FINAL INTERNATIONAL ISO/FDIS

DRAFT
STANDARD 1628-2

ISO/TC 61/SC 9
Secretariat: KATS Plastics — Determination of the
Voting begins on:
viscosity of polymers in dilute solution
2020-02-14 using capillary viscometers —
Voting terminates on:
Part 2: ) EW

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Poly(vinyl chloride) resins

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Plastiques — Détermination de la viscosité des polymères en solution
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diluée à l'aide de viscosimètres à capillaires —

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Partie 2: Résines de poly(chlorure de vinyle)

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IMPORTANT — Please use this updated version dated 2020-01-31, and discard any previous version of
this FDIS. Ballot dates have been modified.

RECIPIENTS OF THIS DRAFT ARE INVITED TO

ISO/CEN PARALLEL PROCESSING
SUBMIT, WITH THEIR COMMENTS, NOTIFICATION
OF ANY RELEVANT PATENT RIGHTS OF WHICH
THEY ARE AWARE AND TO PROVIDE SUPPOR­TING
DOCUMENTATION.
IN ADDITION TO THEIR EVALUATION AS Reference number
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO­
LOGICAL, COMMERCIAL AND USER PURPOSES, ISO/FDIS 1628-2:2020(E)
DRAFT INTERNATIONAL STANDARDS MAY ON
OCCASION HAVE TO BE CONSIDERED IN THE
LIGHT OF THEIR POTENTIAL TO BECOME STAN­
DARDS TO WHICH REFERENCE MAY BE MADE IN
NATIONAL REGULATIONS. © ISO 2020
ISO/FDIS 1628-2:2020(E)


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COPYRIGHT PROTECTED DOCUMENT

© ISO 2020
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
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Published in Switzerland

ii  © ISO 2020 – All rights reserved

 ISO/FDIS 1628-2:2020(E)


Contents Page

Foreword......................................................................................................................................................................................................................................... iv
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references....................................................................................................................................................................................... 1
3 Terms and definitions...................................................................................................................................................................................... 2
4 Principle......................................................................................................................................................................................................................... 2
5 Materials........................................................................................................................................................................................................................ 2
6 Apparatus...................................................................................................................................................................................................................... 2
7 Sampling......................................................................................................................................................................................................................... 3
8 Number of determinations......................................................................................................................................................................... 3
9 Procedure..................................................................................................................................................................................................................... 3
9.1 Preparation of solution..................................................................................................................................................................... 3
9.2 Determination of efflux times..................................................................................................................................................... 3
10 Expression of results......................................................................................................................................................................................... 4
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10.1 Reduced viscosity.................................................................................................................................................................................. 4

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10.2 K-value............................................................................................................................................................................................................ 4

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11 Precision........................................................................................................................................................................................................................ 5
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12 Test report.................................................................................................................................................................................................................... 5
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Bibliography.............................................................................................................................................................................................................................. 15
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ISO/FDIS 1628-2:2020(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. 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.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www​.iso​.org/​directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www​.iso​.org/​patents).
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Any trade name used in this document is information given for the convenience of users and does not

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constitute an endorsement.

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For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
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expressions related to conformity assessment, as well as information about ISO's adherence to the
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World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www​.iso​.org/​
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iso/​foreword​.html.
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This document was prepared by Technical Committee ISO/TC  61, Plastics, Subcommittee SC 9,
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Thermoplastic materials, in collaboration with the European Committee for Standardization (CEN)
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Technical Committee CEN/TC 249, Plastics, in accordance with the Agreement on technical cooperation
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between ISO and CEN (Vienna Agreement).

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This third edition cancels and replaces ISO 1628-2:1998, of which it constitutes a minor revision.
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The change compared to the previous edition is as follows:

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— Clause 2 has been updated.

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A list of all parts in the ISO 1628 series can be found on the ISO website.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www​.iso​.org/​members​.html.

iv  © ISO 2020 – All rights reserved

FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 1628-2:2020(E)

Plastics — Determination of the viscosity of polymers in

dilute solution using capillary viscometers —
Part 2:
Poly(vinyl chloride) resins

1 Scope

1.1 This document specifies conditions for the determination of the reduced viscosity (also known
as viscosity number) and K-value of PVC resins. It is applicable to resins in powder form which consist
of homopolymers of the monomer vinyl chloride and copolymers, terpolymers, etc., of vinyl chloride
with one or more other monomers, but where vinyl chloride is the main constituent. The resins may
contain small amounts of unpolymerized substances (e.g. emulsifying or suspending agents, catalyst
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residues, etc.) and other substances added during the course of the polymerization. This document

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is not applicable, however, to resins having a volatile-matter content in excess of 0,5 % ± 0,1 %, when

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determined in accordance with ISO 1269. In addition to this, it is not applicable to resins which are not
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entirely soluble in cyclohexanone.
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1.2 The reduced viscosity and K-value of a particular resin are related to its molecular mass, but the
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relationship varies depending on the concentration and type(s) of other monomer(s) present. Hence,
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homopolymers and copolymers having the same reduced viscosity or K-value might not have the same
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molecular mass.
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1.3 The values determined for reduced viscosity and K-value, for a particular sample of PVC resin, are
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influenced differently by the concentration of the solution chosen for the determination. Hence the use
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of the procedures described in this document only gives values for reduced viscosity and K-value that are
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comparable when the concentrations of the solutions used are identical.

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Limiting viscosity number is not used for PVC resins.

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1.5 The experimental procedures described in this document can also be used to characterize the
polymeric fraction obtained during the chemical analysis of a PVC composition. However, the values
calculated for the reduced viscosity and K-value in these circumstances might not indicate the actual
values for the resin used to produce the composition because of the impure nature of the recovered
polymer fraction.

2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 1042, Laboratory glassware — One-mark volumetric flasks
ISO 1628-1:2009, Plastics — Determination of the viscosity of polymers in dilute solution using
capillary viscometers — Part 1: General principles
ISO 3105:1994, Glass capillary kinematic viscometers — Specifications and operating instructions

© ISO 2020 – All rights reserved  1

ISO/FDIS 1628-2:2020(E)


3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 1628-1 apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://​w ww​.iso​.org/​obp
— IEC Electropedia: available at http://​w ww​.electropedia​.org/​

4 Principle

4.1 A test portion is dissolved in a solvent. The reduced viscosity and the K-value are calculated from
the efflux times for the solvent and the solution in a capillary tube viscometer.

5 Materials

5.1 Cyclohexanone, having a viscosity/density ratio (kinematic viscosity) between 2,06 × 10−6 m2 s–1
and 2,33 × 10−6 m2 s–1 (2,06 mm2 s–1 and 2,33 mm2 s–1) at 25 °C. The specified boiling point shall be
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155 °C. Store the solvent in the dark in a dark-coloured bottle fitted with a ground-glass stopper. Check

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the kinematic viscosity before use.

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6 Apparatus
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6.1 The apparatus required to carry out viscosity measurements on polymers in dilute solution are in
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accordance with ISO 1628-1:2009, Clause 5. In addition, the following particular items are required for
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the procedures described in this document.

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6.2 Viscometer. From the viscometers described in ISO 1628-1:2009, 5.1, model 1C, with a capillary
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diameter of 0,77 mm ± 2 %, from ISO 3105:1994, Table B.4, shall be used as the reference viscometer.
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Other viscometers described in ISO 1628-1 may be used provided the correlation between the chosen
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viscometer and the reference viscometer has been established over the range of reduced viscosities and
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K-values to be measured, and the results are corrected accordingly.

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6.3 Graduated flask (one-mark volumetric flask), class A, as specified in ISO 1042, with a volume
of 50 ml.
NOTE The use of a flask calibrated at a temperature of 20 °C, as specified in ISO 1042, causes a systematic
error which can, however, be neglected.

6.4 Filter funnel, with fritted-glass filter disc of medium porosity (pore size 40 µm to 50 µm), or glass
funnel with paper filter.

6.5 Mechanical agitator, equipped with a heating device to keep the flask (6.3) and its contents at a
temperature between 80 °C and 85 °C.

As an alternative, a rotary agitator or shaker may be placed in an oven at a temperature between 80 °C
and 85 °C.

6.6 Analytical balance, accurate to 0,1 mg.

6.7 Temperature-regulated bath, capable of being set at 25,0  °C  ±  0,5  °C in steps of 0,1  °C and
maintaining a stability of ± 0,05 °C around the set temperature.

2  © ISO 2020 – All rights reserved

 ISO/FDIS 1628-2:2020(E)


6.8 Thermometer, with a sensitivity of 0,05 °C.

6.9 Time-measuring device, with a sensitivity of 0,1 s.

7 Sampling
Take a sample which is representative of the resin whose properties are to be determined and large
enough for at least two determinations.

8 Number of determinations
Carry out two complete determinations, starting each with a fresh test portion.

9 Procedure

9.1 Preparation of solution

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General requirements for the dissolution of polymer in solvent are given in ISO 1628-1:2009, Clause 6.

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Prepare a solution with a concentration of 5 g/cm3 ± 0,1 g/ cm3 at 25 °C ± 1 °C, as follows.

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Weigh, to the nearest 0,2  mg, 0,250  g  ±  0,005  g of resin and transfer it quantitatively to the 50  ml
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flask (6.3). Add about 40 ml of cyclohexanone (5.1) to the flask, swirling the flask by hand to prevent
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coagulation or the formation of lumps. Continue dissolution by agitating for 1  h between 80  °C and
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85 °C using the agitator (6.5). Check visually that dissolution is complete. If gelatinized particles are
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still visible, start again with a new portion of the resin. Cool the solution to 25 °C ± 1 °C and make up to
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the mark with cyclohexanone at the same temperature. Mix the solution thoroughly by shaking.
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Determine the actual concentration of the solution to an accuracy of ± 0,1 %.

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If a mass of 0,250 g ± 0,000 25 g is taken and made up to 50 ml of solution as described above, Table 1
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can be used to read off the reduced viscosity and K-value from the ratio of the efflux time of the solution
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to that of the solvent (the so-called viscosity ratio).

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Alternative methods for the preparation of the solution may be used, for example the addition of a
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measured volume of solvent to a measured mass of test portion, provided that the values obtained for
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the reduced viscosity and K-value can be shown to be equivalent to those obtained with the method
of solution preparation described above. Such alternative methods of solution preparation requires
the amounts of solvent and test portion taken to be determined by experiment, and can also require
compensation for loss of solvent by evaporation during the dissolution process.
With resins having K-values greater than 85, the ratio of the efflux time of the solution to that of
the solvent will exceed the maximum value of 2,0, which is contrary to the requirement specified in
ISO  1628-1:2009, 6.2. In order to ensure uniformity of testing for PVC, this non-conformity shall be
ignored, and all currently available resins tested using the same test-portion mass.

9.2 Determination of efflux times

The procedure is described in ISO 1628-1:2009, Clause 8.
The temperature of the thermostat (6.7) shall be set such that the actual temperature which is measured
by the thermometer (6.8) lies in the range 25 °C ± 0,5 °C. The measured temperature shall be stable to
−0,05 °C around the temperature at which the thermostat has been set.
When filling the viscometer, filter the solvent and the solution using a filter funnel or a glass funnel and
paper filter (see 6.4).

© ISO 2020 – All rights reserved  3

ISO/FDIS 1628-2:2020(E)


Particular care shall be taken over viscometer cleaning, which shall be based on the procedure described
in ISO 1628-1:2009, Annex A. Efflux times with the control solvent cyclohexanone shall remain constant
to within 0,2 s for a given viscometer. With the solution, repeat the measurement of the efflux time until
two successive measurements differ by less than 0,25 %. Always discard the first efflux time reading.
NOTE This is a manual procedure. Proprietary equipment is available which will organize the charging of
the viscometer with solution and solvent and measure the respective efflux times automatically. The use of such
equipment is included in the scope of this document provided that all the procedures and verification checks
described above are followed by the automated procedure.

10 Expression of results

10.1 Reduced viscosity

Calculate the reduced viscosity, I, for each test portion as specified in ISO 1628:2009, Clause 9, using
Formula (1):
t − t0
I= (1)
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  t and t0 are the efflux times, in seconds, of the solution and solvent, respectively;
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  is the concentration of the solution, in 103 kg/m3, i.e. g/cm3.

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Calculate the reduced viscosity I for the sample as the mean value of the two individual values obtained
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in the two determinations, expressing the result to the nearest whole number. If the I values obtained
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in the two determinations deviate by more than ± 0,4 % from the mean value, these results shall be
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rejected and further determinations carried out with fresh test portions.
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If the solution concentration is 5 g/cm3 ± 0,005 g/cm3, it is more convenient to read off the values of I
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from Table 1, expressing I in (m3/kg) · 10−3, i.e. cm3/g, rounded to the first place of decimals.
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10.2 K-value
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For each test portion, calculate the K-value as specified in ISO 1628-1:2009, Clause 9, using Formula (2):

1 , 5 lgηr −1 + 1 +  + 2 + 1 , 5 lgηr  1 , 5 lgηr

2
K= c  ×1 000 (2)
150 + 300c
where

  η t
ηr = = is the ratio of the viscosities (efflux times) of the solution and solvent;
η0 t0
  t and t0 are the efflux times, in seconds, of the solution and solvent, respectively;

  c is the concentration of the solution, in 103 kg/m3, i.e. g/cm3.

Calculate the K-value for the sample as the mean value of the two individual K-values obtained in the
two determinations, expressing the result to the first place of decimals. If the K-values obtained in the
two determinations deviate by more than ± 0,4 % from the mean value, these results shall be rejected
and further determinations carried out with fresh test portions.
If the solution concentration is 5 g/cm3 ± 0,005 g/cm3, it is more convenient to read off the K-value from
Table 1, rounding to the second place of decimals.

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 ISO/FDIS 1628-2:2020(E)


11 Precision
Interlaboratory trials were conducted on three resins in 11 laboratories on four different dates. These
interlaboratory trials gave the following results for the repeatability standard deviation sr (within the
same laboratory) and the reproducibility standard deviation sR (among different laboratories):

Table 1 — Results for sr, sR of K-value and reduced viscosity

  K-value Reduced viscosity
Approximately Approximately Approximately Approximately Approximately Approximately
50 70 90 61 124 227
sr 0,132 0,115 0,120 0,313 0,458 0,742
sR 0,420 0,291 0,495 0,984 1,202 3,042

12 Test report
The test report shall include the following information:
a) a reference to this document, i.e. ISO 1628-2:2020;
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b) all details necessary for complete identification of the material under test;
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c) the reduced viscosity and/or K-value of the resin sample;
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d) any difference between the type of viscometer used and the reference viscometer specified in this
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document;
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e) the date of the test.

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See Table 2.
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ISO/FDIS 1628-2:2020(E)


Table 2 — Conversion of viscosity ratio (VR) to reduced viscosity (I) and K-value
Unit for reduced viscosity: (m3/kg) × 10−3, i.e. cm3/g
Concentration of resin in solution = 5 g/cm3
VR I K VR I K VR I K
1,195 39,0 39,74 1,237 47,4 44,02 1,279 55,8 47,87
1,196 39,2 39,85 1,238 47,6 44,12 1,280 56,0 47,95
1,197 39,4 39,95 1,239 47,8 44,22 1,281 56,2 48,04
1,198 39,6 40,06 1,240 48,0 44,31 1,282 56,4 48,13
1,199 39,8 40,17 1,241 48,2 44,41 1,283 56,6 48,21
1,200 40,0 40,27 1,242 48,4 44,50 1,284 56,8 48,30
1,201 40,2 40,38 1,243 48,6 44,60 1,285 57,0 48,38
1,202 40,4 40,49 1,244 48,8 44,69 1,286 57,2 48,47
1,203 40,6 40,59 1,245 49,0 44,79 1,287 57,4 48,55
1,204 40,8 40,70 1,246 49,2 44,88 1,288 57,6 48,64
1,205 41,0 40,80 1,247 49,4 44,98 1,289 57,8 48,72
1,206 41,2 40,91 1,248 49,6 45,07 1,290 58,0 48,81
1,207 41,4 41,01 1,249 49,8 45,16 1,291 58,2 48,89
1,208 41,6 41,12 1,250 50,0 45,26 1,292 58,4 48,98
1,209 41,8 41,22 1,251 50,2 45,35 1,293 58,6 49,06
1,210 42,0 41,33 1,252 50,4 45,44 1,294 58,8 49,15
1,211 42,2 41,43 1,253 50,6 ) EW
45,53 1,295 59,0 49,23

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1,212 42,4 41,53 1,254 50,8 45,63 1,296 59,2 49,32
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1,213 42,6 41,64 1,255 51,0 45,72 1,297 59,4 49,40
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1,214 42,8 41,74 1,256 51,2 45,81 1,298 59,6 49,48
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1,215 43,0 41,84 1,257 51,4 45,90

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1,216 43,2 41,94 1,258 51,6 45,99 1,300 60,0 49,65

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1,217 43,4 42,05 1,259 51,8 46,09 1,301 60,2 49,73

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1,218 43,6 42,15 1,260 52,0 46,18 1,302 60,4 49,81

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1,219 43,8 42,25 1,261 52,2 46,27 1,303 60,6 49,90

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1,220 44,0 42,35 1,262 52,4 46,36 1,304 60,8 49,98

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1,221 44,2 42,45 1,263 52,6 46,45 1,305 61,0 50,06

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1,222 44,4 42,55 1,264 52,8 46,54 1,306 61,2 50,14

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1,223 44,6 42,65 1,265 53,0 46,63 1,307 61,4 50,23

d2 s.

1,224 44,8 42,75 1,266 53,2 46,72 1,308 61,6 50,31

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1,225 45,0 42,85 1,267 53,4 46,81 1,309 61,8 50,39

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1,226 45,2 42,95 1,268 53,6 46,90 1,310 62,0 50,47

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1,227 45,4 43,05 1,269 53,8 46,99 1,311 62,2 50,55

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1,228 45,6 43,15 1,270 54,0 47,07 1,312 62,4 50,63

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1,229 45,8 43,25 1,271 54,2 47,16 1,313 62,6 50,71

1,230 46,0 43,34 1,272 54,4 47,25 1,314 62,8 50,79
1,231 46,2 43,44 1,273 54,6 47,34 1,315 63,0 50,87
1,232 46,4 43,54 1,274 54,8 47,43 1,316 63,2 50,95
1,233 46,6 43,64 1,275 55,0 47,52 1,317 63,4 51,03
1,234 46,8 43,73 1,276 55,2 47,60 1,318 63,6 51,11
1,235 47,0 43,83 1,277 55,4 47,69 1,319 63,8 51,19
1,236 47,2 43,93 1,278 55,6 47,78 1,320 64,0 51,27

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