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ADHESIVE COMPOUNDS: UDC 678.

01
TESTS FOR USE IN MARINE ENVIRONMENTS

Key words: Adhesive compounds, sealing, peel strength, shear strength, tensile
strength, tear strength, hardness, classification, marine environments, test method

CONTENTS 1 PREFACE
1 PREFACE 1 This test method describes tests on adhesive compounds
and acts as a basis for the classification of adhesive com-
2 ENVIRONMENTAL EXPOSURES 2
2 pounds. The method allows the choice of an adhesive best
2.1 Effect of sunlight and salt water
suited to the application environment in question, and indi-
2.1.1 Test method 2
cates its most significant durability parameters to enable a
2.1.2 Test specimens 2
2 correct design of the joint.
2.1.3 Test arrangements
2.2 Effect of temperature 2 The method comprises a selection of the most appropriate
2.2.1 Test method 2 of the existing standards. ISO, DIN, SFS, EN and ASTM
2.2.2 Test specimens 2 standards are used. Within the standards there is a rela-
2.2.3 Test arrangements 2 tively large freedom of action, starting with the shape of the
2.3 Chemical durability 2 test specimens. Therefore the set-up has been chosen with-
2.3.1 Test method 2 in the limits of the standards to provide a testing system
2.3.2 Test solutions 2 giving results that can be mutually compared. The use of
2.3.3 Temperatures of the test solutions 2 adhesive has been divided into four clearly defined and
2.3.4 Exposure time 3 separate areas:
2.3.5 Test specimens 3 l Open deck area
2.3.6 Test arrangements 3 l Accommodation
3 DETERMINATION OF STRENGTH l Machinery area
CHARACTERISTICS 3 l Underwater areas
3.1 Shear strength 3 External factors that may have an effect on the physical
3.1.1 Test method 3 characteristics of adhesives have been chosen for each
3.1.2 Test specimens 3 area. Certain physical characteristis of adhesives are de-
3.1.3 Results 3 fined using test pieces prepared in each usage environment,
3.2 Tensile strength 3 or the pieces are tested in the desired environment.
3.2.1 Test method 3
3.2.2 Test specimens 3 Environmental parameters include:
3.2.3 Results 4 l The ageing effect of sunlight and rain (open deck area)
3.3 Peel strength 4
l The effect of temperature (machinery area)
3.3.1 Test method 4
3.3.2 Test specimens 4 l The effect of chemicals, such as water, petrol, oil, diesel
3.3.3 Results 4 oil and solvents (underwater areas and machinery area).
3.4 Hardness 4 The aim has been to determine the mechanical character-
3.4.1 Test method 4 istics of the adhesive compounds with as few tests as poss-
3.4.2 Test specimens 4 ible, but the requirements has been that the critical proper-
3.4.3 Results 5 ties can be found. The test parameters are:
APPENDIX 6-7 l shear strengh τ
l tensile strength σ
l peel strength p
l hardness m

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NORDTEST METHOD NT POLY 175 2

Table 1 shows the strength parameters to be measured, as the relative humidity shall be 65 % ± 5 %. The composition
well as the exposures. The character ‘X’ marks the ex- of the spraying water should be equivalent to sea water, as
posures to be carried out for each durability test. defined in the standard DIN 50900. During the spraying
period the xenon lamps must be on.
Table 1. Exposures carried out for different strength tests.
After the exposure the test pieces are stored in an environ-
ment with a temperature of 20 °C ± 3 °C and a relative
humidity of 65 % ± 5 %. The storage period should be 16-
24 hours.

2.2 The effect of temperature


2.2.1 Test method
1) This is of little importance, if the object with the adhesive bond is opaque. The test method used is ASTM D 1151-84 standard test
No need for separate testing. In bonds where sunlight can affect the bond method for effect of moisture and temperature on adhesive
from the edge, the relative change in tensile strength can be used as a
guide. joints. The test environment used is environment No. 15,
with a temperature of 85 °C and the test specimens are
Appendix lists the standards necessary for the test method. suspended above a vessel of water. The exposure time is
48 hours.
The tests are carried out with test specimens determined by
2 ENVIRONMENTAL EXPOSURES Table 1.
2.1 Effect of sunlight and salt water
2.1.1 Test method 2.2.2 Test specimens
The test method used is ISO 4892-2:1994 Plastics - Meth- The test specimens have been defined in Section 1. “Defi-
ods of exposure to laboratory light sources - Part 2: Xenon nition of Durability Characteristics”, separately for each test.
arc sources. The standard emulates the ageing effect of
sunlight and water.
2.2.3 Test arrangements
The lamps used in the test are xenon lamps, which have
been found to have a radiation distribution equivalent to The test arrangements are according to the standard.
natural light. Compared with the effect of natural sunlight,
this test is not necessarily accelerated.
2.3 Chemical durability
The xenon arc lamps used in the test should have a relative
spectrum in accordance with Method A, and their absolute
2.3.1 Test method
radiation intensity should be 550 W/m2 ± 50 W/m2 within the The test method used is ISO 175:1981 Plastics - Determi-
wavelength range of 280 nm - 800 nm. nation of resistance to liquid chemicals. The standard is
The tests are carried out with test specimens determined by used with the adjustments listed below.
Table 1.
2.3.2 Test solutions

2.1.2 Test specimens The following solutions listed in the standard are used, each
separately:
The test specimens have been defined in Section 1. “Defi-
l Petrol (standard fuel, ISO 1817 liquid 2)
nition of Durability Characteristics”, separately for each test.
l Lubricating oil (SAE 10W40, ISO 1817 oil 3)
l Solvents (toluene)
2.1.3 Test arrangements
The test specimens should be placed in the climate chamber 2.3.3 Temperatures of the test solutions
so that their wider edge is exposed to radiation. The test The temperatures of the test solutions and the test temper-
specimen clamps should be protected on the rear side of the atures are listed in the following table:
test specimen using a matte stainless steel plate. In order to
allow for the free circulation of air, a gap of at least 2 mm Test solution Exposure Test
should remain between the plate and the test specimen. The temperature temperature
(°C) (°C)
expansions at the ends of the test specimens should also be
protected against radiation using matte stainless steel Standard fuel, ISO 1817
liquid 2 60 60
plates.
Lubricating oil SAE 10W40,
The duration of the dry period should be 102 minutes, fol-
ISO 1817 oil 3 82 82
lowed by a 18-minute spraying period. During the dry period,
Toluene 23 23
the black standard temperature should be 65 °C ± 3 °C and
NORDTEST METHOD NT POLY 175 3

2.3.4 Exposure time When the specimens are at least two weeks old, the necess-
ary environmental exposures are carried out. After this, the
The exposure time should be 100 hours. During this period,
actual mechanical characteristics can be tested.
the test specimen should be totally immersed in the test
solution.

3.1.3 Results
2.3.5 Test specimens Each test series should give a minimum of five acceptable
The test specimens have been defined in Section 1. “Defi- test results. The results are given using the unit N/mm2 with
nition of Durability Characteristics”, separately for each test. the accuracy specified in the standard.
The change caused by the exposure is given as a relative
change in strength, according to the formula
2.3.6 Test arrangements
The test arrangements are according to the standard. τR - τ0
τre =
τ0

where
3 DETERMINATION OF STRENGTH
τR is shear strength after the environmental exposure
CHARACTERISTICS
τ0 is shear strength before the environmental exposure.
3.1 Shear strength A positive strength change indicates an increase in strength
3.1.1 Test method and a negative strength change indicates a decrease in
strength.
The test method used is ISO 110003-2:1994 Structural ad-
hesives - Determination of shear strength behaviour - Part
2: Thick adherend tensile test method.
The test is intended for thick adhesive joints and is well 3.2 Tensile strength
suited for elastic adhesive compounds. Stiff test specimens 3.2.1 Test method
with a short adhesive layer overlap are used in the test. This
provides as equal shear stress distribution as possible, and The test method used is the standard DIN 53504:1985,
enables minimisation of undesired tensile stress. The stan- Determination of tensile stress/strain properties of rubber.
dard is used with the adjustments listed below. The test is actually intended for rubber, but it is well suited
The thickness of the adhesive layer is 2 millimetres. This also for elastic adhesive compounds. The standard is used
can be done by using padding pieces of the same thickness with the adjustments listed below.
which are fastened outside the joint to be measured in the The test method presented in the standard defines the ten-
cut test specimens. sile strength at break, tensile stress at yield, elongation at
The following strength parameters are defined with the test: break and secant modulus. Defining the modulus of elas-
ticity is not recommended. Instead, the secant modulus is
· The shear strength of the adhesive joint defined for the strain ranges of 0.5 - 5 %, 0.5 - 10 %, 0.5 -
· The shear modulus of the adhesive joint. 25 % and 0.5 - 50 %.
The method is used to test specimens prepared using the The method is used to test specimens prepared using the
environments defined in Table 1. environments defined in Table 1.

3.1.2 Test specimens


3.2.2 Test specimens
The material of the test specimens is AIMg4,5Mn aluminium.
Blanks for specimens can be either precut sheets or uncut Bone-shaped specimens of type S2 are used as test speci-
sheets, in which case all cutting of the test specimen is mens. The test specimens should be manufactured by cast-
performed after bonding. When precut blanks are used, it is ing between two plates that do not bond with the adhesive,
possible to avoid the effects of the heat generated by cut- or by using a suitable stiff plastic film (PTFE film) between
ting. the plates and the adhesive. To ensure that the cast is as
even as possible, padding pieces of the required thickness
The test specimens are made according to the standard. should be used between the plates. Before the cast is cut to
The surfaces to be bonded are prepared according to the shape, or exposed to the test environment, the test material
standard ISO 4588-1989 Adhesives - Preparation of metal should be set throughout. Special attention should be paid
surfaces for adhesive bonding, and the actual bonding is to the mixing of the adhesive and casting, so that the access
carried out according to the instructions of the adhesive of air into the adhesive or between the adhesive and the
manufacturer. casting mould is avoided.
There should be enough test specimens so that at least five There should be enough test specimens so that at least five
acceptable test results are obtained in each test series. acceptable test results are obtained in each test series.
NORDTEST METHOD NT POLY 175 4

When the specimens are at least two weeks old, the necess- adhesive layer is as even as possible, a 2.0-mm thick ribbon
ary environmental exposures are carried out. After this, the or string should be placed between the sheets, outside the
actual mechanical characteristics can be tested. area to be measured. After the adhesive has set, the
bonded sheets are cut into strips. It is important to try to
avoid any detrimental heating caused by the cutting.
3.2.3 Results When the specimens are at least two weeks old, the necess-
ary environmental exposures are carried out. After this, the
Each test series should give a minimum of five acceptable
actual mechanical characteristics can be tested.
test results. The results are given using the unit N/mm2, with
the accuracy specified in the standard. There should be enough test specimens so that at least
three acceptable test results are obtained in each test
The change caused by the exposure is given as a relative
series.
change in strength, according to the formula

3.3.3 Results

where Each test series should give a minimum of three acceptable


- test results. The results are given as the average of the test
σR is tensile strength after the environmental exposure results, using the unit N/mm2, with the accuracy specified in
σ0 is tensile strength before the environmental exposure. the standard.
A positive strength change indicates an increase in strength The change caused by the exposure is given as a relative
and a negative strength change indicates a decrease in change in strength, according to the formula
strength.
PR - P0
Pr =
P0
3.3 Peel strength
where
3.3.1 Test method
PR is peel strength after the environmental exposure
The test method used is the standard ASTM D 3167:1976, P0 is peel strength before the environmental exposure.
Standard Test Method for Floating Roller Peel Resistance of A positive strength change indicates an increase in strength
Adhesives. The standard is used with the adjustments listed and a negative strength change indicates a decrease in
below. strength.
The aim of the test is to define the peel strength of an
adhesive joint between two metal plates so that good re-
peatability is achieved at both low and high strength levels. 3.4 Hardness
The test is carried out by pulling the thinner of two bonded
3.4.1 Test method
metal strips, with a pulling load, through a metal roller
equipped with bearings. This gives as even a pulling load as The test method used is the standard DIN 53505:1987,
possible. During the test the average load per unit of width Harteprufung nach Shore A und Shore D. The hardness is
is measured. measured as Shore A hardness. If the material exceeds the
upper limit of Shore A hardness, Shore D hardness may
As the bending of the metal strip also binds energy, only the
be used. The standard is used with the adjustment listed
actual bending energy should be measured. This can be
below.
achieved by measuring a test specimen that has been
bonded at the end only. The load per unit width obtained is The method is used to test specimens prepared using the
deducted from the results obtained. environments defined in Table 1.
The method is used to test specimens prepared using the
environments defined in Table 1.
3.4.2 Test specimens
The test specimens should be at least 6 mm thick, with a
3.3.2 Test specimens minimum diameter of 35 mm. Suitable test specimens can
be made from the waste left over from manufacturing the
The test specimens are manufactured from a stiff and a
tensile strength test specimens. In this case, three of the 2-
flexible aluminium sheet by bonding the sheets with an even
mm thick specimens are places on top of each other as
2 mm thick adhesive layer. The sheet material used is
stated in the standard. The detailed definition of the test
AIMg4,5Mn aluminium. The thickness of the stiff sheet
specimens is given in the standard. One 6-mm thick test
should be 2.5 mm, and that of the flexible one 0.5 mm. The
specimen is sufficient for each test.
bonding surfaces are prepared according to the standard
ISO 4588-1989 Adhesives - Preparation of metal surfaces When the specimens are at least two weeks old, the necess-
for adhesive bonding, unless the adhesive manufacturer has ary environmental exposures are carried out. After this, the
provided his own, specific requirements. To ensure that the actual mechanical characteristics can be tested.
NORDTEST METHOD NT POLY 175 5

3.4.3 Results where


The results are given as specified in the standard. mR is hardness after the environmental exposure
m0 is hardness before the environmental exposure.
The change caused by the exposure is given as a relative
change in hardness, according to the formula A positive hardness change indicates an increase in hard-
ness and a negative change indicates a decrease in hard-
mR - m0 ness.
mr =
m0
NORDTEST METHOD NT POLY 175 6

APPENDIX

A LIST OF THE MOST SIGNIFICANT STANDARDS RELATING TO THE METHOD

SHEAR STRENGTH EN 28 510-1-1993


ISO 11003-2 Structural adhesives - Determination of ISO 8510/2 Adhesives - Peel test for a flexible - to
shear behaviour. Part 2: Thick adherent - rigid bonded assembly. Part 1: 180°
tensile-test method. peel.
ISO 1922-1981 Cellular plastics - Determination of EN 28 510-2-1993
shear strength of rigid materials. ISO 4578-1990 Adhesives - Determination of peel re-
ISO 1827-1976 Rubber, vulcanised - Determination of sistance of high-strength adhesive
modulus in shear - Quadrible shear bonds. Floating roller method.
method. EN 1464-1994
DIN 53445 Testing of polymer materials; torsion DIN 53515-1990 Determination of tear strength of rubber
pendulum test. elastomers and plastic film using
DIN 53399-1982 Testing of reinforced plastics, shear Glaves angle test piece.
test on plane specimens. DIN 16860 Dispersion adhesives and adhesives
ASTM D 732-1990 Test method for shear strength of plas- based on synthetic rubber solutions for
tics by Punch tool. use with PVC floor coverings without
backing.
SFS 3258 Muovit - Kiertoheilurikoe.
DIN 53507-1983 Testing rubber and elastomers - Deter-
ISO 4587-1979 Adhesives - Determination of tensile
mination of the tear strength of elasto-
lap-shear strength of high-strength ad-
mers, Trouser test piece.
hesive bonds.
SFS 3563 Kumit - Repimislujuuden maaritys.
ASTM 1876-1972 Standard test method for peel resist-
TENSILE STRENGTH ance of adhesives.
IS0 527.2-1985 Plastics - Determination of tensile ASTM D 903-1949 Standard test method for peel or strip-
properties. ping stength of adhesive bonds.
ISO 37-1977 Rubber, vulcanised - Determination of ASTM D 3807-1979 Standard test method for strength proper-
tensile stress - strain properties. ties of adhesives cleavage peel by
ISO 1798-1983 Polymeric materials, cellular flexible - tension loading.
Determination of tensile strength and ASTM D 3167-1976 Standard test method for floating roller
elongation at break. peel resistance of adhesives.
ISO 1926-1979 Cellular plastics - Determination of ten-
sile properties of rigid materials.
HARDNESS
ISO 1421-1977 Fabrics coated with rubber or plastics -
Determination of breaking strength and IS0 2039 Plastics and ebonite - Determination of
elongation at break. hardness. Part 1: Ball indention meth-
od.
ISO 527-1994 Testing of plastics - Tensile test.
ISO 48 Vulcanised rubbers - Determination of
DIN 53504-1985 Determination of tensile stress strain
hardness (Hardness between 30 and
properties of rubber.
85 IRHD).
DIN 53455-1981 Testing of plastics - Tensile test.
ISO 866 Plastics and ebonite - Determination of
SFS 3151 Muoviputket - Vetokoe. indentation hardness by means of a
SFS 3562 Kumit - Vetomurto-ominaisuuksien durometer (Shore hardness).
maaritys. ISO 2039-2 Plastics - Determination of hardness by
ASTM 638-1991 Test method for tensile properties of the indentation method. Part 2: Rock-
plastics. well hardness.
ISO 1400 -1975 Vulcanised rubbers of high hardness
(85-100 IRHD) - Determination of hard-
PEEL STRENGTH ness.
ISO 8510/1 Adhesives - Peel test for a flexible - to ISO 1818-1975 Vulcanised rubbers of low hardness
- rigid bonded assembly. Part 1: 90° (10-35 IRHD) - Determination of hard-
peel. ness.
.

NORDTEST METHOD NT POLY 175 7


APPENDIX

ISO 2439-1980 Polymeric materials, cellular flexible - ISO 2440-1983 Polymeric materials, cellular flexible -
Determination of hardness (indentation Accelerated ageing test.
technique). ISO 8580-1987 Rubber and plastics hoses - Determi-
ISO 2783-1975 Ebonite - Determination of hardness by nation of ultra-violet resistance under
means of a dyrometer. static conditions.
DIN 53505-1987 Härteprüfung nach Shore A und Shore EN ISO 8580-1995
D. ISO 8586-1987 Rubber and plastics hoses - Determi-
SFS 4771 Muovit - Kovuuden määrittaminen. Osa nation of ultra-violet resistance under
2: Rockwell-kovuus. static conditions.
SFS 3561 Kumit - Kovuuden maaritys (kovuus - ISO 1419-1977 Fabrics coated with rubber or plastics -
alue 10-85 IRHD). Accelerated ageing and simulated ser-
SFS 3912 LM-tuotteet. Barcol-kovuuden maaritys. vice test.
DIN 53386-1982 Testing of plastics and elastomers -
ASTM D 2240-1991 Test method for rubber property - Du-
rometer hardness. Exposure to neutral weathering.

ASTM D 2583-1987 Test method for indentation hardness DIN 53387-1989 Artificial weathering and ageing of plas-
of rigid, plastics by means of a Barcol tics and elastomers by exposure to fil-
tered xenon-arc radiation.
impressor.
SFS 3567 Kumit - Otsonikestävyyden määritys
staattisissa olosuhteissa.
CHEMICAL RESISTANCE
SFS 3574 Kumit - Kumi 64. Säätä ja roiskeöljyä
ISO 175-1981 Plastics - Determination of resistance kestävät kumit.
to liquid chemicals. ASTM D 2565-1989 Standard practice for operating xenon
ISO 4611 Plastics - Determination of the effects arc-type light-exposure of plastics.
of exposure to damp heat, water spray
and salt mist.
ISO 1817-1985 Rubber, vulcanised - Determination of HEAT RESISTANCE
the effect of liquids.
ISO 1110 Plastics, Polyamides - Accelerated
ISO/TR 7473-1981 Unplasticized polyvinyl chloride pipes conditioning of test specimens.
and fittings - Chemical resistance with
ISO/DIS 306 Plastics, Thermoplastics materials -
respect to fluids.
Determination of Vicat softening tem-
lSO/TR 7474-1981 High density polyethylene pipes and fit- perature.
tings - Chemical resistance with re-
ISO/DIS 483 Plastics - Small enclosures for con-
spect to fluids.
ditioning and testing at relative humidi-
DIN 53393-1976 Testing of textile glass-reinforced plas- ties maintained by aqueons solutions.
tics - Behaviour to the effects of chemi-
ISO 188-1982 Rubber, vulcanised - Accelerated age-
cals.
ing or heat-resistance tests.
SFS 4568 Muovit - Kuuman höyryn, vesisumun ja
SFS 3565 Kumit - Lämpövanhentamiskoe.
suolasumun vaikutuksen määrittaminen.
SFS 3568 Kumit - Standardilämpötilat, kosteudet
SFS 3566 Kumit - Nesteiden vaikutuksen määri-
ja ajat koekappaleiden ilmastoinnille ja
tys.
testaamiselle.
SFS 4978 Tiivistelevyt - Öljynkestava kumi. Tyyp-
ASTM D 1151-1984 Standard test method for effect of
pi 0.
moisture and temperature on adhesive
ASTM 581-1987 Practice for determination of chemical bonds.
resistance of thermosetting resins used
ASTM D 1183-1970 Standard test method for resistance of
in glassfiber reinforced structures in-
adhesives to cyclic laboratory ageing
tended for liquid service.
conditions.

AGEING
PREPARATION OF ADHESIVE BONDING
ISO 877-1994 Testing of plastics and elastomers -
Exposure to daylight under glass. ISO 4588-1989 Adhesives - Preparation of metal sur-
faces for adhesive bonding.
ISO 4892-1994 Plastics - Method of exposure to
laboratory light sources. Part 2: Xenon
arc sources.

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