IEC 60450:2004+AMD1:2007 CSV
(Main)Measurement of the average viscometric degree of polymerization of new and aged cellulosic electrically insulating materials
Measurement of the average viscometric degree of polymerization of new and aged cellulosic electrically insulating materials
Describes a standardized method for the determination of the average viscometric degree of polymerization (DPv) of new and aged cellulosic electrically insulating materials. It may be applied to all cellulosic insulating materials such as those used in transformer, cable or capacitor manufacturing. The methods described can also be used for the determination of the intrinsic viscosity of solutions of chemically modified kraft papers, provided that these dissolve completely in the selected solvent. Caution should be taken if the method is applied to loaded kraft papers. Note: Within a sample of material, all the cellulose molecules do not have the same degree of polymerization so that the mean value measured by viscometric methods is not necessarily the same as that which may be obtained by, for instance, osmotic or ultra centrifuging methods. Experience has indicated the need for improved description of the experimental method. It describes a revised procedure that overcomes the limitations of the first edition. This consolidated version consists of the second edition (2004), and its amendment 1 (2007). Therefore, no need to order amendment in addition to this publication.
Mesure du degré de polymérisation moyen viscosimétrique des matériaux isolants cellulosiques neufs et vieillis à usage électrique
Décrit une méthode normalisée pour déterminer le degré de polymérisation moyen viscosimétrique (DPv) des matériaux isolants cellulosiques neufs et vieillis, à usage électrique. Elle peut s'appliquer à tous les matériaux isolants cellulosiques comme ceux utilisés dans la fabrication des transformateurs, des câbles et des condensateurs. Les méthodes décrites peuvent également être utilisées pour déterminer la viscosité intrinsèque des solutions de papiers kraft modifiés chimiquement, pourvu que ceux-ci se dissolvent totalement dans le solvant choisi. Il convient de prendre des précautions si la méthode s'applique à des papiers kraft chargés. Note: Dans un échantillon de matériau, toutes les molécules de cellulose n'ont pas le même degré de polymérisation de sorte que la valeur moyenne mesurée par les méthodes viscosimétriques n'est pas nécessairement la même que celle obtenue, par exemple, par les méthodes par osmose ou par ultra-centrifugation. L'expérience a mis en évidence le besoin d'améliorer la description de la méthode expérimentale. La procédure ainsi revue permet de surmonter les limitations de la première édition. Cette version consolidée comprend la deuxième édition (2004), et son amendement 1 (2007). Il n'est donc pas nécessaire de commander l'amendement avec cette publication.
General Information
Standards Content (Sample)
IEC 60450
Edition 2.1 2007-07
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
Measurement of the average viscometric degree of polymerization of new and
aged cellulosic electrically insulating materials
Mesure du degré de polymérisation moyen viscosimétrique des matériaux
isolants cellulosiques neufs et vieillis à usage électrique
IEC 60450:2004+A1:2007
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IEC 60450
Edition 2.1 2007-07
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
Measurement of the average viscometric degree of polymerization of new and
aged cellulosic electrically insulating materials
Mesure du degré de polymérisation moyen viscosimétrique des matériaux
isolants cellulosiques neufs et vieillis à usage électrique
INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
COMMISSION
ELECTROTECHNIQUE
PRICE CODE
INTERNATIONALE
CH
CODE PRIX
ICS 17.220.99; 29.035.01 ISBN 2-8318-9234-1
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– 2 – 60450 © IEC:2004+A1:2007
CONTENTS
FOREWORD.3
INTRODUCTION.5
1 Scope.6
2 Normative references .6
3 Terms, definitions and symbols .6
3.1 Terms and definitions .6
3.2 Symbols .7
4 Principle .8
5 Apparatus and reagents .8
6 Specimens .9
6.1 Preparation of specimens .9
7 Experimental procedure.10
7.1 Measurement of water content of paper.10
7.2 Determination of viscosity .10
8 Test report.16
Annex A (normative) Cuen solution.17
Annex B (normative) Preparation of Cuen solution.18
c
En
Annex C (normative) Procedure for the verification of the ratio
c
Cu
of the Cuen solution.21
.
Annex D (informative) Numerical values of the product [ν] c as a function of ν
s
according to Martin's formula .22
Bibliography.23
Table 1 – Symbols .7
Table 2 – DP values of specimen .10
v
.
Table D.1 – [ν] c as a function of ν (k = 0,14).22
s
Figure 1 – Chemical structure of cellulose .6
Figure 2 – Ubbelohde viscometer tube.14
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60450 © IEC:2004+A1:2007 – 3 –
INTERNATIONAL ELECTROTECHNICAL COMMISSION
–––––––––––
MEASUREMENT OF THE AVERAGE VISCOMETRIC DEGREE OF
POLYMERIZATION OF NEW AND AGED CELLULOSIC ELECTRICALLY
INSULATING MATERIALS
FOREWORD
1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising
all national electrotechnical committees (IEC National Committees). The object of IEC is to promote
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patent rights. IEC shall not be held responsible for identifying any or all such patent rights.
International Standard IEC 60450 has been prepared by subcommittee 15E: Methods of test,
of IEC technical committee 15: Insulating materials.
This second edition cancels and replaces the first edition, published in 1974, and constitutes
a technical revision. Experience has indicated the need for improved description of the ex-
perimental method. It describes a revised procedure that overcomes the limitations of the first
edition.
This consolidated version of IEC 60450 consists of the second edition (2004) [documents
15E/229/FDIS and 15E/235/RVD] and its amendment 1 (2007) [documents 112/49/CDV and
112/66/RVC].
The technical content is therefore identical to the base edition and its amendment(s) and has
been prepared for user convenience.
It bears the edition number 2.1.
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– 4 – 60450 © IEC:2004+A1:2007
A vertical line in the margin shows where the base publication has been modified by
amendment 1.
This publication has been drafted in accordance with the ISO/IEC Directives, Part 3.
The committee has decided that the contents of the base publication and its amendments will
remain unchanged until the maintenance result date indicated on the IEC web site under
"http://webstore.iec.ch" in the data related to the specific publication. At this date,
the publication will be
• reconfirmed,
• withdrawn,
• replaced by a revised edition, or
• amended.
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60450 © IEC:2004+A1:2007 – 5 –
INTRODUCTION
Experience has indicated the need for an improved description of the experimental method for
the reproducible determination of the average viscometric degree of polymerization of new
and aged cellulosic electrically insulating material.
The major error appears to arise from oxidative degradation occurring during processing and
effluxing. Other significant factors include the need to ensure that all of the material is
dissolved and used, as well as the effect of the speed of effluxing.
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– 6 – 60450 © IEC:2004+A1:2007
MEASUREMENT OF THE AVERAGE VISCOMETRIC DEGREE OF
POLYMERIZATION OF NEW AND AGED CELLULOSIC ELECTRICALLY
INSULATING MATERIALS
1 Scope
This International standard describes a standardized method for the determination of the
average viscometric degree of polymerization ( DP ) of new and aged cellulosic electrically
ν
insulating materials. It may be applied to all cellulosic insulating materials such as those used
in transformer, cable or capacitor manufacturing.
The methods described can also be used for the determination of the intrinsic viscosity of
solutions of chemically modified kraft papers, provided that these dissolve completely in the
selected solvent.
Caution should be taken if the method is applied to loaded kraft papers.
NOTE Within a sample of material, all the cellulose molecules do not have the same degree of polymerization so
that the mean value measured by viscometric methods is not necessarily the same as that which may be obtained
by, for instance, osmotic or ultra centrifuging methods.
2 Normative references
The following referenced documents are indispensable for the application 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.
IEC 60814, Insulating liquids – Oil-impregnated paper and pressboard – Determination of
water by automatic coulometric Karl Fischer titration
ISO 287, Paper and board – Determination of moisture content – Oven-drying method
ISO 3105, Glass capillary kinematic viscometers – Specifications and operating instructions
3 Terms, definitions and symbols
For the purposes of this document, the following terms, definitions and symbols apply.
3.1 Terms and definitions
3.1.1
degree of polymerization of a cellulose molecule
number of anhydrous-β-glucose monomers, C H O , in the cellulose molecule
6 10 5
NOTE Figure 1 shows the chemical structure of cellulose.
CH OH
CH OH
2
2
OH
O O
HO
HO
O
O
HO
HO OH
O
OH
OH
CH OH
2
n – 2
IEC 424/04
Figure 1 – Chemical structure of cellulose
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60450 © IEC:2004+A1:2007 – 7 –
3.1.2
Cuen
1 mol/l aqueous solution of bis(ethylenediamine)copper(II) hydroxide
1
Cu(H NCH CH NH ) (OH) . [CAS 14552-35-3]
2 2 2 2 2 2
NOTE In some countries the abbreviation CED is used for bis(ethylenediamine)copper(II) hydroxide.
3.1.3
paper
cellulosic electrically insulating material, such as paper, presspaper, pressboard and
components made thereof
NOTE In the present document such paper is termed “paper”.
3.2 Symbols
Symbols used in this standard are shown in Table 1.
Table 1 – Symbols
Symbol Definition
Mark Houwink constant of the cellulose monomer
α
c Molarity of copper in Cuen solution
Cu
Molarity of ethylenediamine in Cuen solution
c
En
Constants for viscometer tubes 0, 1 and 2 respectively
C , C and C
0 1 2
c Concentration of solution
Average viscometric degree of polymerization
DP
ν
Kinematic viscosity of solution
ν
v Kinematic viscosity of solvent
0
K Mark Houwink characteristic constant of the polymer/solvent system
k Constant in Martin's formula
m Mass of dry paper
D
Mass of swollen paper in tared vessel
m
T
Mass of added water
m
H O
2
Density of water
ρ
H O
2
v Volume of added water
H O
2
Volume of added Cuen
v
Cu
Intrinsic viscosity
[ν]
v Specific viscosity
s
t t Efflux time for tests A and B on dissolved specimen 1
,
1A 1B
t t Efflux time for tests A and B on dissolved specimen 2
,
2A 2B
Efflux time for tests A and B on pure solvent
t t
,
0A 0B
Efflux time for diluted Cuen solvent (50 % Cuen and 50 % water)
t
0
t Efflux time for Cuen dissolved specimen
S
———————
1
Chemical Abstracts Service (CAS) Registry numbers®
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4 Principle
The specific viscosity ν of a solution of the paper in Cuen is determined. From this result the
s
intrinsic viscosity [ν] of the solution is deduced, and from this the degree of polymerization is
calculated.
NOTE Solutions of cellulose are non-Newtonian fluids. Their viscosity decreases as the flow velocity increases
(sometimes known as “structural viscosity”). Although the viscosity of dilute solutions varies only slightly with the
gradient of the velocity modulus, the use of conditions outside those specified in this standard may result in
unacceptable errors.
Specific viscosity ν is defined by
s
viscosity of paper solution − viscosity of solvent
v = (1)
s
viscosity of solvent
Intrinsic viscosity [ν] is defined by
⎡ν ⎤
s
ν =lim (2)
⎢ ⎥
c→0 c
⎣ ⎦
where c is the concentration of the solution.
The average viscometric degree of polymerization DP (the ratio of the mean molecular mass
ν
indicated viscometrically to the molecular mass of the monomeric unit) is related to the
intrinsic viscosity [ν] by the equation:
α
[ (v] = K ⋅ DP 3)
ν
K and α being characteristic Mark Houwink coefficients of the polymer-solvent system
(paper/Cuen) and of the monomer respectively.
v
The intrinsic viscosity [ν] is calculated from the specific viscosity and the concentration c
s
by Martin’s empirical formula:
k[v]⋅c
v = [ν ] ⋅ c ⋅10 (4)
s
where k is Martin’s constant. For kraft papers k = 0,14.
5 Apparatus and reagents
NOTE 1 Apparatus and reagents for the preparation of Cuen are given separately in Annexes A and B.
During the analysis, unless otherwise specified, use only reagents of recognized analytical
grade and only distilled /de-ionized water or equivalent quality.
A glass fronted, thermostatically controlled bath, suitable for the immersion of the viscometer
tubes, capable of maintaining a temperature of 20 °C to within ±0,1 K and fitted with
appropriate means for illuminating the tubes. It shall be fitted with a means of displaying the
temperature to within an accuracy of ±0,05 K.
NOTE 2 To obtain the required degree of temperature stability, it may be necessary to use a refrigeration unit in
addition to the bath heater.
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60450 © IEC:2004+A1:2007 – 9 –
Calibrated capillary type viscometer tubes according to ISO 3105 with a capillary constant of
0,005 or 0,01. Non calibrated tubes can be used as long as the viscosities of the Cuen solvent
and solution of paper in Cuen are measured in the same tube.
A timer/stopwatch capable of measuring to within an accuracy of ±0,1 s.
Suitable blender or grinder to “activate” the paper sample to allow dissolution.
Suitable vials (typically 25 ml to 50 ml) with lids (not paper) that make an effective seal for the
preparation of paper/Cuen solution. Alternative glass containers can be used. However, these
shall be sealed during dissolution to minimize oxidative degradation of the Cuen.
Cuen (see Annex A).
Distilled or de-ionized water.
Low oxygen content nitrogen supply (minimum 99,9 % nitrogen).
Acetone minimum 99,0 % pure.
Pentane or hexane minimum 99,0 % .
20 % aqueous nitric acid.
Vented drying oven thermostatically controlled to 105 °C ± 2 K.
Analytical balance capable of weighing 20 g to within ±0,1 mg.
Soxhlet extractor.
Pipette to deliver ±0,1 ml.
Mechanical shaker capable of holding the glass vials used to prepare the paper/Cuen
solutions or a magnetic stirrer can be used to dissolve the paper/Cuen solution.
6 Specimens
6.1 Preparation of specimens
The paper under evaluation shall only be handled with gloves or forceps. It shall not be
touched by hand.
Pressboard with a thickness greater than 1 mm, shall be split into layers of less than 1 mm.
The samples shall be cut into pieces sufficiently small to facilitate the subsequent processes.
For very thin paper, the material may be cut into small pieces using scissors.
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6.1.1 Impregnated papers
Impregnated papers shall be degreased before weighing and absorbing solution.
Wash a sufficient amount of the paper under evaluation so as to give a degreased mass of
approximately 3 g in a Soxhlet using pentane or hexane for a minimum of five washings, or by
rinsing in five portions of fresh pentane or hexane in an appropriate glass vessel. Allow the
degreased material to dry and leave it exposed to the atmosphere until equilibrium with the
atmospheric humidity is reached. Two portions of the paper are separated, one for use in the
DP determination and one for use in the moisture determination.
ν
6.1.2 Non-impregnated papers
Take a sample having an approximate mass of 3 g and continue with the test procedures. Two
portions of the paper are separated, one for use in the DP determination and one for use in
ν
the moisture determination.
7 Experimental procedure
7.1 Measurement of water content of paper
Measure the water content according to ISO 287 or IEC 60814.
The water content shall be measured at the same time as the Cuen/paper solution is
prepared.
7.2 Determination of viscosity
7.2.1 Number of test specimens
One specimen shall be used in a preliminary experiment to obtain data on which to base a
valid test.
One specimen shall be used for each valid test, unless otherwise specified. If [ν] ⋅ c of the
preliminary experiment is outside of the range 0,5 to 1,5, two test specimens shall be used.
7.2.2 Concentration of the solution
The concentration of the solution to be used is dependent upon the expected DP value as
ν
given in the following table.
Table 2 – DP values of specimen
v
Specimen condition Approximate resulting
Expected DP
v
concentration
g/dl or %
New 1 000 to 2 000 0,05 to 0,15
Good 650 to 1 000 0,08 to 0,25
Average 350 to 650 0,15 to 0,45
Aged < 350 0,25 to 0,80
NOTE The purpose of this operation is to achieve a fixed value of the product’s intrinsic viscosity and
concentration which is in the range 0,5 ≤ [ν]⋅c ≤ 1,5 . The higher the product of [ν]⋅c the more accurate its
precision.
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60450 © IEC:2004+A1:2007 – 11 –
7.2.3 Fibre separation
The cellulose fibres need to be separated in order to facilitate dissolution in Cuen. Two
techniques are described as follows.
7.2.3.1 Dry fluffing
Fluff the material in a suitable blender or grinder. Ensure enough sample remains after fluffing
as some sample may be lost during the process. The temperature rise during fluffing must not
cause any detrimental effect to the specimen.
The fluffed sample is left to acclimatize with the atmospheric humidity before determining the
water content.
Weigh the necessary amount of sample to the nearest 0,1 mg according to Table 2 and place
it in a suitable vessel for dissolution. Calculate the mass of dry paper as m .
D
Add water and allow the fibres to disperse.
7.2.3.2 Wet mulching
Weigh the necessary amount of sample to the nearest 0,1 mg and place in the blender cup
with sufficient distilled/de-ionized water to cover it. Mulch the paper by operating the blender
at approximately 18 000 r/min for about 30 s or until the fibres are well separated. After
mulching, remove the excess water by either centrifuging or using a Grade 3 sintered glass
filter.
Place the swollen paper in a tared vial and weigh it to within ±0,1 mg (m ). Calculate the total
T
mass of water (i.e. original mass of water plus the mass of water remaining after mulching) by
subtracting the dry paper mass (m ) and the tare mass from m .
D T
Calculate the quantity of water required to make the total water content up to 10,000 g.
Selecting this amount to within ±0,5 mg, use a sufficient amount of this water to rinse any
residual paper out of the centrifuge/filter into the vial and then place the remainder of the
water into the vial. Alternatively, make up to 10,000 g, then weigh to within ±0,5 mg and
calculate the concentration.
7.2.4 Dissolution of specimen
Before use, the Cuen solution sample shall be inspected, refurbished and verified as follows:
• ensure that the solution contains no precipitate by filtering or decanting;
c
En
• using the method described in Annex C, verify that the ratio = 2,0 ± 0,1
c
Cu
• in the event of non-conformance, reject the solution and prepare a new sample.
Transfer into the same vial the same volume (±0,1 ml, using a pipette) of Cuen as the quantity
of water already added to the cellulose fibres.
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If there is some contact between the solution and the atmospheric air in the vial, flush the vial
with nitrogen and shake by hand to ensure good mixing of the components. Flush the vial
again with nitrogen and seal it to ensure a low oxygen environment. Preferably the vial should
be flushed with nitrogen throughout the whole time of dissolution.
NOTE 1 The solution is placed in a nitrogen environment and sealed in the vial because the alkaline solvent is
susceptible to oxidative degradation.
Mechanically shake or stir the specimen until dissolution is complete.
NOTE 2 The time taken is dependent upon the type of paper and the extent of degradation.
a) For heavily aged papers ( DPν < 350) a shaking time of 1h to 2 h is usually adequate.
b) For most papers ( DP > 350) shaking for a period of 16 h (overnight) usually ensures
ν
complete dissolution.
c) Some types of new or nearly new papers do not dissolve easily at room temperature. The
dissolution rate may be increased by using a magnetic stirrer to stir the specimen at 4 °C,
in a refrigerator overnight. The use of a few glass balls can also aid the dispersion of the
cellulose fibres.
When testing heavily degraded papers ( DP < 150) they should be tested immediately after
ν
dissolution.
7.2.5 Determination of the viscosity
7.2.5.1 Selection and filling of the viscometer tube
Select a viscometer tube and support it in a constant temperature bath at 20 °C ± 0,1 K.
Ensure that the viscometer tube is dry, dust free and flushed thoroughly with nitrogen.
Fill the viscometer according to the manufacturer’s instructions. Figure 2 gives an example of
a viscometer.
During the filling and the following measurement procedure, visually observe the solution to
determine the presence of any undissolved matter. In the event of finding undissolved matter,
reject the solution and repeat the experiment.
Wait for 5 min to 10 min before the first measurement of the viscosity, until the solution has
reached its temperature equilibrium.
7.2.5.2 Measurement procedure
An Ubbelohde viscometer is used as an example (see Figure 2). For other viscometers, see
ISO 3105 as well as the manufacturer’s instructions.
Seal the ventilation tube (1) with a finger, a stopper or with plastic film and apply a vacuum to
the capillary tube (2) until the lower reservoir ( 10), the working capillary (6), the timing bulb
( 5), and the upper reservoir ( 4) are filled.
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60450 © IEC:2004+A1:2007 – 13 –
Remove the vacuum and seal.
Ensure that the liquid separates at the lower end of the capillary.
Measure and record the time interval (t , efflux time) with an accuracy of ±0,5 s for the upper
1A
meniscus to travel between the two timing marks M and M on the timing bulb ( 5) .
1 2
Repeat the measurement on the same specimen and record as t . Record the percentage
1B
difference between the two results.
Inspect the results to assess whether the efflux time is within the allowa
...
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