse it with the solvent, of these two values, rounded off to the nearest whole
adding the rinsings to the flask before further dilution. number, as the viscosity number of the Sample.
VN =
Filter the Solution through the sintered-glass filter is the flow time of the Solution;
(6.5) or the metal sieve into tube L of the viscometer is the flow time of the solvent;
(see figure 1). Alternatively, centrifuge the Solution at
a rotational frequency of approximately 50 s-’ and ep is the concentration of the polymer in
pour the clear supernatant liquid into the viscometer grams per millilitre of Solution.
iTeh STANDARD PREVIEW
(6.6). The volume of liquid shall be such that, after
draining, the level lies between the filling marks. NOTE 7 Density differente and kinetic energy cor-
(standards.iteh.ai)
Preferably, the filling should be done with the vis- rections tan be neglected in this method; therefore, in cal-
cometer out of the thermostatic bath (6.7) to avoid culating the viscosity number of the polymer, the ratio of
contamination of the bath in case of accidental Spills. ISO the
307:1994 viscosities of the solution and the solvent (see
clause 3) tan be replaced by the ratio of the corresponding
https://standards.iteh.ai/catalog/standards/sist/db4de2f9-82fd-4cdb-bf83-
times of flow. Furthermore, the concentration of the
Mount the viscometer in the thermostatic bath 4e15806c3328/iso-307-1994
main-
polymer may be expressed as grams per millilitre of solvent
tained at 25 “C k 0,05 “C, ensuring that tube N is instead of grams per millilitre of Solution, without introduc-
vertical and that the upper graduation mark, E, is at ing appreciable error.
least 30 mm below the surface of the liquid in the
bath. Allow at least 15 min for the charged viscometer
to attain the temperature of the bath.
12 Repeatability and reproducibility
Close tube M and blow or draw the liquid into the
upper bulb of tube N using a rubber bulb or similar The repeatability and reproducibility of the determi-
equipment. Close tube N. Open tube M so that the nation of the viscosity number depend on the solvent
liquid drops away from the lower end of the capillary used. The values are given in table2.
tube. Open tube N and measure the flow time, to the
nearest 0,2 s, as the time taken for the bottom of the
meniscus to pass from mark E to mark F. With cloudy
solutions, view the top of the meniscus. Repeat the 13 Interconversion of the viscosity
measurement of the flow time until two successive
values agree within 0,25 %. Take the mean of these
numbers determined in different solvents
two values as the flow time of the Solution. and interconversion of viscosity numbers
determined in 96 % sulfuric acid and
Determine the mean flow time of the solvent in the relative viscosities determined in
Same viscometer and in the same manner as that of
accordance with ASTM D 789
the Solution. Measure the solvent mean flow time
only once for each series of determinations; however,
The relation between the viscosity numbers deter-
measure the time at least once each day the solvent
mined in different solvents was determined in the
is used. If two successive determinations of the sol-
interlaboratory investigation referred to in the note to
vent mean flow time differ more than 0,4 s, clean the
table 2.
viscometer (see 10.1).
0 ISO ISO 307:1994(E)
Table 3 - Interconversion of relative viscosity (RV) and viscosity number (VN) for PA 6 and PA 66 (values
taken from curve in figure4)
RV VN RV VN
(ISO 307) (ISO 307)
(ASTM D 789) (ASTM D 789)
(in 96 % H,SOJ (in 96 % H2S0,)
RV VN
(ISO 307)
(ASTM D 789)
(in 96 % H2S04)
177 260,54
179 261,56
181 262,56
183 263,55
185 264,53
187 265,50
189 266,46
191 267,41
193 268,35
195 269,28
197 270,20
199 271,11
201 272,Ol
203 272,91
205 273,79
207
209
iTeh STANDARD
274,67
275,54
PREVIEW
211 (standards.iteh.ai)
276,40
213 277,25
215 278,09
ISO 307:1994
https://standards.iteh.ai/catalog/standards/sist/db4de2f9-82fd-4cdb-bf83-
217 278,93 4e15806c3328/iso-307-1994
219 279,75
221 280,57
223 281,39
225 282,19
I