Adhesives - Animal glues - Methods of sampling and testing (ISO 9665:1998)

Klebstoffe - Tierleime - Verfahren für Probenahme und Prüfung (ISO 9665:1998)

Diese Internationale Norm legt Verfahren zur Probenahme und Prüfung von Knochen- und Hautleimen in Pulver-, Granulat-, Perl- oder Würfelform fest. ANMERKUNG 1: Diese Verfahren lassen sich bei geeigneter Umrechnung des entsprechenden Leimtrockengehalts auch bei Tierleimen anderer Form anwenden. Zur Präzision der in dieser Internationalen Norm beschriebenen Prüfverfahren sind gegenwärtig keine Aussagen möglich, da Ergebnisse mit Beteiligung mehrerer Laboratorien nicht vorliegen. Wenn derartige Ergebnisse
verfügbar sind, werden bei der nächsten Überprüfung dieser Norm Angaben zur Präzision in die entsprechenden Prüfverfahren aufgenommen. ANMERKUNG 2: Einzelheiten zur Angabe der Präzision sind ISO 5725-1 : 1994 "Accuracy (trueness and
precision) of measurement methods and results - Part 1: General principles and definitions" zu entnehmen.

Adhésifs - Colles d'origine animale - Méthodes d'échantillonnage et d'essai (ISO 9665:1998)

La présente Norme internationale prescrit des méthodes applicables à l'échantillonnage et à l'essai des colles à base d'os et de peau se présentant sous forme de poudres, granulés, de perles ou de cubes.  
NOTE 1 Ces méthodes peuvent être étendues pour tester d'autres formes de colles animales avec un calcul adéquat de la teneur en colle sèche équivalente.  La fidélité de méthodes d'essai ci-après n'est pas connue parce que des données interlaboratoires ne sont pas disponibles. Lorsque des données interlaboratoires seront obtenues, des déclarations de la fidélité seront ajoutées aux méthodes d'essai correspondantes lors de la prochaine révision.  
NOTE 2 Au sujet de la fidélité, il convient de se référer à l'ISO 5725-1:1994, Exactitude (justesse et fidélité) des résultats et méthodes de mesure - Partie 1: Principes généraux et définitions.

Lepila - Lepila živalskega izvora - Metode vzorčenja in preskušanja (ISO 9665:1998)

General Information

Status
Published
Publication Date
18-Jul-2000
Current Stage
9093 - Decision to confirm - Review Enquiry
Completion Date
22-Jan-2007

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SLOVENSKI STANDARD
SIST EN ISO 9665:2001
01-junij-2001
1DGRPHãþD
SIST EN ISO 9665:1998

/HSLOD/HSLODåLYDOVNHJDL]YRUD0HWRGHY]RUþHQMDLQSUHVNXãDQMD ,62

Adhesives - Animal glues - Methods of sampling and testing (ISO 9665:1998)
Klebstoffe - Tierleime - Verfahren für Probenahme und Prüfung (ISO 9665:1998)
Adhésifs - Colles d'origine animale - Méthodes d'échantillonnage et d'essai (ISO
9665:1998)
Ta slovenski standard je istoveten z: EN ISO 9665:2000
ICS:
83.180 Lepila Adhesives
SIST EN ISO 9665:2001 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 9665:2001
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SIST EN ISO 9665:2001
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SIST EN ISO 9665:2001
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SIST EN ISO 9665:2001
INTERNATIONAL ISO
STANDARD 9665
Second edition
1998-09-15
Adhesives — Animal glues — Methods
of sampling and testing
Adhésifs — Colles d’origine animale — Méthodes d’échantillonnage
et d’essai
Reference number
ISO 9665:1998(E)
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SIST EN ISO 9665:2001
ISO 9665:1998(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.
Draft International Standards adopted by the technical committees are
circulated to the member bodies for voting. Publication as an International
Standard requires approval by at least 75 % of the member bodies casting
a vote.
International Standard ISO 9665 was prepared by Technical Committee
ISO/TC 61, Plastics, Subcommittee SC 11, Products.
This second edition cancels and replaces the first edition (ISO 9665:1993),
annex A of which has been updated.
Annex A of this International Standard is for information only.
© ISO 1998

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced

or utilized in any form or by any means, electronic or mechanical, including photocopying and

microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case postale 56 • CH-1211 Genève 20 • Switzerland
Internet iso@iso.ch
Printed in Switzerland
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SIST EN ISO 9665:2001
ISO ISO 9665:1998(E)
Introduction
The physical and chemical properties of animal glue depend firstly on the
nature of the raw material and secondly on the methods of processing. It is
not possible to develop any simple tests that will evaluate completely the

quality of a glue, or its suitability for a particular use. If, however, the glue is

made from a specific type of raw material by a usual method of
manufacture, then the following tests provide indications of the behaviour
of the glue in use, and may be taken as reliable criteria of quality.
Amongst these properties, the gel strength or viscosity, or both, are usually
included as general indices of quality. The foam test is of interest when the
glue is to be applied by special machines. Many of the physical tests (e.g.
gel strength, water absorption, foam) are of an empirical character, but if
the methods are carefully followed consistent results are obtainable which
will provide useful information both to the manufacturer and user.
Small samples of glue rapidly change their moisture content in response to
changes in atmospheric humidity. It is essential to keep the moisture
content of samples unchanged after they are taken. The use of sealed
waterproof storage containers is recommended for this purpose.
If a consignment undergoes long delays in transit, the average moisture
content may change between the times of sampling by producer and
consumer. To avoid this problem causing unnecessary disputes, it is
recommended that, when gel strengths or viscosities are reported, the
results of moisture content tests should also be given, if an accurate
comparison is required. Although the remaining tests listed in table 1 may
also be slightly affected by changes in moisture content, the differences
are not significant and it is not necessary to report moisture contents for
them.
iii
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SIST EN ISO 9665:2001
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SIST EN ISO 9665:2001
INTERNATIONAL STANDARD ISO ISO 9665:1998(E)
Adhesives — Animal glues — Methods of sampling and
testing
1 Scope

This International Standard specifies the methods to be used for sampling and testing bone and skin glues in the

form of powder, granules, pearls or cubes.

NOTE 1 The methods may be extended to the testing of other forms of animal glues by suitable calculation of the equivalent

dry glue content.

The precision of the test methods included in this International Standard is not known because interlaboratory data

are not available. When interlaboratory data are obtained, precision statements will be added to the corresponding

test methods at the next revision.

NOTE 2 For details of precision statements, refer to ISO 5725-1:1994, Accuracy (trueness and precision) of measurement

methods and results — Part 1: General principles and definitions.
2 Normative references

The following standards contain provisions which, through reference in this text, constitute provisions of this

International Standard. At the time of publication, the editions indicated were valid. All standards are subject to

revision, and parties to agreements based on this International Standard 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.

ISO 3105:1994, Glass capillary kinematic viscometers — Specifications and operating instructions.

ISO 4788:1980, Laboratory glassware — Graduated measuring cylinders.
3 Definitions

For the purposes of this International Standard, the following definitions apply.

3.1 moisture content: The percentage loss in mass of the sample when a thin, evenly distributed film of the glue

is dried at 105 °C for 18 h – 1 h under standard conditions (see clause 6).

3.2 gel strength: A measure in arbitrary units of the rigidity modulus of a gel prepared and matured under

standard conditions (see clause 7).
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SIST EN ISO 9665:2001
ISO
ISO 9665:1998(E)
4 Sampling
4.1 General

The results of the analysis of glue carried out in accordance with this International Standard are limited in their

practical use by the degree to which the 1 kg test sample represents the whole consignment.

4.2 Initial selection of sample

The containers shall be selected from various parts of the consignment in such a manner that the widest

representation is obtained. The number of containers to be sampled shall be fixed by agreement between purchaser

and vendor. State the number of containers sampled in the test report.

From containers of 50 kg or more of glue, take a sample weighing not less than 1 kg when there is only one

container, and an increment of not less than 500 g from each container when there is more than one; from

containers of less than 50 kg of glue take a proportionate amount. This sample is called the preliminary sample.

Take appropriately sized samples by means of a sampling tube, scoop or similar tool to ensure that glue is taken

from the top, middle and bottom of the container.

Store these preliminary samples in clean, dry, airtight, non-absorbent containers until required.

NOTE — For further guidance, reference should be made to ISO 3951:1989, Sampling procedures and charts for inspection

by variables, for percent nonconforming, and ISO 8213:1986, Chemical products for industrial use — Sampling techniques —

Solid chemical products in the form of particles varying from powders to coarse lumps.

4.3 Final selection of sample

Mix the preliminary samples thoroughly and take one or more samples from the bulk, each weighing not less than

1 kg, and store them in clean, dry, airtight, non-absorbent containers. These samples shall be known as the

laboratory samples.
5 Preparation of test sample
5.1 Reduction of solid (powdered, pearl, cube and granulated) glue sample

Grind the sample by hand in a mortar, or alternatively in a laboratory disintegrator, of a type capable of grinding the

sample to a particle size of 3 mm or smaller. This sample is called the test sample. If necessary, quarter this sample

in the usual manner to bring the final mass to 500 g, taking care that a representative amount of all particle sizes is

included in the quartering. Keep the powdered samples so obtained in two air-tight containers, one container for the

test sample for moisture content (see clause 6) and the second container for all other tests.

The type of disintegrator used to grind the sample shall be agreed on between the purchaser and vendor because

different types of disintegrator generate different amounts of heat and have different effects on the moisture content

of the sample.

Because of the loss of moisture in grinding, take a separate sample for the moisture content test from the material

obtained by the preliminary breaking up, before the material is put through the disintegrator. This small separate

sample is then powdered by hand in a mortar and pestle, or cut with scissors, and is suitable for the moisture

content test. Make adjustment for the moisture content of the mechanically ground sample by comparison with the

hand-ground sample, which is considered as having the more reliable moisture content. By comparing the actual

moisture content found on the hand-ground sample with the moisture content of the mechanically ground sample,

the necessary adjustment to be made to the mass of the glue to be used in the various tests is determined by

calculation.
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SIST EN ISO 9665:2001
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ISO 9665:1998(E)

Place all samples immediately into an air-tight container because even a small change in the moisture content will

affect the result of some of the tests; for example, an increase of 1 % moisture will result in a decrease of about

2,5 % in gel strength when determined on the Bloom-type gelometer.
5.2 Concentrations for solid glues

Table 1 summarizes the mass of glue and volume of water required for each of the tests described. Weigh the

specified quantity of the powdered sample for each test separately, rather than by working from a large quantity of

stock solution.
Table 1 — Glue concentrations
Clause Test Mass of glue Volume of water
g ml
6 Moisture content 1 10
7 Gel strength (see 7.5.2) 15 (7,5) 105 (105)
8 Comparison of gel strength 5 to 10 50
9 Viscosity 15 105
10 Softening point 37,5 75
11 Setting point 37,5 75
12 Foam 5 50
13 pH 1 100
14 Grease 10 15
16 Keeping quality 20 80
5.3 Dissolving solid glues

Weigh the test portion in a beaker and add the requisite amount of cold distilled water, stirring with a thin metal or

glass rod. Place a watch glass over the mouth of the beaker and allow the sample to soak for 2 h at a temperature

not exceeding 22 °C. Heat the beaker in a water bath adjusted to a maximum temperature of 70 °C for about

15 min, taking care that the final temperature of the solution when in the bath reaches, but does not exceed, 60 °C.

During this heating period, gently stir the solution with the rod. Take care that the glue is completely dissolved: this

may be ascertained by lifting up the beaker and inspecting its contents through the bottom. When the test portion

has all dissolved, remove the beaker from the water bath.

If the sample gives a gel strength above 400 g Bloom, prepare the gel at a concentration of 6,67 %, and note this

observation in the report. The results on a 6,67 % solution are sometimes expressed as “single Bloom”, and those

on a 12,5 % solution as “double Bloom”.
6 Determination of moisture content
6.1 Principle

A weighed test portion of the glue is maintained at 105 °C for 18 h and is then reweighed.

6.2 Apparatus

6.2.1 Stainless-steel dish, flat-bottomed, 70 mm in diameter and 15 mm high, weighing about 30 g, preferably

fitted with an aluminium cover for use when cooling and weighing.
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ISO 9665:1998(E)
6.2.2 Oven, capable of being maintained at 105 °C – 1 °C.
6.2.3 Water bath.
capable of weighing to the nearest 0,01 g.
6.2.4 Balance,
6.2.5 Desiccator.
6.3 Procedure

Weigh into the tared dish (6.2.1), to the nearest 0,01 g, about 1 g of the test sample for moisture content (see 5.1,

third paragraph).

Add 10 ml of distilled water and allow the glue to soak. Place the dish on a warm water bath (6.2.3) so that the glue

is dissolved and a homogeneous solution obtained and leave there until most of the water has evaporated, giving a

uniformly thin film.

Transfer the dish to the oven (6.2.2) set at 105 °C – 1 °C, and allow it to remain there for 18 h – 1 h, during which

time the oven door shall not be opened. Remove the dish from the oven and, after allowing it to cool in a desiccator

(6.2.5), weigh it.
Carry out the determination in duplicate.
6.4 Expression of results
Calculate the moisture content (M) as a percentage by mass, using the equation:
mm-
M= · 100
where
m is the initial mass, in grams, of the test portion;
m is the mass, in grams, of the test portion after drying.

Express the result as the mean of the two values obtained in the duplicate determination.

6.5 Test report
The test report shall include the following information:
a) a reference to this International Standard;
b) all details necessary for the complete identification of the glue tested;

c) the number of containers sampled and the mass of glue taken from each container;

d) the results of the test, including the individual values, and any circumstances that may have affected the

results.
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SIST EN ISO 9665:2001
ISO
ISO 9665:1998(E)
6.6 Variation of gel strength and of viscosity with moisture content

If greater precision is required, adjust the result to allow for variations in the moisture content.

An approximate formula for the change in gel strength (DF) as a result of a change in moisture content (DM) is:

-·2FMD
DF=
100-M
where F is the gel strength at a percentage moisture content M .
1 1

This formula may be used to calculate the gel strength of glue at an agreed moisture content, e.g. 15 %.

NOTE — If M is taken as 15 %, then DF = F/42,5 for each 1 % change in moisture content. As an example of the scale of this

effect, an increase in moisture content from 15 % to 16 % reduces the measured gel strength of a 250 g gel strength glue by

6 g.

There is no satisfactory formula for the change of viscosity, Dh, with moisture content, DM, but a rough guide is

given by
Dhh=- 26, ·
100
This formula applies to 12,5 % solutions of glue.
7 Measurement of gel strength
7.1 Principle

The gel strength of the sample for the test is measured under arbitrary conditions. A suitable instrument measures

the force necessary to give a 4 mm depression in a gel of 12,5 % concentration by mass, matured for 16 h to 18 h

at 10 °C, using a standard plunger (7.2.4).

By convention, this force has normally been expressed as a mass in grams (see, however, 7.6).

7.2 Apparatus

7.2.1 Wide-neck bottle, of internal diameter 59 mm – 1 mm, approximately 85 mm high, having a capacity of

approximately 155 ml. The bottle shall have a stopper approximately 43 mm in diameter, pierced centrally with an

air vent about 2,5 mm in diameter.

7.2.2 Thermostatically controlled bath, capable of being maintained at 65 °C – 1 °C.

7.2.3 Totally enclosed thermostatically controlled bath, fitted with a thermometer, and capable of being

maintained at 10 °C – 0,1 °C.

7.2.4 Plunger, made of a suitable, stable polymer with a diameter of 12,7 mm and an edge radius of

0,39 mm – 0,04 mm (see figure 1).
NOTES

1 The diameter of the plunger and its edge radius are mandatory; other dimensions are for guidance only.

2 Some types of commercially available apparatus may have plungers that do not conform to the dimensions specified for the

diameter and edge radius, and it is essential that compliance, particularly with reference to the radius of curvature, be

ascertained.
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SIST EN ISO 9665:2001
ISO
ISO 9665:1998(E)
Dimensions in millimetres
Key
1 Tap
2 Brass locknut
3 Plunger
Figure 1 — Detail of plunger for gelometer

7.2.5 Gel-testing instrument (penetrometer), that enables the plunger to be brought just into contact with the

surface of the gel and then measures the force required to depress it vertically to a depth of 4 mm – 0,01 mm, either

at a constant rate of loading not exceeding 40 g/s or at a constant rate of penetration not exceeding 0,8 mm/s.

(See annex A for details of suitable instruments.)
7.2.6 Balance, capable of weighing to the nearest 0,01 g.
7.3 Dissolving the sample

Weigh out, to the nearest 0,01 g, 15 g of the test sample (see clause 5), and dissolve this test portion in 105 ml of

water in the wide-neck bottle (7.2.1) in the manner specified in 5.3, closing the bottle with the stopper. To prevent

caking, swirl the bottle vigorously to wet the glue completely. At this stage, take care not to build up more froth by

excessive agitation than will collapse before the bottle is inserted in the bath (7.2.2) maintained at 65 °C – 1 °C.

Particular care is necessary to see that the glue is all dissolved and that the solution is homogeneous. Place a

finger over the hole in the stopper and invert the bottle several times to mix in the water that has condensed on the

walls of the bottle and the under-side of the stopper.
7.4 Chilling the solution

To prevent cracking, allow the bottle to cool for 15 min at room temperature, and then place in the enclosed

thermostatic bath (7.2.3), maintained at 10 °C – 0,1 °C, for not less than 16 h and not more than 18 h. Ensure that

the platform of the thermostatic bath is horizontal and that the bottle stands evenly on it.

7.5 Procedure for determining gel strength
NOTE — See annex A for detailed instructions for particular instruments.

7.5.1 It is essential that the instrument stands perfectly level on a rigid support, that the plunger face is parallel to

the gel surface, and that the direction of plunger travel is perpendicular to the gel surface.

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SIST EN ISO 9665:2001
ISO
ISO 9665:1998(E)

7.5.2 Place the test bottle containing the gel on the platform of the penetrometer so that the centre of the gel is

underneath the plunger. Proceed with the sequence of operations required for the particular type of instrument in

use and record the force required to depress the plunger 4 mm into the gel. If the gel strength is above 400 g,

repeat the test using a solution prepared by dissolving 7,5 g of the test sample in 105 ml of water to give a solution

concentration of 6,67 %.
7.6 Expression of results

Express the result as the force, in newtons, required to depress the plunger 4 mm into the gel.

NOTE — In some instruments, the force is applied by the addition of weights to a container attached to a counter-balanced

plunger, and it has been customary with such instruments to quote the gel strength as “grams Bloom”, this being numerically

equal to the mass of the container plus the added weights. To enable comparison of current results with earlier records, it

should be noted that 1 N is numerically equal to 101,972 “grams Bloom”.
7.7 Test report
The test report shall include the following information:
a) a reference to this International Standard;
b) all details necessary for the complete identification of the glue tested;

c) the number of containers sampled and the mass of glue taken from each container;

d) the result of the test, the concentration of the glue solution and any circumstances which may have affected the

results;
e) the method and instrument used.
7.8 Validation of the test method

The following three criteria shall be satisfied in order to validate the test method:

a) The diameter of the gelometer plunger and the radius of curvature of its lower circular edge shall conform to the

dimensions given in figure 1.

NOTE 1 A profilometer is a satisfactory instrument for measuring the radius of curvature.

b) The gelometer used shall be calibrated using a device consisting of a strip of metal, supported near each end,

which offers a pre-determined resistance, simulating that of the surface of a gel being tested.

NOTE 2 This device is sometimes known as a “dummy Bloom” device and can usually be obtained from the

manufacturer of the test equipment. (See figure 2.)
Key
1 Spring steel strip
2 Support
3 Base
Figure 2 — Dummy Bloom device
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SIST EN ISO 9665:2001
ISO
ISO 9665:1998(E)

c) The full procedure shall be checked using samples standardized against reference samples of known gel

strength to ensure that differences in sample preparation and operating technique have not introduced variations.

All standard samples shall be corrected for variations due to moisture content if the moisture content differs by more

than 0,4 % from the value at the time of standardization (see 6.6).
8 Comparison of gel strength
8.1 Principle

Solutions of glues to be compared are prepared under identical conditions, allowed to gel for 16 h and their gel

strengths compared using any suitable instrument.

NOTE — This method is frequently used to compare batches of glues and to compare a given sample of glue against a

reference sample.
8.2 Apparatus
8.2.1 Balance, capable of weighing to the nearest 0,01 g.

8.2.2 Thermostatically controlled bath, capable of being maintained to within 0,1 °C at a temperature between

5 °C and 30 °C (for use if numerical results are required).
glass, 150 ml capacity.
8.2.3 Beaker,
8.2.4 Instrument for comparing gel strengths.
8.3 Procedure

Weigh, to the nearest 0,01 g, 5 g to 10 g, according to grade and use, of each test sample (see clause 5) into a

150 ml beaker (8.2.3), and add 50 ml of cold distilled water from a pipette. Dissolve the test portion in the manner

specified in 5.3. Pour the glue solution immediately into a suitable cylindrical container and, after 2 min, put the lid

on.

Cool the container for 16 h using method a) if numerical results are to be obtained, or either method a) or method b)

if only comparative (ranking) results are required:

a) place in a water bath (8.2.2), thermostatically controlled at a temperature to be stated in the test report;

b) place in a bath of cold running water.

Numerical values obtained using methods a) and b) above are to be used only for ranking samples of glue and not

for obtaining values to be quoted as “gel strengths”, for which the method given in clause 7 is used.

8.4 Expression of results

Express the results by identifying the glue samples and listing them in the order of their apparent gel strengths.

If the temperature of gelling was controlled, this temperature shall be stated, and the numerical values of the

apparent gel strengths as indicated by the instrument (8.2.4) selected to measure them may be quoted as

“comparative strengths”.
8.5 Test report
The test report shall include the following information:
a) a reference to this International Standard;
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SIST EN ISO 9665:2001
ISO
ISO 9665:1998(E)
b) all details necessary for the complete identification of the glue tested;

c) the number of containers sampled and the mass of glue taken from each container;

d) the concentrations of the glue solutions used and, if numerical results are to be quoted, the gelling temperature,

in degrees Celsius;

e) the results of the test, the instrument used and any circumstances that may have affected the results.

9 Determination of viscosity
9.1 Method 1: Glass-capillary viscometer
9.1.1 Principle

The viscosity of a sample of the glue is determined at 60 °C with a glass-capillary viscometer. (See also the

Introduction.)
9.1.2 Apparatus

9.1.2.1 Glass-capillary viscometer, of any type as described in ISO 3105. It is essential that the time of efflux is

within the range of accuracy of the chosen instrument. The viscometer shall be calibrated.

9.1.2.2 Thermostatically controlled bath, capable of being maintained at 60 °C – 0,2 °C.

9.1.3 Procedure

Weigh, to the nearest 0,01 g, 15 g of the test sample (see clause 5) into a corked bottle or flask and add 105 ml of

cold distilled water. Swell and dissolve the test portion in the manner specified in 5.3. Pour the liquid through a

funnel loosely plugged with cotton wool (see however the note) into the viscometer (9.1.2.1) and allow to stand in

the thermostatically controlled bath (9.1.2.2), maintained at 60 °C – 0,2 °C, for 15 min before making the

measurement.

NOTE — A sintered-glass filter of suitable porosity may be used instead of the cotton-wool plug.

9.1.4 Expression of results

Express the result either as the kinematic viscosity, in square millimetres per second (1 mm /s = 1 cSt), or as the

dynamic viscosity, in millipascal seconds (1 mPa�s = 1 cP).
NOTES

1 For most routine test purposes, it is reasonable to use 1,02 g/ml as the density of the solution in calculating the dynamic

viscosity from the kinematic viscosity.

2 The present industry convention is to express viscosity in millipoises (1 cP = 10 mP).

9.1.5 Test report
The test report shall include the following information:
a) a reference to this International Standard;
b) all details necessary for the complete identification of the glue tested;

c) the number of containers sampled and the mass of glue taken from each container;

d) the result of the test, together with a full description of the apparatus used and any circumstances which may

have affected the results;
e) the method used, i.e. method 1 of this International Standard.
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9.2 Method 2: American pipette
9.2.1 General

This method is a convenient secondary method which may be used for production control. The method is suitable

for the range of viscosities of 2,5 mPa�s (2,5 cP) to 20 mPa�s(20 cP).
9.2.2 Principle

The viscosity of a sample is determined at 60 °C by measuring the flow time of the sample from a standard pipette.

9.2.3 Apparatus

9.2.3.1 American pipette and container (see figure 3). This consists of a modified 100 ml pipette immersed in a

thermostatic bath which may be in the form of an inverted bell jar or transparent plastic container, and which is

capable of being maintained at 60 °C – 0,2 °C. The bath shall have a means for circulating water.

NOTES

1 A suitable method for circulating the water is to use a small external air pump which produces a fine stream of air bubbles.

2 Any other 100 ml pipette with a calibrated precision tube may be used.
9.2.3.2 Timing device

9.2.3.3 Thermostatically controlled bath, capable of being maintained at 65 °C – 2 °C.

9.2.4 Procedure

Prepare the samples as described in 9.1.3, but place the bottle or flasks in a thermostatically controlled bath

(9.2.3.3) at a temperature of 65 °C – 2 °C for a period of not more than 15 min. Close the lower end of the pipette

with the finger and pour sample liquid into the pipette in the thermostatic bath (see 9.2.3.1), maintained at

60 °C – 0,2 °C, as quickly as possible, without trapping air, until the level of the solution is approximately 1 cm

above the upper mark. Place the bottle or flask below the end of the pipette. Insert the thermometer, which has

been maintained at 60 °C to 65 °C in warm water, into the bath and move slowly up and down until a temperature of

60 °C is shown when the thermometer bulb is midway between the top and bottom of the bulb of the pipette.

Remove the thermometer and adjust the level of the solution in the pipette so that the bottom of the meniscus

coincides with the upper mark on the pipette.

Remove the finger from the end of the pipette and measure the time for the pipette to deliver 100 ml of the solution.

Clean the interior of the apparatus immediately after the determination by rinsing with water at 60 °C.

9.2.5 Calibration of the pipette
Calibrate the pipette by one of the following procedures:

a) carry out measurements using standard-viscosity oils and plot flow time against viscosity;

b) compare results obtained with the pipette with results obtained with viscosities specified in method 1 and plot

flow time against viscosity.
9.2.6 Expression of results

Express the results either as the kinematic viscosity, in square millimetres per second (1 mm /s = 1 cSt), or as the

dynamic viscosity, in millipascal seconds (1 mPa�s = 1 cP), at 12,5 % concentration at 60 °C.

NOTE — The dynamic viscosity (measured in millipascal seconds or centipoises) is obtained by multiplying the kinematic

viscosity (measured in square millimetres per second or centistokes) by the density of the glue solution at 60 °C,

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