BS 2972-1989
BS 2972-1989
BS 2972-1989
Inorganic thermal
insulating materials
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
UDC 662.998:699.86:691:546.08:620.1
BS 2972:1989
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
Combustion Engineering Association
Cranfield Institute of Technology
Department of Health and Social Security
Department of the Environment (Building Research Establishment)
Department of Trade and Industry (National Engineering Laboratory)
Department of Trade and Industry (National Physical Laboratory)
Electricity Supply Industry in England and Wales
Engineering Equipment and Materials Users’ Association
Eurisol (UK Mineral Wool Association)
Gypsum Products Development Association
Phenolic Foam Manufacturers’ Association
Refrigeration Industry Board
Royal Institute of British Architects
Thermal Insulation Manufacturers’ and Suppliers’ Association (TIMSA)
Thermal Insulations Contractors’ Association
Water Tube Boiler Group, Power Plant Contractors’ Association
The following bodies were also represented in the drafting of the standard,
through subcommittees and panels:
© BSI 02-2000
Amendments issued since publication
First published May 1961
First revision August 1975
Second revision November 1989 Amd. No. Date of issue Comments
Contents
Page
Committees responsible Inside front cover
Foreword iv
Section 1. General
1 Scope 1
2 Definitions 1
3 Sampling 1
Section 2. Dimensions
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
4 General 4
5 Measurement before application 4
6 Measurement after application 10
7 Weighing 11
Section 3. Bulk density
8 General 12
9 Preformed materials 12
10 Plastic composition materials 13
11 Flexible materials 13
12 Loose-fill materials 13
13 Blown materials 18
Section 4. Thermal properties
14 Thermal conductivity 21
15 Specific heat capacity 21
16 Thermal diffusivity 21
Section 5. Assessment of fire hazard
17 General 22
18 Assessment of self heating hazard 22
Section 6. Heat stability
19 General 24
20 Apparatus 24
21 Preparation of test specimen 24
22 Procedure 24
23 Expression of results 24
Section 7. Resistance to compression
24 Apparatus 25
25 Specimens 25
26 Procedure 25
27 Expression of results 26
Section 8. Interlaminar strength
28 General 27
Section 9. Vibration settlement
29 Vibration at high frequency and small amplitude 29
30 Expression of results 29
31 Description of a gauge for measuring settlement of fibrous materials 30
Section 10. Covering capacity
32 General 32
33 Apparatus 32
34 Procedure 32
35 Expression of results 32
© BSI 02-2000 i
BS 2972:1989
Page
Section 11. Moisture content
36 General 34
37 Specimens 34
38 Preparation of test specimens 34
39 Procedure 34
40 Expression of results 34
Section 12. Water absorption
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41 General 35
42 Specimens 35
43 Procedure 35
44 Expression of results 35
Section 13. Water vapour permeance
45 Procedure 36
46 Conversion of units 36
Section 14. Coarse shot content
47 General 38
48 Apparatus 38
49 Procedure 38
50 Expression of results 38
Section 15. Oil content
51 General 39
52 Apparatus 39
53 Procedure 39
54 Expression of results 39
Section 16. Organic matter
55 General 40
56 Method 1. Determination of organic matter 40
57 Method 2. Determination of the concentration of carbon in
inorganic insulation materials without combined water and/or
carbonates 40
58 Method 3. Determination of the concentration of carbon in
inorganic insulating materials containing combined water
and/or carbonates 41
Section 17. Air permeability
59 General 45
60 Apparatus 45
61 Procedure 45
62 Expression of results 45
Section 18. Flexural strength
63 General 47
64 Apparatus 47
65 Specimens 47
66 Procedure 47
67 Expression of results 47
Section 19. Fibre diameter
68 General 48
69 Apparatus 48
70 Specimen preparation 48
ii © BSI 02-2000
BS 2972:1989
Page
71 Slide preparation 48
72 Measurement procedure 48
73 Expression of results 50
Section 20. Electrical conductivity of aqueous extract
74 General 51
75 Apparatus 51
76 Conditioning atmosphere 51
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77 Sample 51
78 Procedure 51
Section 21. Trace quantities of water-soluble chlorides
79 General 53
80 Method 1 53
81 Method 2 54
Section 22. pH value of water extract
82 Preparation of sample 56
83 Determination of pH value of water extract 56
Figure 1 — Thickness gauge 6
Figure 2 — Determination of deviation from square of a board 9
Figure 3 — Apparatus for determining bulk density of powders 15
Figure 4 — Alternative apparatus for determining bulk density of
powders 16
Figure 5 — Apparatus for determining bulk density of powder and
granular insulating materials after attrition 17
Figure 6 — Measuring device 19
Figure 7 — Top views of vibration boxes: showing positions for height
measurements 20
Figure 8 — Specimen mounting for interlaminar strength test 28
Figure 9 — Vibration tester 31
Figure 10 — Apparatus for determining carbon dioxide produced
by ignition 41
Figure 11 — Apparatus for determining carbon dioxide produced
by boiling in acid 43
Figure 12 — Apparatus for measuring air permeability of
insulating materials 46
Figure 13 — Illustration of measurement rules 49
Figure 14 — Field scanning sequence 50
Table 1 — Sample sizes and rates of additional sampling 2
Table 2 — Size and number of specimens 3
Table 3 — Methods of thickness measurement 5
Table 4 — Calculation of insulation thickness 11
Table 5 — Thickness test under pressure 25
Table 6 — Water vapour permeance conversion factors 37
Publications referred to Inside back cover
Foreword
This revision of BS 2972 was prepared under the direction of the Refrigeration,
Heating and Air Conditioning Standards Policy Committee. It supersedes
BS 2972:1975, which is withdrawn.
All the test methods of the 1975 edition have been reviewed. A few remain in their
original form, with some minor amendments. The sections on odour, and
emissivity of metal foil (sections 13 and 15 in the 1975 edition) have been deleted.
The new section 8 gives a test for interlaminar strength. The new section 22 gives
a method of test for pH value of a water extract.
Significant modifications have been made to the following sections:
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
Section 2. Dimensions. Measurement of the deviation from squareness of a
board has been added.
Section 3. Bulk density. This now includes a method of test for blown
materials.
Section 6. Heat stability. This has been re-written to clarify and improve
the test equipment and method.
Section 9. Vibration settlement. Requirements for testing the settlement
of blown materials have been added to the high frequency/small amplitude
test.
The test for jolting at low frequency/high amplitude has been deleted because
it was rarely, if ever, used.
The test for stability under heat and vibration has been deleted pending the
development of a more suitable method.
Section 12. Water absorption. A new test method has been added for
resistance to capillary absorption.
Section 14. Coarse shot content. A new dry method has been introduced in
place of the former wet method, which used a special glass elutriator.
Section 19. Fibre diameter. The method has been revised to facilitate the
identification and measurement of fibre diameters.
Section 21. Trace quantities of water-soluble chlorides. The
potentiometric titration method, introduced by amendment in 1982, has been
deleted and replaced by a polarographic titration method.
It is very important that claims for technical quality of materials should be
related to well established methods of test which are based on sound fundamental
principles, and the purpose of this standard is to provide details of basic tests for
the assessment of a range of properties which are likely to be of value to a
potential user. Some of these tests may not be suitable for quick routine control
checking; essentially, they should be regarded as the basis for reference purposes
in the event of dispute or of doubt concerning the accuracy of such more rapid
methods as may be used as a matter of convenience. It is strongly recommended
that, where any dispute arises, the methods of this standard only be used.
A British Standard does not purport to include all the necessary provisions of a
contract. Users of British Standards are responsible for their correct application.
Compliance with a British Standard does not of itself confer immunity
from legal obligations.
Summary of pages
This document comprises a front cover, an inside front cover, pages i to iv,
pages 1 to 56, an inside back cover and a back cover.
This standard has been updated (see copyright date) and may have had
amendments incorporated. This will be indicated in the amendment table on the
inside front cover.
iv © BSI 02-2000
BS 2972:1989
Section 1. General
© BSI 02-2000 1
BS 2972:1989
Plastic composition materials are particularly When samples are to be drawn from material which
vulnerable to such modification, if only through the has already been applied to a portion of plant,
method of application, so that tests at the source of e.g. for bulk density determination on plastic
supply may not be a reliable guide to the behaviour composition or loose-fill insulating materials, care
of the material during service on the plant. shall be taken to ensure that the portion of material
3.2 Selection of samples selected is representative of all the material on the
plant.
Samples shall be taken only from unbroken
packages or from undamaged units and, as far as 3.3 Size of sample
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
possible, they are to be representative of each The sample will vary in size according to the
material in the consignment. number of tests that are to be carried out, but it
Where the consignment comprises more than one should contain a sufficient number of units to
type of insulating material and/or more than one permit random selection of specimens for each test.
thickness or density, each type, each thickness and Although, statistically, the minimum size of sample
each density shall be treated as a separate required is not dependent on the size of the batch
consignment for the purposes of sampling, unless being sampled, it is usually convenient to base a
other arrangement is made between the purchaser sampling schedule to some extent on the size of the
and the vendor. consignment. Subject to there being a sufficient
Samples of materials consisting of relatively small number of specimens or bulk of material selected for
and similar units, e.g. insulating bricks, shall be the tests required, recommendations for sampling
obtained by random selection, preferably while the are detailed in Table 1.
consignment is being unloaded, as it is not 3.4 Specimens
practicable to ensure correct sampling from a
Specimens which are cut from larger units shall be
stock-pile of the units.
taken from an inner area of the unit, avoiding the
Samples of granular, powdered and plastic outer edges as far as possible. Unless otherwise
composition materials shall be prepared by specified both original faces of the unit shall be
withdrawing material from each container selected retained in each specimen and not more than one
for sampling: the material shall be taken after specimen for a given test shall be taken from each
emptying and thoroughly mixing the contents of the unit of the sample.
container. All the samples of one type (preferably
Table 2 is a guide to the number and size of
not less than 2 kg total) shall be thoroughly mixed
specimens required for the tests which are described
together and gathered into a conical heap which
in this standard. Each test is normally carried out
shall then be divided into quarters by vertical cuts. three times, and the individual results quoted.
Any two diametrically opposite quarters shall be
discarded and the two remaining quarters mixed
together and quartered as before. The process of
mixing, quartering, discarding and remixing shall
be repeated until a sample of size requisite for the
tests remains.
Table 1 — Sample sizes and rates of additional sampling
Minimum size
Material Rate of additional sampling
of sample
Small similar types of units, e.g. insulating 10 units 1 unit per 3 000 units above first 30 000 units
bricks and small blocks
Plastic composition, loose-fill granular and 2 kga 0.5 kg per 1 000 kg above first 5 000 kg
powdered materials
Other materials 5 units 1 unit per 200 units
a
Taken from a minimum of five containers, where possible.
2 © BSI 02-2000
BS 2972:1989
© BSI 02-2000 3
BS 2972:1989
Section 2. Dimensions
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
where these methods are impracticable, owing to
measurements of width may be called for and
size and nature of the insulating material and other
turning the material may be omitted.
difficulties, other methods may be agreed between
the manufacturer and the purchaser. Cut test samples under a template and check the
bottom face against the template for accuracy of
This section does not attempt to lay down tolerances
square cut edges. When cutting round the template
of manufacture of application; the tolerances quoted
take care to avoid any extrusion of the material from
are essentially those of measurement only.
the edges due to excessive pressure on the template.
5 Measurement before application Take measurements of length and breadth of the
template as in 5.1.2, but on one face only, and
5.1 Length and breadth of flat surfaces consider these measurements to be those of the
5.1.1 Apparatus sample.
5.1.1.1 Steel rule, graduated in millimetres. 5.1.4 Procedure for loose-fill materials.
5.1.1.2 Tee square Measurements of material as delivered are not
relevant. In the case of test samples, the length and
5.1.1.3 Template for cutting test sample, the size of breadth of the material correspond to the internal
which is dependent on the test for which the sample dimensions of the container used in the test.
is to be used. Measure the internal length and breadth of the
5.1.1.4 Container of constant cross section container and record the measurements taken.
throughout its height, to determine the volume of Measure the position where the insulating material
loose-fill materials, the dimensions of which being is levelled off and record the depth of material in the
dependent on the test for which the sample is to be container.
used (see 12.3). 5.2 Thickness of flat surfaces
5.1.2 Procedure for materials with clearly defined
5.2.1 Methods of measurement. Four methods are
edges. For rectangular surfaces, lay the material on
available for use in determining thickness. These
a flat plane and measure length and breadth by
are detailed in 5.2.3 to 5.2.6 and their applicability
laying a steel rule across the surface parallel to one
with respect to different types of material is given
edge and at right angles to an adjacent edge. Take
in Table 3.
measurements at three positions on one face for
NOTE These methods may be varied by agreement between the
both length and breadth, namely at about 10 mm user and the supplier in such details as the mass of the plate
inwards from each edge and across the centre. Turn in 5.2.3 or the load on the plate in 5.2.6.
the material over and repeat the measurements for 5.2.2 Apparatus
the opposite face, in all cases taking measurements
to the nearest millimetre. 5.2.2.1 Steel rule, graduated in millimetres.
Record the mean of the six representative 5.2.2.2 Thickness gauge, as shown in Figure 1 (for
measurements as the length and breadth of the use with the method given in 5.2.3). The apparatus
material. comprises three parts: a probe, a collar and
a 200 mm × 200 mm plate. The mass of the plate
For surfaces which are not rectangular,
and the collar together shall be such as to exert a
measurements shall be taken as appropriate.
pressure of 30 N/m2, i.e. 122 ± 1 g.
Cut test samples required for other tests in this NOTE This can be achieved by making the plate from 3 mm
standard to the specified rectangular size, with acrylic sheet and the collar of aluminium, as detailed in Figure 1.
square edges, preferably using a template. The plate may be made from other materials provided that it is
rigid and presents a flat, smooth, continuous surface to the
5.1.3 Procedure for materials with indeterminate insulation.
edges. Unpack and unroll materials which are 5.2.2.3 Straightedge (for use with methods given
compressed or tightly rolled during transit and in 5.2.4 and 5.2.6).
allow them to expand freely for 4 h before
measuring. 5.2.2.4 Callipers (for use with the methods given
in 5.2.5 and 5.2.6).
4 © BSI 02-2000
Table 3 — Methods of thickness measurement
© BSI 02-2000
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
Method to be
BS number Type of material Notes
used
BS 3958-1 Magnesia:
flat slabs 5.2.4 or 5.2.5
curved surfaces 5.2.5
BS 3958-2 Calcium silicate:
flat slabs 5.2.4 or 5.2.5
curved surfaces 5.2.5
BS 3958-3 Metal mesh faced man-made mineral fibre mattresses 5.2.6 Facing materials shall not be disturbed. Sample size to
be the same as plate
BS 3958-4 Bonded preformed man-made mineral fibre pipe sections 5.2.3
BS 3958-5 Bonded man-made mineral fibre slabs 5.2.3, 5.2.4
or 5.2.5
BS 5803-1 Man-made mineral fibre mats 5.2.3 Material shall be allowed to expand freely for 4 h
Compressible sheet materials 5.2.3 after unpacking or unrolling. Test area shall be not
less than 400 mm × 400 mm
Enclosed loose-fill materials 5.2.6 Enclosing material shall not be disturbed
All materials after application in even layers, including 5.2.3
unenclosed loose-fill materials
BS 2972:1989
5
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© BSI 02-2000
Figure 1 — Thickness gauge (continued)
BS 2972:1989
6
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© BSI 02-2000
Figure 1 — Thickness gauge (concluded)
7
BS 2972:1989
BS 2972:1989
5.2.2.5 Weighted plate (for use with the method 5.3 Volume of a flat shape
given in 5.2.6). Calculate and record the volume from the
5.2.3 30 N/m2 method. Place the sample (not less significant length, breadth and thickness
than 400 mm × 400 mm) on a plane, hard surface measurements obtained as in 5.1 and 5.2.
and lay the plate centrally on the upper surface of 5.4 Deviation from square of a board
the insulating material. Insert the probe with the
sliding collar through the hole in the centre of the 5.4.1 General. Methods are given for the
plate and push through the insulating material, determination of the deviation from square for the
normal to the principle surface, until its point thickness, width and length of boards that are
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
touches but does not penetrate the underlying plane nominally square.
surface. Hold the collar firmly to the probe by 5.4.2 Apparatus
pressure of the thumb in the position where it just
5.4.2.1 Steel square, with limbs of at least 500 mm
touches the upper surface of the plate and, after
in length.
withdrawal, measure the distance between the
point of the probe and the underside of the collar to 5.4.2.2 Steel tape or ruler, graduated in millimetres.
the nearest millimetre by means of a suitable rule. 5.4.3 Specimen. The specimen under test shall be a
Record the thickness of the material as this full board laid on a flat surface.
measurement minus the thickness of the plate. 5.4.4 Thickness deviation. Place steel square with
5.2.4 Straightedge method. Place the sample on a limbs longer than the board thickness on the flat
plane surface and lay a straightedge across the face surface against one end of the board as shown
of the material in three positions parallel to one in Figure 2(a). Using a steel tape or ruler, take
edge of the material and at distances from the edge measurements to the nearest millimetre around the
of one-sixth, half and five-sixths of the length of the edge corners of the board.
adjacent edge. Determine the thickness by The deviation from square is the distance between
measuring with a steel rule the distance between the edge corner of the board and the edge of the steel
the plane surface and the straightedge at both edges square at the point of greatest deviation (A).
of the slab. Repeat measurements for the three
Report the deviation in millimetres.
positions of the straightedge at right angles to the
initial set. Read measurements to the nearest 5.4.5 Width or length deviation. Place a steel square
millimetre and record the thickness as the mean of along one of the parallel sides of the insulation with
the 12 measurements. the right angle of the square aligned against the
adjoining edge as in Figure 2(b). Using a steel tape
5.2.5 Calliper method. Rule the sample of material
or ruler measure the distance (C) between the edge
into nine rectangles of equal area. Apply callipers at
of the board and the edge of the square at each
the centre of each area, taking care not to penetrate
corner and determine the greatest deviation (C). B is
the surfaces. Take measurements to the nearest
the distance over which the deviation is measured
millimetre and record the thickness as the mean of
[see Figure 2(b)].
nine measurements.
Calculate and report the deviation from square as
5.2.6 Weighted plate method. Place the specimen on
millimetres gap per 100 mm of width or length.
a plane surface and subject it to a pressure
of 725 N/m2. A flat, stiff plate measuring at 5.5 Length and circumference of curved
least 200 mm × 200 mm may be used for this. The shapes
specimen size is to be the same as the plate size. 5.5.1 General. This sub-clause applies to materials
Determine the combined thickness of the specimen of regular curvature in one direction only, this
and plate by the use of a straightedge (see 5.2.4). curvature being built into the material so that
Determine the thickness of the plate by callipers before application it conforms without change of
(see 5.2.5) and record the thickness as the difference shape to the surface it is intended to fit, e.g. circular,
between these two measurements. semi-circular and segmental pipe sections, radiused
NOTE A plate measuring 200 mm × 200 mm and weighing or and bevelled lags. It does not apply to flexible
loaded to weigh 2.96 kg exerts a pressure of 725 N/m2. The shapes which when not applied will lie flat, or to
methods appropriate to the different types of material are listed
in Table 3. special shapes such as hemispheres, domes or
dished shapes etc.
When the thickness of an insulating material after
application in an uneven layer (e.g. plastic
compositions “finger-marked”) is to be determined
and it cannot be measured by any of the methods
described in 5.2 the methods described in 6.2.2
and 6.5.2 shall be used.
8 © BSI 02-2000
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI BS 2972:1989
© BSI 02-2000 9
BS 2972:1989
5.5.2 Length. Take length measurements along the 6 Measurement after application
straight dimension by laying a steel rule along this
6.1 Length and breadth on flat surfaces
direction at four positions equally spaced around the
outside circumference in the case of completely Measurement of length and breadth after
circular sections, and at two positions for each application is not normally required in situ (except
semi-circular or segmental section or lag, or similar. as indicated below). If specimens can be removed,
Repeat the measurements for the inner surface, the length and breadth can be measured by any of
i.e. inside the bore of the section or on the other face the methods outlined in 5.1.
of the lag. Read measurements to the nearest The process of removal may result in a break-up of
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
millimetre and record the length as the mean of the the specimen, preventing length and breadth
measurements taken. measurement after removal. In this case, mark off
5.5.2 Circumference or breadth. Measure the the applied material into an area not less
circumference, part circumference or breadth by than 0.1 m2 before removal, the developed area
laying a flexible steel rule in close contact with the being as far as possible rectangular and of sides as
surface. Take measurements at three positions on far as possible dimensionally similar. Measure the
the external face and three positions on the internal length and breadth between the markings by means
face, namely, at about 10 mm inwards from each of a steel rule as in 5.1.2, but on one face
end and in the centre. In the case of completely (i.e. exposed insulation face) only. Record the length
circular sections the internal centre measurement and breadth as the mean of these three respective
may be omitted. Read measurements to the nearest measurements.
millimetre. Record the mean of the external If it is not found possible to remove the marked area
measurements as the breadth or circumference over accurately trim the sides until an approximately
the external curved surface and the mean of the rectangular hole is obtained and the length and
internal measurements as the breadth or breadth of the hole measured as above.
circumference over the internal curved surface.
6.2 Thickness on flat surfaces
5.6 Thickness of a curved shape
6.2.1 Even layers. Where the surface is sufficiently
Thickness should preferably be measured by means uniform, thickness shall be measured by means of a
of a probe and collar, (see 5.2.2.2 and Figure 1). Fit probe and collar as specified in 5.2.2.2. Insert the
the material over a hard surface of radius equal to probe from the outer face only and record the
or less than the internal radius of the material and thickness as the mean of the nine measurements.
push the probe radially through the insulation from
6.2.2 Uneven layers. When the applied insulating
the external surface until the point is in contact material has an uneven surface, its thickness
with the hard surface lining held in close contact cannot be satisfactorily measured by the methods
with the internal surface of the insulation. Measure
already described. The most usual example of this is
the thickness from the probe setting as in 5.2.3.
when plastic composition is left “finger-marked”
Divide the material along its length into three equal ready for the addition of a layer of some different
distances and take thickness measurements to the material. In such cases determine the average
nearest millimetre at the centre of each division at thickness by measuring in situ the length and
three positions equidistant around the breadth of a marked off area of minimum 0.1 m2,
circumference or part circumference. then carefully remove all the material in this area
Record the thickness as the mean of the and weigh the material removed. The bulk density
measurements taken. of the material is determined as in section 3 and the
Thickness shall not, unless required otherwise, average thickness calculated from the following
include the thickness of any external covering. equation:
Alternatively, take thickness measurements by 1000 m
L = -------------------
means of suitable callipers at positions outlined ÔA
above. Where measurements at the centre are not
where
possible due to the length of the calliper arms other
positions may be chosen. L is the average insulation thickness (in mm);
5.7 Volume of a curved shape m is the mass of insulation removed (in kg);
Calculate and record the volume as the product of Ô is the bulk density of insulation (in kg/m3);
the mean length, the mean of the breadth of the
A is the area of insulation removed (in m2).
internal and external curved surfaces, and the
thickness, as measured in 5.5 and 5.6.
10 © BSI 02-2000
BS 2972:1989
6.3 Volume applied on flat surfaces If the circumference is less than the values given in
The volume shall be recorded as the product of the column 2, the insulation shall be completely
mean length, breadth and thickness as measured removed from a 250 mm straight length of pipe (in
in 6.1 and 6.2 above. this case ignoring the minimum 0.1 m2 area earlier
specified) and the following equation used:
6.4 Length and circumference on curved
surfaces
Measurement of length and circumference after
application is not normally required in situ (except where C1 is the external circumference of the pipe
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© BSI 02-2000 11
BS 2972:1989
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
e) blown materials. 9.1 Specimens
Some insulating materials may be provided in Flat specimens should be not less than 0.05 m2 in
composite form with a surface finish or protective area or, failing this, the largest size available. Pipe
covering which is substantially different in sections shall be not less than 250 mm in length.
composition from that of the insulating material
9.2 Determination of dimensions
itself. Thus, it is common practice for flexible
materials to be enclosed in galvanized wire netting, Each sample shall be measured by the methods
expanded metal, cloth etc., while flexible or specified in section 2.
preformed insulating materials may have a surface 9.3 Calculation of results
finish of man-made mineral fibre tissue, board or
The bulk density (Ô)in kg/m3 shall be calculated
sheet material to facilitate handling or to provide an
abrasion resisting surface. Normally, the from the equation.
contribution of this surface sheet to the thermal a) For flat specimens
characteristics of the insulating material is m
negligible. Its mass shall therefore be omitted from Ô = -----------
abL
bulk density figures referring to the insulating
material. where
Alternatively it may be desirable to know the total m is the mass of test specimen (in kg);
mass of the complete assembly of insulating a is the length of specimen (in m);
material together with the surface finish; this shall
be given in terms of mass per square metre or, for b is the width of specimen (in m);
pipe insulation, mass per linear metre, as a L is the thickness of specimen (in m).
supplementary figure to the bulk density of the
insulating material alone and such a figure shall be b) For pipe sections (complete cylinder):
accompanied by the corresponding total thickness of 2m
Ô = -----------------------------------------
the composite insulation. Ï aL ( d 1 + d 2 )
The test for bulk density shall be carried out on the
material as ready for application in the case of where
preformed and flexible materials. It is m is the mass of specimen (in kg);
recommended that the packing density of loose-fill a is the length of specimen (in m);
materials be determined after application and bulk
density of blown materials determined after the L is the thickness = " (d2 – d1), (in m);
material has been blown through a suitable blowing d1 is the internal diameter (in m);
unit. In the case of plastic composition materials,
the test shall be carried out on the material after d2 is the external diameter (in m).
mixing the water, applying either to a test plate or
to a portion of the plant, and drying. The amount of 9.4 Expression of results
water used for mixing shall be noted as a percentage The results of the test shall be expressed in kg/m3. If
of the weight of the material. required, the moisture content shall be given as a
Where required by the purchaser or supplier, the percentage of the dry mass.
moisture content at the time of test shall be stated
(see section 11).
In every case, three specimens shall be tested and
the result expressed as the average of three tests.
12 © BSI 02-2000
BS 2972:1989
© BSI 02-2000 13
BS 2972:1989
The average bulk density may be deduced from the 12.3.2.2 Procedure. Mount the measuring cylinder
total volume of a section of insulation and the mass on the table of the apparatus, fill to the 25 mL mark,
of insulating material that has been put into it. This drop ten times at 5 s intervals and determine the
may be misleading since it takes no account of level of the powder. Weigh the powder.
possible variations in the degree of compression 12.3.3 Other materials
throughout the section. It is therefore desirable to
test at a number of points in a given section of 12.3.3.1 Apparatus
insulation. If this is done after the installation has 12.3.3.1.1 Box, 200 mm × 200 mm × 250 mm high.
been completed, as is preferable, it is generally
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
12.3.3.1.2 Straightedge
necessary to remove part of the containing
12.3.3.1.3 Means of weighing the sample.
structure, such as a panel, so that the insulation
from a measurable volume can be removed and 12.3.3.2 Procedure. Fill the box by allowing the
weighed. material to fall evenly and loosely into it from a
height of 150 mm above the upper edge. When the
The procedure for removing the insulation, and the
container is full, smooth the surface off with a
accuracy with which the volume of space from which
straightedge and drop the box ten times from a
it is removed can be determined, depend upon the
distance of 25 mm onto a hard surface. Determine
nature of the material and upon the site. A coherent
powder can fairly easily be divided from the the level of the upper surface of the material below
surrounding material and removed without the edge. Weigh the contents of the box.
disturbing the latter. Fibrous materials are not so 12.3.4 Expression of results. The results of the tests
easily separated and therefore reasonably large carried out in 12.3.2 and 12.3.3 shall be expressed
amounts should be removed so as to reduce the ratio in kg/m3. If required, the moisture content shall be
of edge to area. The controlled removal of freely given as a percentage of the dry mass.
flowing granules from a vertical cavity is likely to be 12.3.5 Determination of the loose bulk density
difficult and their subsequent replacement may be and the bulk density
impracticable.
12.3.5.1 General. The object of the test given
If access can be gained to a horizontal space, in 12.3.5.3 is to determine the loose bulk density of
however, it may be possible to press into the the insulating material and also the bulk density
material a light sheet metal frame from within after a specified regime of compaction. It is
which the granules can be removed. Variations of applicable to powders and granular materials.
the above methods should be devised to suit the
particular material and site. 12.3.5.2 Apparatus
If it is impracticable to test after the insulation is 12.3.5.2.1 500 mL graduated plastics measuring
complete, the less desirable course may be adopted cylinder of known mass.
of removing samples of material as the work 12.3.5.2.2 The apparatus shown in Figure 4. This is
proceeds. The general principles are much the same provided with a platform which can be
as those outlined in the preceding paragraph. raised 19 mm by a motorized cam and then allowed
12.3 Bulk density of powdered and granular to fall onto a 6.3 mm thick pad of flexible closed pore
materials before application expanded PVC (not shown in Figure 4). The cam is
driven at 15 ± 1 r/min by a geared induction motor.
12.3.1 Indication of bulk density. An indication of
12.3.5.2.3 Means of weighing the sample.
the bulk density of the material may be obtained by
using one of the procedures given in 12.3.2, 12.3.3 12.3.5.3 Procedure, Using a scoop, transfer material
or 12.3.5. from a coned sample, tipped from its packed or other
container, into a cylinder held at approximately 45°
12.3.2 Material passing an 850 Èm nominal
to the vertical which is slowly rotated. Fill the
aperture BS 410 test sieve
cylinder to the 500 mL mark, weigh the cylinder
12.3.2.1 Apparatus and its contents and determine the mass of the
12.3.2.1.1 Measuring cylinder of 25 mL capacity. specimen, m (in kg) by deducting the weight of the
cylinder.
12.3.2.1.2 Apparatus which can raise the cylinder
through a distance of 5 mm by means of a cam Place the cylinder and contents onto the platform of
(see Figure 3). the apparatus, close the cover plate by means of the
wing nuts and run the motor of the apparatus for a
12.3.2.1.3 A means of weighing the sample.
specified time, (e.g. for 20 min or until no further
settling appears), after which read the new
(compacted) volume, V (in litres) of the specimen
from the cylinder graduations.
14 © BSI 02-2000
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI BS 2972:1989
© BSI 02-2000 15
BS 2972:1989
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
Figure 4 — Alternative apparatus for determining bulk density of powders
16 © BSI 02-2000
© BSI 02-2000
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
Figure 5 — Apparatus for determining bulk density of powder and granular insulating materials after attrition
BS 2972:1989
17
BS 2972:1989
12.3.5.4 Expression of results. The loose bulk A mass of material shall be determined from the
density shall be given by 2m kg/L. equation:
The compacted bulk density shall be given by m = ÔV
m/V kg/L. where
The mean of two determinations shall be quoted in m is the mass of material (in kg);
each case.
Ô is the preselected bulk density (in kg/m3);
12.4 Test for bulk density of powder and
granular insulating materials after attrition V is the volume of the container (in m3).
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
12.4.1 Object. The object of the test is to determine The material shall be uniformly packed by hand in
the change in bulk density produced by a specified convenient increments into a box of known
regime of oscillatory movement of the material. It is dimensions, e.g. a 300 mm cube. The investigation
particularly applicable to insulation materials will indicate whether or not the loose-fill material
composed of expanded minerals. can or cannot be packed at the preselected bulk
12.4.2 Apparatus density.
12.4.2.1 Apparatus as shown in Figure 5, consisting
of two cylindrical vessels 111 mm i.d. × 340 mm
13 Blown materials
long closed at both ends and mounted on a common 13.1 General
shaft rotatable at 30 r/min by an induction motor. The installation of blown insulation requires a
12.4.2.2 3 L graduated glass vessel with flat base knowledge of the bulk density of the material after
which can be mounted on the bulk density passing through a blowing machine. A test
apparatus of the previous test, shown in Figure 4. procedure is described which is suitable for use with
12.4.3 Procedure a commercial insulation blowing machine.
12.4.3.1 Preparation of specimen. Prepare the 13.2 Apparatus
specimen by putting such a quantity of insulating 13.2.1 Commercial blowing machine
material into the 3 L glass vessel that after 13.2.2 Open-topped collection box constructed
compaction on the apparatus of the previous test from 10 mm thick plywood with internal
(see Figure 4) for 40 s the volume is 2 760 mL. measurements of 600 mm × 300 mm × 100 mm
Prepare two such specimens, one being transferred deep. The top edges of the box shall be smooth and
to each of the cylinders which shall thus be filled in the same plane.
to 85 % of its capacity at the compacted bulk 13.2.3 Measuring device, constructed as shown
density. Close the cylinders. in Figure 6.
12.4.3.2 Testing. Rotate the cylinders continuously
13.3 Procedure
for 48 h after which return the contents of each
separately to the 3 L glass vessel, compacted Carry out the procedure as follows.
for 40 s and measure the new volume V. a) Make positioning marks on the top of the
12.4.4 Expression of results. The result shall be collection box such that the rule carried by the
expressed as the percentage reduction in the measuring device may be located over the
volume, i.e.: principal axis of the box at six points:
50, 150, 250, 350, 450 and 550 mm (measured
2760 – V
100 × ----------------------- from one end).
2760
b) Weigh this box to the nearest 10 g and place it
quoted as the mean of that for the two cylinders.
on a level floor surface.
12.5 Packing test for loose-fill materials c) Position the measuring device at each of the six
The density of loose-fill materials is dependent upon locations pre-marked on the top of the collection
the compression applied during packing and the box, with the inside edge of its feet aligned with
procedure described in 12.3 is not always the inside faces of the box.
appropriate, particularly for fibrous or cellular d) Take readings by pushing the rule gently
materials. When it is desired to determine if a downwards until its end contacts the floor of the
sample of the material can be packed at a collection box with the rule vertical.
preselected bulk density, a convenient method is as
follows.
18 © BSI 02-2000
BS 2972:1989
e) With the blowing nozzle of the commercial unit 13.4 Expression of results
held horizontally and approximately 1 m above Determine the mass of insulation material used to
the floor, blow the fibre into the box to a depth fill the box (in kilograms) from the difference of the
marginally above 100 mm and such that a masses obtained in b) and f). Determine the initial
sensibly smooth and level surface is obtained. thickness of material blown into the box as the
Carefully remove any material resting on the top arithmetic mean, to the nearest millimetre, of the
edges of the box. difference between the pairs of readings taken at
f) Weigh the filled collection box to the each of the six locations in d) and g).
nearest 10 g. Calculate the density Ô of the insulation (in kg/m3)
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
g) Take readings with the measuring device used to fill the collection box using the following
positioned as in Figure 7(c) by pushing the rule equation:
gently downwards until its end contacts the
m
Ô = --------------------------
surface of the insulation with the rule vertical.
0.00018 L
where
m is the mass of the insulation (in kg);
L is the thickness (in mm).
© BSI 02-2000 19
BS 2972:1989
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
Figure 7 — Top views of vibration boxes: showing positions for height measurements
20 © BSI 02-2000
BS 2972:1989
ambient temperatures. Æ
µ = ------
Ôc
Method 610 of BS 1902-6 is applicable to ceramic
fibres and some other fibrous insulating materials where
used at elevated temperatures. The method given in µ is the thermal diffusivity (in m2/s);
ASTM-C351-82 is also suitable for materials used in
hot conditions. 2 is the thermal conductivity [in W/(m.K)];
Results should be expressed in J/(kg.K). Ô is the bulk density (in kg/m3);
c is the specific heat capacity [in J/kg.K)].
NOTE Thermal diffusivity can be calculated from the
conductivity, density and specific heat capacity as shown by the
above expression or, alternatively, it can be determined
experimentally. There are several experimental methods
available for the direct determination of thermal diffusivity but
at present there is no standard method for measuring this
quantity in the sense that the guarded hot plate apparatus is
regarded as standard for the determination of thermal
conductivity.
© BSI 02-2000 21
BS 2972:1989
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
18 Assessment of self heating hazard surface, to the required test temperature whilst
covered with a pack of insulation of the thickness
18.1 General and bulk density required for the actual test.
Some insulation materials which contain organic Meanwhile prepare the actual test pack, this being
matter, e.g. as bonding material, although suitable of the same surface dimensions as the hot plate and
for the service temperatures anticipated, may, in of the full thickness and bulk density ultimately to
fact, constitute a fire risk under certain conditions, be used. Not less than three thermocouples shall be
e.g. through the incidence of welding sparks, or positioned within a radius of 25 mm from the centre
through an internal self heating phenomenon. of the pack in a horizontal plane. This is aided if the
Evidence of this internal self heating may be a pack can be split open along a mid-plane.
transient rise in temperature above the theoretical When the hot plate has reached a steady state
value within the insulation. If excessive, this rise within ± 2 % of the required test temperature,
may present a hazard. Manufacturers normally quickly remove the insulation on the hot plate and
state the limiting temperature of use and the replace with the prepared test pack.
limiting thickness (if one applies) that may be used
The temperatures are recorded as follows:
at that temperature. The purpose of the tests in 18.2
and 18.3 is to ensure that the degree of self heating a) until those of the mid-position thermocouples
does not exceed safe limits. They differ from each have passed or reached their maximum value and
other as follows. do not vary by more than 2 % of the hot face
temperature in 1 h when the recorded
The test described in 18.2 applies to the thickness,
temperature shall be taken as steady;
bulk density and the maximum hot-face
temperature that may be attained during intended or
use. Accidental overheating from external sources, b) for 16 h;
e.g. welding sparks, is excluded from the test. whichever is the longer.
The test described in 18.3 intentionally utilizes NOTE It is recommended that duplicate test packs be tested.
excessive over-heating to well beyond the Each individual result, together with the average of these
recommended maximum service temperature of a results, should be quoted in the report.
material to instigate any self heating which may 18.2.3 Test criteria. The material shall be deemed to
subsequently occur. be satisfactory at the temperature, bulk density and
thickness used in the test if the following conditions
These tests are intended to refer to homogeneous
insulating materials excluding added facings. are satisfied:
If there is a danger of the emission of noxious gases, a) there shall be no sign of flame or glow from the
stack during the test;
the test should be carried out under conditions of
adequate ventilation. b) there shall be no visible collapse or fusing of
the interior when the stack is dismantled;
18.2 Self heating test: hot plate test
c) at no time during the test shall the average
18.2.1 Apparatus mid-position temperature exceed the hot surface
18.2.1.1 Hot plate of minimum temperature.
size 300 mm × 300 mm if materials of total In the event of self-heating (see 18.1) the record of
thickness not exceeding 100 mm are to be tested, or the mid-position thermocouples will show a peak,
of minimum size 450 mm × 450 mm if the test and then will decline, tending towards a steady
thickness exceeds 100 mm. For thicknesses greater value. Criterion c) above shall apply to the
than 300 mm consideration should be given to a mid-point temperature at all times during the test.
larger plate.
In all cases the hot plate shall be positioned
horizontally and be capable of being controlled to
within ± 2 % of the predetermined temperature.
22 © BSI 02-2000
BS 2972:1989
18.2.4 Test report. The test report shall include the 18.3.4 Procedure. Uniformly heat the bolt to more
following data: than 900 °C. Observe the temperature of the bolt as
a) the type, designation and grade of the material it cools in air free of draughts.
tested; Insert the bolt between the two specimens as its
b) the bulk density of the material at the start of temperature reaches 900 °C. Place a steel
the test; plate (3 mm thick and 300 mm2) on top of the
sample so that its weight ensures good contact
c) the applied thickness of insulation;
between the two specimens. Take readings of all the
d) the temperature of the hot face during the test; thermocouples at intervals of not more than 5 min
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
e) the maximum temperature reached at the for the first 2 h and 10 min thereafter. Continue the
mid-point during the test. test until all thermocouples have cooled to 200 °C or
18.3 Self heating test: hot bolt test less after passing through a maximum temperature,
or until it is indicated that the material has failed to
18.3.1 Sample preparation. Two specimens of the pass the test.
material, each 300 mm × 300 mm × 150 mm, shall NOTE It is recommended that duplicate samples be tested.
be prepared so that when placed one on top of the Each individual result, together with the average of these
other they form a sample or test piece consisting of results, should be quoted in the report.
a 300 mm cube. Each specimen may be formed of 18.3.5 Test criteria. In order to pass the test the
several layers and the sample shall be material shall satisfy the following conditions:
representative of the material as a whole. a) there shall be no indication of flame or glow on
18.3.2 Bolt specification. The “bolt” shall be a steel the exterior of the cube during the test;
cylindrical block 36 mm in length and 32 mm in b) the bolt temperature at any reading shall be
diameter, and weighing approximately 225 g. not greater than at any previous readings, but
If the material to be tested is rigid or semi-rigid, readings during the first 5 min shall be ignored;
hollows to fit the bolt shall be cut out from the centre c) none of the three thermocouples at the sample
of each specimen so that when the bolt is placed in interface shall indicate a temperature of more
the centre of the sample, good contact shall be than 10 °C above the temperature of the bolt at
retained between the two adjacent interfaces of the that time.
specimens.
NOTE With fibrous insulating material of low bulk density, or
18.3.3 Temperature measurement. Three with material which may tend to soften at the temperature
thermocouples shall be positioned on the top surface involved, it may be found that the bolt sinks downwards into the
sample. Note should be taken of any such displacement when the
of the bottom specimen. These shall be positioned results of the test are assessed.
at 25 mm, 50 mm and 75 mm from the edge of the
bolt. A thermocouple shall be securely attached to
the bolt. The thermocouples shall be chromel/alumel
with elements of approximately 0.5 mm diameter. It
may be found most convenient to use thermocouple
wire 1 m long and short lengths of ceramic beading
to allow greater flexibility.
© BSI 02-2000 23
BS 2972:1989
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
of certain materials can assume greater importance than heat NOTE Where there is a danger of degradation due to thermal
resistance as defined by conditions of test given in this section. shock, the specimens should be allowed to cool initially in the
BS 903-A19 specifies an ageing test conducted in an air oven furnace.
for 168 h at 70 ± 1 °C.
22.2 Inspection and testing of specimens after
20 Apparatus heating
A furnace or oven having a cavity size sufficient to Inspect and test the specimens as follows.
accommodate at least two test specimens a) The specimens shall be weighed and examined
measuring 100 mm × 100 mm × 50 mm and two visually for cracking and distortion immediately
shielding specimens of similar size spaced so as to after removal from the desiccator.
allow a clearance of at least 10 mm on all surfaces of b) The dimensions shall then be redetermined
every test specimen. The temperature of the furnace without delay in accordance with the procedure
shall be controlled to within ± 1 % of the desired given in clause 21.
temperature.
c) The specimens shall be subjected to a
compression test either immediately after
21 Preparation of test specimen measuring or later provided that they are stored
Test specimens measuring 100 mm × 100 mm × in a desiccator. The tests shall be conducted as
50 mm maximum thickness shall be cut from a given in section 7 of this standard except that the
sample leaving at least one of the original principal conditioning procedure shall be omitted.
faces of the insulation. The length, width and NOTE It is a requirement of this section that the resistance to
thickness of each specimen shall be measured compression of unheated material should also be determined. It
accurately using a calliper gauge which can be read is essential that the specimens for both tests be cut from the same
samples.
to 0.1 mm and they shall be dried in a ventilated
oven at 105 °C to 110 °C to constant mass. 23 Expression of results
22 Procedure Results shall be reported as follows.
22.1 Heating of specimens a) Average percentage change of length, width,
thickness, and volume of the specimens.
Place the specimens in the furnace at a temperature
b) Percentage change (positive or negative)
not exceeding 100 °C. Arrange them face to face
between the average dry mass of the specimens at
resting vertically on their edges on at least three
ceramic supporting bars and separated from each the commencement of the test and the
other by a distance of at least 10 mm. The corresponding average dry mass after the test.
supporting bars shall be of such a size that the c) Details of compression resistance as
specimens are at least 10 mm above the base of the determined in section 7 of this standard on
furnace cavity with a clearance of at least 10 mm unheated material and the corresponding details
above them. of compression after heating.
Place shielding blocks of calcium silicate insulation d) Any visible signs of cracking or distortion of the
with similar dimensions to the test specimens in the specimens both before and after heating.
furnace at each end of the group of specimens as
protection against direct radiation from the furnace
cavity walls.
24 © BSI 02-2000
BS 2972:1989
© BSI 02-2000 25
BS 2972:1989
26.4 Measurement of reduction in thickness The statement of results shall include details of the
The reduction in thickness shall be derived from the conditioning which the specimen has received, the
mean of four measurements taken near to the bulk density (see 25.6) and the nominal thickness.
vertical edges of the specimen or, if an automatic If failure of the specimen is observed during the test,
recording of thickness is being made the thickness the loading at which failure occurred shall be
should be noted from the record at convenient load recorded.
intervals.
27 Expression of results
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
The percentage reduction in thickness after
application of the load shall be derived from the
following expression which may be represented
graphically as a function of loading:
A–B
-------------- × 100
A
where
A is the initial thickness of the specimen
(see Table 5);
B is the thickness under load.
26 © BSI 02-2000
BS 2972:1989
© BSI 02-2000 27
BS 2972:1989
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
Figure 8 — Specimen mounting for interlaminar strength test
28 © BSI 02-2000
BS 2972:1989
29 Vibration at high frequency and 29.2.2 Procedure. Calculate the mean height of the
small amplitude specimen from measurements made at three points
as shown in Figure 7(a).
NOTE This test has been used mainly for assessing the
behaviour of mineral fibre and granular products for transport Place the lid on the box and vibrate the rig
service and may not be acceptable for other purposes. continuously for 16 h.
29.1 Apparatus Calculate the mean height of the specimen as above.
29.1.1 A wooden box with smooth interior 29.3 Loose fill materials
surfaces, having internal dimensions
29.3.1 Specimen. Apply the specimen to the box at a
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
© BSI 02-2000 29
BS 2972:1989
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
consisting of a 15 mm diameter hardwood dowel,
having at its lower end a 22 mm diameter mild steel
disc, 3 mm thick. The dowel is graduated in
millimetres.
To measure settlement involves gently lowering the
measuring rod so that it rests under its own weight
upon the surface of the material in the positions
described in 29.2.2, 29.3.2 or 29.4.2 as applicable.
30 © BSI 02-2000
31 Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
© BSI 02-2000
BS 2972:1989
BS 2972:1989
32 General When the mould is filled the surface of the mix shall
be lightly trowelled over to give a smooth finish.
The test for covering capacity involves the
Care shall be taken that undue pressure is not
preparation of a sample slab of a plastic composition
employed.
material under standardized conditions from a
known mass of dry material and determining the 34.3 Drying of specimen
dimensions. The specimen shall be dried in the mould to
NOTE A similar technique may be used for finishing materials constant mass at a temperature not
which are applied in the wet state except that a mould depth exceeding 110 °C. For this purpose, the mould may
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
of 13 mm may be used where this is appropriate.
be placed in a well ventilated oven or, alternatively,
over a hot plate.
33 Apparatus
If the manufacturer so recommends, specimens
33.1 Rigid mould, with one end open, for which shall be allowed to stand at room temperature for a
convenient internal dimensions specified initial setting period before drying at
are 450 mm × 300 mm × 50 mm deep. A piece of elevated temperature.
wood of dimensions
approximately 50 mm × 25 mm × 297 mm shall be 34.4 Removal of specimen from mould
a sliding fit within the mould walls to close the open After drying to constant mass, the specimen shall be
end. removed from the mould and its dimensions
The base of the mould may be of metal plate or of determined.
other non-absorbent smooth, flat material. The The length and breadth shall be measured in at
walls may be of angle section steel or of wood firmly least three places. The thickness shall be measured
secured to the baseplate by tap bolts or screws. by means of a depth gauge or suitable callipers in
NOTE The provision of wing nuts for securing the walls to the not less than nine different places, preferably at the
baseplate is of assistance for each removal of the specimen. intersection of lines of quadrisection.
33.2 Trowel
33.3 Steel rule 35 Expression of results
33.4 Depth gauge or probe Results shall be expressed as follows.
a) The wet covering capacity is expressed as
34 Procedure dbl –5
C w = --------- × 4 × 10
34.1 Preparation m
34.1.1 Preparation of the mix. Weigh the sample of b) The dry covering capacity is expressed as
plastic composition material as supplied and place
in a bucket or bowl. Mix water with the material in d ′ b ′l ′ –5
C d = -------------- × 4 × 10
accordance with the recommendations of the m
manufacturer. Take care not to over-work the mix. where
It may be necessary to carry out a preliminary test Cw is the wet covering capacity per 1 000 kg
to determine the mass of material to be taken. In the at 25 mm thickness
case of hydraulic setting cements the mass of the [in (m2/1 000 kg)/25 mm];
final dried block is greater than the mass of the dry
material used in the mix. Cd is the dry covering capacity per 1 000 kg
at 25 mm thickness
34.1.2 Preparation of the mould. The inside of the [in (m2/1 000 kg)/25 mm];
mould shall be lubricated or lined with polyethylene
film to prevent the plastic composition material d is the depth of mould (in mm);
sticking or drying and to facilitate removal of the b is the breadth of mould (in mm);
dried specimen.
l is the length of mould filled by sample
34.2 Application of the mix (in mm);
The entire sample of wet mix shall be trowelled into m is the mass of sample taken (in kg);
the mould. The mix shall be levelled off to the top of
the mould by means of a straightedge, and shall be d½ is the average thickness of dried sample
drawn towards the open end of the mould. The loose (in mm);
end-piece of the mould shall be adjusted to give a b½ is the average breadth of dried sample
rectangular shape of the specimen. (in mm);
l½ is the average length of dried sample
(in mm).
32 © BSI 02-2000
BS 2972:1989
© BSI 02-2000 33
BS 2972:1989
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
37.1 Number of specimens 39.4 Moisture content after conditioning at
The appropriate number of specimens shall be high humidity
taken as laid down in clause 3. Condition the dried specimen (see 39.1) to constant
37.2 Size of specimens mass in an atmosphere of 90 ± 5 % r.h. and
The specimens shall be of suitable size to allow at 20 ± 2 °C (see note to 39.2). Determine the mass
determination of the moisture content to of the specimens before and after conditioning.
within 0.5 % based on the dry mass of the specimen.
Each specimen shall weigh not less than 5 g. 40 Expression of results
The results shall be given as the moisture content
38 Preparation of test specimens expressed as a percentage by mass based on the dry
The determination of the moisture content shall be mass of the specimen or, alternatively, in terms of
conducted on specimens in a condition given by kilograms of moisture per cubic metre. If:
either or both of the following: m1 is the mass of specimen as received (in kg);
a) as received; m2 is the mass of specimen after drying to
b) conditioned to constant mass at 20 °C under constant mass (in kg);
one or more of the following conditions: low m3 is the mass of specimen after conditioning at
humidity, medium humidity and high humidity. the required humidity (in kg);
39 Procedure a1 is the moisture content as received (in % by
mass);
39.1 Moisture content as received
b1 is the moisture content after conditioning
Weigh the specimens as received and subsequently (in % by mass);
dry to constant mass. Determine the dry mass of the
specimen. a2 is the moisture content as received
For materials having a recommended upper (in kg/m3);
temperature limit of less than 120 °C, dry the b2 is the moisture content after conditioning
specimen in a desiccator. Where the upper (in kg/m3);
temperature limit is 120 °C or over, dry the
specimen in a ventilated oven at 105 °C to 110 °C. then:
39.2 Moisture content after conditioning at m1 – m2
low humidity a1 = ---------------------- × 100,
m2
Condition the dried specimens (see 39.1) to constant
mass in an atmosphere of 35 ± 5 % r.h. and m1 – m2
a2 = ---------------------- × bulk density as received,
at 20 ± 2 °C (see note). Determine the mass of the m1
specimens before and after conditioning.
m3 – m2
NOTE If a controlled humidity chamber is not available the b1 = ---------------------- × 100
required humidity conditions may be obtained approximately by m2
using an airtight vessel containing saturated solutions of salts.
Convenient salts with their corresponding relative humidity and
at 20 ± 2 °C are given below.
m3 – m
Sodium carbonate 90 %
b2 = ---------------------2- × bulk density as received.
Ammonium nitrate 65 % m1
Magnesium chloride 35 %
The temperature and relative humidity to which the
sample was exposed shall be stated.
2)
Available through the British Library Lending Division, Boston Spa, Wetherby, W. Yorks LS23 7BA.
34 © BSI 02-2000
BS 2972:1989
the report.
42.1 Number and size
43.3 Resistance to capillarity
The appropriate number of specimens shall be
taken as laid down in Table 2. Their size shall Place the specimens vertically on edge in tap
be 150 mm square and preferably not less water 6 mm to 10 mm deep containing 0.05 g/L of
than 25 mm thick. For the test for capillarity, the fluorescence indicator.
thickness shall be not less than 50 mm. NOTE It is convenient to use a water bath with an overflow
drain fixed at the required depth; it may be necessary to top up
42.2 Preparation of test specimens the bath with more fluorescence solution after the specimens
have been positioned to replace displaced water, and at intervals
Specimens shall be dried as in 39.1. during the test period.
Plastic composition materials shall be compounded Leave the samples standing in the fluorescent
with water, made into block form and dried before solution for 24 h.
being subjected to the test. Record to the nearest 1 mm, the depth of solution,
Loose, fibrous, granular and powdered materials do, in which the specimens are immersed.
shall be carefully and evenly packed to a specified At the end of the 24 h period, remove the specimens
bulk density into an open topped, perforated and examine each in ultraviolet light.
sheet-metal or gauze container,
measuring 150 mm × 150 mm × preferably 25 mm Record, to the nearest 1 mm, the maximum extent
internally, fitted with a lid of the same material. of fluorescence on each specimen, d1. Calculate the
mean value of the six observations.
43 Procedure 43.4 Drying after test
43.1 Partial immersion If desired, the specimens may subsequently be dried
to constant mass as specified in 39.1 and any
Suspend the specimen, prepared as in 42.2,
change in dimensions or condition reported.
vertically with one 150 mm × 25 mm side
immersed 6 mm below the surface of tap water
for 48 h. Maintain the water at constant level by
44 Expression of results
means of a slow constant feed and fixed overflow The results of the tests shall be expressed as follows.
pipe. a) The increase in mass expressed in kg of water
At the end of the period of immersion, suspend the per m2 of immersed horizontal surface (partial
specimen by one corner and allow to drain for 5 min. immersion), or per m3 of dry material (total
When applicable, wipe off the excess surface water immersion). For the capillarity test record the
with a dry cloth or remove by the careful application extent of capillary absorption for each specimen,
of blotting paper. Weigh the specimen immediately. d1 – d0, in mm and the mean extent of capillary
absorption for the six specimens in mm.
43.2 Total immersion
b) The bulk density of the specimen before
Completely immerse the specimen, prepared as testing.
in 42.2, in tap water for 2 h3). Immerse the
c) The condition of the specimen, particularly any
specimen horizontally, with the upper surface
signs of deterioration.
approximately 25 mm below the surface of the
water. Additionally, for the total immersion test, any
change in volume (increase or decrease) shall be
At the end of the period of immersion, suspend the
expressed as a percentage of the dry volume.
specimen by one corner and allow to drain for 5 min.
3) For materials used in low temperature insulation, the time of immersion shall be six weeks at 15 °C to 20 °C.
© BSI 02-2000 35
BS 2972:1989
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
When a thick specimen has to be tested and the standard atmosphere, or any of the units shown
apparatus of BS 3177 is unsuitable then reference in Table 6, the original test conditions shall be
should be made to method 8 of BS 4370-2 where a stated because the conversion factors to different
beaker test is specified (method for water vapour units are only applicable to the same test conditions.
permeability of expanded polystyrene).
46 Conversion of units
If it is desired to express the results normalized to a
standard atmosphere this can be calculated from a
knowledge of the vapour pressure at each of the test
conditions.
Temperate 25 °C and 75 % r.h. = 0.0234
atmospheres
Tropical 38 °C and 90 % r.h. = 0.0588
atmospheres
36 © BSI 02-2000
Table 6 — Water vapour permeance conversion factors
© BSI 02-2000
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
g/(s · MN) g/(cm2 · s · mbar) g/(m2 · 24 h · mmHg) lb/(ft2 · h · atm) gr/(ft2 · h · mbar) gr/(ft2 · h · inHg) Temperate Tropical
(see note 2) (see note 4) = 1 perm g/(m2 · 24 h) g/(m2 · 24 h)
g/(s · MN) 1 1 × 10–8 1.152 × 10 7.471 × 10–2 5.161 × 10–1 1.749 × 10 2.052 × 102 5.149 × 102
g/(cm2 · s · mbar) 1 × 108 1 1.152 × 109 7.471 × 106 5.161 × 107 1.749 × 109 2.052 × 1010 5.149 × 1010
g/(m2 · 24 h · mmHg) 8.681 × 10–2 8.681 × 10–10 1 6.486 × 10–3 4.481 × 10–2 1.517 1.782 × 10 4.472 × 10
lb/(ft2 · h · atm) 1.339 × 10 1.339 × 10–7 1.542 × 102 1 6.909 2.339 × 102 2.747 × 103 6.896 × 103
(see note 2)
gr/(ft2 · h · mbar) 1.937 1.937 × 10–8 2.233 × 10 1.447 × 10–1 1 3.388 × 10 3.975 × 102 9.980 × 102
(see note 4)
gr/(ft2 · h · inHg) 5.719 × 10–2 5.719 × 10–10 6.590 × 10–1 4.275 × 10–3 2.951 × 10–2 1 1.174 × 10 2.948 × 10
= 1 perm
Temperate 4.874 × 10–3 4.874 × 10–11 5.613 × 10–2 3.641 × 10–4 2.515 × 10–3 8.514 × 10–2 1 See note 3
g/(m2 · 24 h)
Tropical 1.942 × 10–3 1.942 × 10–11 2.236 × 10–2 1.450 × 10–4 1.002 × 10–3 3.392 × 10–2 See note 3 1
g/(m2 · 24 h)
NOTE 1 To convert units in the first column to the units shown in the heading, multiply by the factor given at the intersection of the appropriate row and column.
NOTE 2 This was the term used by the building industry.
NOTE 3 No conversions from temperate to tropical are shown for the reasons given in clause 46.
NOTE 4 The symbol “gr” refers to grains.
BS 2972:1989
37
BS 2972:1989
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
48.1 Laboratory balance (accurate to ± 1 mg). sieve assembly on the shaker and allow to shake
48.2 Electric muffle furnace (temperature for 30 min. Inspect the material in the sieve;
controlled). continue shaking if necessary.
48.3 Silica or other suitable refractory basin (90 mm NOTE 1 Difficult material may benefit from hand teasing of
diameter × 35 mm deep approximately). remaining lumps. Small amounts should be brushed through
using a bristle sieve brush.
48.4 Sieve, 200 mm diameter, complying with Weigh the foil dish (48.7), then transfer the
BS 410: 250 4m aperture, receiver and lid. separated shot carefully from the sieve to the foil
48.5 Mechanical sieve shaker dish.
48.6 Three ceramic cylinders, 19 mm Reweigh the foil dish and shot.
diameter × 19 mm long, (see note 1 to clause 49). NOTE 2 Suitable ceramic cylinders are available from Royal
48.7 Aluminium foil dish or other suitable Worcester Industrial Ceramics Ltd. under the trade name
Regalox Cylpebs.
container, approximately 70 mm in diameter. NOTE 3 Heating mineral wools to a predetermined high
temperature aids the sieving process:
49 Procedure a) rock wools should be heated at a temperature of 600 °C
for 1 h.
Weigh the refractory basin (48.3). Cut a specimen of b) glass wools should be heated at a temperature of 500 °C for
approximately 10 g from the insulation, preferably at least 16 h.
from the full thickness, and place in the basin, then
weigh the basin and contents. 50 Expression of results
Results shall be expressed in the form:
mass of shot
Percentage shot = --------------------------------------------------- × 100
* mass of specimen
* Corrected if necessary for loss on ignition.
38 © BSI 02-2000
BS 2972:1989
51 General 53 Procedure
Though applied to the determination of oil in Weigh at least 15 g to the nearest 0.1 mg of dried
mineral wool, the result as here obtained may sample into the tared dry thimble ensuring that it is
include other soluble components, for example, well tamped down (see note 1). Extract with carbon
bitumen and certain resins. tetrachloride or other suitable solvent (see note 2).
If this is so and the oil alone is required, further Remove the thimble from the soxhlet extractor,
tests will be necessary. drive off the excess solvent in a suitable vented
oven, cool in a desiccator and reweigh.
52 Apparatus
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
© BSI 02-2000 39
BS 2972:1989
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
carbonates. The object of this method is to determine the
Where doubt exists concerning the value of the concentration of carbon in inorganic insulating
content of organic matter, it will be advisable to materials. This concentration is calculated from the
apply method 1 initially with one sample, followed mass of carbon dioxide produced when a known
by method 2 or 3 with a fresh sample, since if mass of insulating material is ignited in oxygen
method 2 or 3 were to be used initially with excess at 500 ± 50 °C. The method is applicable only to
carbonaceous material, a violent reaction could insulating materials with low concentrations
occur. (e.g. less than 1 %) of carbon.
57.1 Apparatus
56 Method 1. Determination of organic
NOTE The apparatus required is shown in Figure 10.
matter
57.1.1 Flowmeter (A).
By this method, both moisture and total organic
57.1.2 Bottle containing soda lime between two
material are normally determined. If, however,
layers of anhydrous magnesium perchlorate to
thermosetting resins in an uncured or partially
remove moisture and carbon dioxide from the
cured state are believed to be present, moisture
oxygen supply (B).
cannot be reliably estimated since in removing it the
resin will crosslink, giving rise to a change in mass. 57.1.3 Electric furnace with combustion tube having
Hence, in such cases the sample should be fully water cooled ends and a glass inspection inlet. A
cured at an appropriate temperature and time, plug of glass wool in the outlet retains solid
before any weighing is carried out. particles (C).
Apart from the foregoing case, any volatile organic 57.1.4 Bottle containing manganese dioxide to
materials will be represented in the result as remove sulphur dioxide formed during combustion
“moisture”. of sulphur compounds. The inlet and outlet
connections are ground glass fittings. They are held
56.1 Apparatus in place and a gas tight joint formed by covering the
56.1.1 Silica dish or other suitable container. surface with picien wax, not grease (D).
56.1.2 Coring tube, about 10 mm diameter (if used). 57.1.5 A tube containing anhydrous magnesium
56.2 Sampling perchlorate retained between plugs of glass wool to
absorb water produced in the ignition (E).
Representative material shall be used, obtained if
57.1.6 Bottle containing soda asbestos with a layer
necessary by taking corings through the whole
of anhydrous magnesium perchlorate, to absorb the
thickness of a mat or slab at representative points.
carbon dioxide. It is fitted with a one way stopcock
Other methods of cutting the sample may be used.
outlet, and is connected to drying tube E by means
56.3 Procedure of a rubber joint, the glass ends being pressed as
Weigh not less than 10 g of the sample to ± 0.01 g closely together as possible (F).
into a tared dry dish. Dry in a ventilated oven 57.1.7 Unglazed porcelain boats
at 105 °C to 110 °C for 40 min, cool in a desiccator 57.1.8 Balance capable of weighing the sample and
and reweigh. bottle (F) to 0.1 mg.
Ignite the sample in a muffle furnace at 550 ± 50 °C 57.1.9 Commercial oxygen in accordance with
for 10 min. Partially cool, for example on a BS 4364 to be supplied from a high pressure
heat-resistant mat, and then transfer to a cylinder through a suitable regulator.
desiccator. When cool, reweigh the sample.
56.4 Expression of result
The mass of moisture shall be obtained by difference
and shall be expressed as a percentage of the
original sample mass.
40 © BSI 02-2000
BS 2972:1989
a rate of 15 L/h for 12 min. Remove bottle F, water and/or carbonates. This concentration is
reweigh and reconnect, leaving the apparatus ready calculated from the difference between the mass of
for the next test. carbon dioxide produced when a known mass of
insulating material is ignited in oxygen
57.3 Results at 1 000 ± 50 °C (stage A) and the mass of carbon
Results shall be expressed as follows. dioxide produced when an equivalent mass of
insulating material is boiled in acid solution
( m 2 – m 1 ) × 12/4 4 × 100 (stage B).
a) Carbon, % = -----------------------------------------------------------------
S 58.2 Stage A
where 58.2.1 Apparatus. The apparatus used is shown
S is the mass of sample; in Figure 10 and consists of the items detailed
in 57.1.
m1 is the initial mass of bottle F;
58.2.2 Procedure. Weigh not less than 5 g of the
m2 is the final mass of bottle F. sample to ± 0.01 g into a tared dry dish. Dry in a
ventilated oven at 105 °C to 110 °C for 2 h, cool in a
b) If it is desired to express the carbon content in
desiccator and reweigh.
terms of the equivalent hydrocarbon, the
following equation may be used on the Bring the furnace to the operating temperature and,
assumption that carbon forms 85 % by mass of before the first test, pass oxygen through the
equivalent hydrocarbon. apparatus at a rate of 15 L/h for 20 min. Remove
bottle F, weigh and reconnect. Repeat until the mass
carbon % × 100 of the bottle is constant to 0.2 mg.
Hydrocarbon, % = ------------------------------------------
85 Place at least 0.5 g of the dried test material in a
= 1.176 × carbon % weighed combustion boat, weigh again and insert
into the hot part of the combustion tube. Pass
( m2 – m1 ) oxygen through at a rate of 15 L/h for 20 min.
= 32.07 × --------------------------- Remove bottle F, reweigh and reconnect, leaving the
S
apparatus ready for the next test.
© BSI 02-2000 41
BS 2972:1989
58.2.3 Results. Results shall be expressed as follows. The absorption tubes for CO2 are of the Midvale
Carbon and carbonates (expressed as carbon). Stetser-Norton pattern, and shall be carefully
( m 2 – m 1 ) × 12/4 4 × 100 packed. A thin layer of cotton-wool is placed at the
% = ----------------------------------------------------------------- bottom of the tube to prevent the end of the
S inlet-tube from becoming blocked with soda
where asbestos granules (14 mesh to 20 mesh). The tube is
then filled with soda asbestos granules (14 mesh
S is the mass of sample;
to 20 mesh) up to approximately the point where the
m1 is the initial mass of bottle F; inlet-tube passes through the wall of the body of the
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
m2 is the final mass of bottle F. absorption tube. Care shall be taken to ensure that
“channelling” does not take place between the glass
58.3 Stage B and the granules; this may be eliminated by tapping
lightly with the finger-nail while packing. Next is
58.3.1 Apparatus
placed a thin layer of cotton wool, followed by
NOTE The apparatus required is shown in Figure 11. anhydrous magnesium perchlorate to within 6 mm
58.3.1.1 U-tube containing soda asbestos to 3 mm of the neck, and the anhydrous magnesium
granules (14 mesh to 20 mesh) and anhydrous perchlorate is covered with a final layer of dried
magnesium perchlorate to remove CO2 from the air cotton wool.
entering the apparatus (A). The second absorption tube is to act as a guard, and
58.3.1.2 Reaction flask (B). to indicate when the first absorption tube is
58.3.1.3 5 % copper sulphate to remove H2S (C). beginning to fail. Both tubes are to be weighed in the
course of a determination.
58.3.1.4 Empty tube (D).
Ensure that all taps and joints are gas tight,
58.3.1.5 Flake calcium chloride to remove water
applying petroleum jelly where necessary.
(E and F).
58.3.2 Procedure. Transfer at least 0.5 g of the dried
58.3.1.6 Anhydrous magnesium perchlorate to
sample, accurately weighed, to the flask and cover
complete the drying of the gas (G and H).
with water. (It is convenient to use an amount of
58.3.1.7 Absorption tubes containing soda asbestos sample, if possible, which will evolve about 0.2 g
granules (14 mesh to 20 mesh) and anhydrous CO2.) Insert the stopper carrying the
magnesium perchlorate (I and J). dropping-funnel and condenser, and connect the
58.3.1.8 U-tube as in a) above and serving the same latter with C, D, E, F, G and H, but at present omit
purpose if air or moisture should travel back from the CO2 absorption tubes, connect H across to K by
the pump (K). inserting an empty U-tube. Connect A to the 2-way
58.3.1.9 Safety trap immediately before the filter tap of the dropping-funnel and pass air that is free
pump (L). from CO2 through the system for 5 min to 10 min (or
until it is judged that all CO2 has been removed from
Use is made of a Davies condenser of 140 mm
the apparatus). Close the stopcocks X, Y and Z in
nominal effective length and joint size either
that order, remove the empty U-tube between H and
B. 19/26 or B. 24/295) to condense most of the water K, and insert the weighed absorption tubes I and J.
and hydrochloric acid (if this acid is used).
5) See BS 5922.
42 © BSI 02-2000
43 Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI © BSI 02-2000
BS 2972:1989
BS 2972:1989
Prepare a quantity of concentrated phosphoric acid, 58.3.3 Results. Results shall be expressed as follows.
or dilute hydrochloric acid (1 : 1), approximately a) Carbonates, % (expressed as carbon)
equal to twice the amount theoretically necessary,
turn the tap water on for the condenser, running
this steadily, and nearly fill the dropping-funnel
with the acid; check again to see that incoming
CO2-free air is connected and instantly available. where
Now turn the stopcock in the dropping-funnel so S is the mass of sample (in g);
that acid runs down into the reaction flask B. This
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
m1 is the initial mass of absorption tube (I)
should be done slowly to prevent violent evolution of (in g);
gas; also the dropping-funnel should not be allowed
to empty completely, to avoid entraining air m2 is the final mass of absorption tube (I)
containing CO2 into the apparatus. (in g);
Immediately open the stopcock Y and then without m3 is the initial mass of absorption tube (J)
loss of time gradually open the stopcock X, and (in g);
see that the gas is bubbling steadily and m4 is the final mass of absorption tube (J)
consistently through the train. (The greatest speed (in g).
should be not more than two to three bubbles per
second.) The difference between the result obtained for
Continue with the addition of acid if necessary with stage A and that for stage B represents the
careful regulation, and then when all the acid has “organic carbon” content of the sample.
been used (except for a drop left to seal the b) If it is desired to express the carbon content in
dropping-funnel), turn the stopcock Z so that terms of the equivalent hydrocarbon, the
CO2-free air is feeding steadily through the train. following equation may be used on the
Light the burner under the reaction flask and slowly assumption that carbon forms 85 % by mass of
heat the reactants, keeping careful observation and the equivalent hydrocarbon.
control over the rate of flow of the CO2 through the carbon % × 100
train. Hydrocarbon, % = ------------------------------------------
85
Eventually, the system will come to a balanced
condition with the solution boiling gently in the = 1.176 × carbon %
flask.
When it is judged that all CO2 has been boiled out of
the solution in the flask, simultaneously decrease
the heat and increase the suction with a view to
keeping the gas flow rate reasonably steady until
the flame is removed altogether and the flask and
contents are cooling down. Continue with the air
flow until it is judged that all the CO2 has been
swept over to the absorption tubes containing the
soda asbestos granules (14 mesh to 20 mesh). Now
close the stopcocks X, Y and Z in that order, and
open the leading part of the system to atmosphere
by disconnecting the flask from its bung. Remove
the suction line.
Transfer the absorption tubes to the balance case
for 10 min and reweigh.
44 © BSI 02-2000
BS 2972:1989
59 General 61 Procedure
A test for air permeability is applied in order to give Pack the tube carefully with the calculated mass of
an indication of the relative air flow resistance to the insulating material, inserting small quantities
convection currents that are likely to occur within at a time to ensure uniform packing density. If the
the body of an insulant when it is applied to large tube is marked off in equal lengths, each section
vertical areas, for example, in the cold box of an air should be filled with a separately weighed quantity.
separation plant. The main object of the test is to Connect an air supply and measure the pressure
compare the behaviour of materials for use at very drop for a number of flow rates, the normal range
low temperatures, down to 90 K. being from 10 mL/min to 1 000 mL/min,
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
6) Separate flowmeters may be required to cover the range 10 mL/min to 1 000 mL/min with sufficient accuracy.
© BSI 02-2000 45
BS 2972:1989
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
Figure 12 — Apparatus for measuring air permeability of insulating materials
46 © BSI 02-2000
BS 2972:1989
© BSI 02-2000 47
BS 2972:1989
68 General A cover slip shall be placed over the drop and the
drop allowed to spread for 1 min before a little
The purpose of this test is to determine the mean pressure is applied to the centre of the cover slip.
fibre diameter of fibrous insulation products by
NOTE 1 A mounting medium of refractive index at least 0.03
optical means. less than that of the fibre is recommended. For most purposes a
mixture of equal volumes of analytical grade glycerol and
69 Apparatus distilled water will suffice.
NOTE 2 It is imperative that the sample bottle containing the
69.1 Optical microscope having a magnification fibre is shaken vigorously before the 0.01 g specimen is taken,
of × 1 000 and measuring graticule. and that the drop be taken from the suspension whilst it is still
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
in motion so that the fibres do not have time to settle.
69.2 Ultrasonic bath
69.3 Mounting medium 72 Measurement procedure
69.4 Microscope slides and covers Measure the diameters of the shortened fibres at a
magnification of 1 000 ± 100 using an eyepiece
70 Specimen preparation graticule. An example of such a device is the
The bulk sample of the material shall be “Walton-Beckett” graticule.
representative of the product, and bonded products Alternatively the images may be projected optically
shall be of the full original thickness. A specimen onto a screen or electronically onto a TV monitor,
shall be taken weighing approximately 10 g, and and a rule graduated in millimetres used for the
shall be cut through the full thickness of the measurement. An eyepiece graticule provides an
material at several places over the complete area of area, smaller than the total field of view, in which
the sample. A cork borer is a useful tool for cutting measurements are made. Such a defined area,
a specimen from bonded products. Specimens of smaller than the total field, which is projected on a
loose-fill totalling 10 g shall be taken from several screen, shall be approximately two thirds of the edge
places in bag or bale of this type of product. length or diameter (see Figure 13).
Any original binder in the specimen shall be Place the slide on the microscope stage and position
removed by ignition in a furnace. the stage so that the first area to be viewed is in
NOTE Rock wools should be heated at 600 °C for 1 h. Glass position 1 (see Figure 14). Measure the diameters of
wools should be heated at 500 °C for at least 16 h. all fibres in the defined area of the field, adjusting
The length of the fibres shall be reduced so that for the focus to scan through the-thickness of the
most of the fibres the whole reduced length is mounted specimen on the slide.
capable of being seen within the field of view of the When all the fibres in the field of position 1 have
microscope. been measured, move the stage to position 2. Space
One way of achieving this is by using a metallurgical position 2 five field diameters from position 1 to
press capable of applying a pressure of 30 MPa to avoid the possibility of double counting the same
a 25 mm diameter mould assembly. As much fibre. When all the fibres in position 2 have been
unbonded material as possible is placed in the measured move the slide systematically until 200
mould and a pressure of 30 MPa is applied for a fibre diameters have been recorded. The
period of 10 s. After crushing carefully, the material measurement rules are as follows.
is removed from the mould. a) A particle is regarded as a fibre in this test if
Whichever method of length reduction is employed, its length to diameter ratio is 2 : 1 or greater.
the shortened fibre shall be placed in a clean dry Particles with a length to diameter ratio of less
sample bottle fitted with a lid and large enough to than 2 : 1 are regarded as debris and ignored.
hold approximately 12 g of fibre. If necessary the b) All fibres with both ends within the defined
length reduction process shall be repeated until 6 g area are measured.
of fibre have been collected. The sample bottle shall
c) Fibres with neither end within the defined area
be shaken vigorously to mix the fibres.
are not measured.
71 Slide preparation d) Fibres with one end only within the defined
area are measured provided that the fibre crosses
80 mL of mounting medium shall be placed in the bottom or right hand side of a rectangular
a 125 mL beaker and approximately 0.1 g of the defined area or crosses the right hand half of the
fibre added. The beaker shall be placed in an circumference of a circular area. Fibres crossing
ultrasonic bath and the mounting medium stirred other parts of the boundary are not measured.
vigorously with a glass rod for 1 min. While the
NOTE These rules are illustrated in Figure 13.
mounting medium/fibre suspension is still in
motion, a drop shall be removed by means of the
glass rod and deposited on a glass microscope slide.
48 © BSI 02-2000
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
© BSI 02-2000
Figure 13 — Illustration of measurement rules
49
BS 2972:1989
BS 2972:1989
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
f is the number of fibres in that class;
N is the total number of fibres measured.
50 © BSI 02-2000
BS 2972:1989
© BSI 02-2000 51
BS 2972:1989
78.4 Conductivity of repeat extractions The results of each of the three measurements will
The extract prepared as described in 78.1 shall be then provide an indication of the efficiency of
re-extracted a second and a third time; the extraction; if a large discrepancy still exists between
conductivity of both these extractions shall also be the results of the second and third extractions, it
measured as in 78.2. will be necessary to proceed to even further
extractions until successive conductivity
measurements are sensibly constant.
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
52 © BSI 02-2000
BS 2972:1989
substantially in accordance with BS 2690-6, but solution to six one-mark volumetric flasks to 50 mL
with some modifications in the reagents. capacity.
b) Method 2. A polarographic titration method Add 4 mL of the 0.25 M solution of ferric ammonium
with amperometric indication. sulphate to each of the six samples, then add 4 mL
of the saturated solution of mercuric thiocyanate to
80 Method 1 each of the six samples. Dilute to the graduation
80.1 Apparatus for extraction mark with de-ionized water, and allow to stand
for 15 ± 1 min.
80.1.1 Standard soxhlet extractor as described in
BS 2071, with a flask and condenser of the requisite Measure the absorption of each of the ferric
size. thiocyanate complex solutions against the blank
sample at the peak absorption wavelength
80.1.2 Thimble complying with one of the following
(approximately 460 nm, but the exact wavelength
requirements7):
shall be checked for each spectrophotometer).
a) glass with a sintered base (grade 3 to 4);
Prepare a calibration curve for absorption versus
b) wholly sintered glass (grade 3 to 4); milligrams of chloride. This calibration covers the
c) cellulose8). range zero to 0.05 %.
80.2 Extraction procedure 80.3.4 Procedure B. Determination of chloride. By
means of a pipette, introduce 25 mL of the extract
Ensure that all apparatus is free from chloride and
solution into a clean one-mark volumetric flask
provide a supply of de-ionized water as described in
of 50 mL capacity.
BS 2690-6.
Add 4 mL of the 0.25 M solution of ferric ammonium
Accurately weigh about 5 g of the sample of
sulphate to the flask then add 4 mL of the saturated
insulating material into the extraction thimble.
solution of mercuric thiocyanate. Dilute to the
Extract until no further chloride can sensibly be graduation mark with de-ionized water and allow to
detected, using approximately 200 mL of de-ionized stand for 15 ± 1 min.
water. (An extraction time of about 5 h is normally
Measure the absorption at peak absorption
sufficient.)
wavelength against a freshly prepared blank
Transfer the extract to a standard 250 mL sample.
one-mark volumetric flask (see BS 1792) and make
Read off the chloride concentration from the
up to the mark with de-ionized water.
calibration curve.
80.3 Colorimetric estimation procedure Calculate the percentage chloride (Cl½) content
80.3.1 Apparatus. A visual range spectrophotometer based on the mass of the original sample of
is required. insulating material.
80.3.2 Reagents (analytical grades). The following 80.3.5 Method of calculation. If
reagents are required. x is the mass of original sample of insulating
a) Sodium chloride. material (in g);
b) 0.25 M ferric ammonium sulphate y is the mass of chloride as determined from
solution. (121 g ferric ammonium sulphate the calibration curve (in mg);
in 270 mL of concentrated nitric acid of relative F is the dilution factor (10 as above);
density 1.42). Dilute to 500 mL with de-ionized
water. then:
c) Saturated mercuric thiocyanate in 95 % 100 yF y
ethanol. content of chloride (Cl½) = ------------------- = --- %
1000 x x
7) See BS 1752.
8) Cellulose thimbles contain measureable amounts of chloride and thus in addition necessitate a blank determination.
© BSI 02-2000 53
BS 2972:1989
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
capacity. 81.3.3.2 Silver nitrate solution, 0.01N.
81.2 Extraction procedure 81.3.3.3 Sodium chloride solution, 0.1N.
Ensure that all apparatus is free from chloride and 81.3.3.4 Sodium chloride solution, 0.01N.
provide a supply of de-ionized water. 81.3.3.5 Nitric acid, 2N.
Accurately weigh 20 ± 1 g of sample into 81.3.3.6 Nitric acid, 1 : 1 (v/v).
the 1 000 mL flask. Add approximately 350 mL of
de-ionized water, connect the Dimroth condenser 81.3.3.7 Mercury (II) nitrate [Hg(NO3)2].
and boil under reflux conditions for 30 min. Allow to 81.3.3.8 Etching solution, 1.7 g [Hg(NO3)2] dissolved
cool to ambient temperature and transfer the in 50 mL 2N nitric acid.
extract to a 500 mL glass beaker. 81.3.3.9 Mercury (polarographic quality).
Acidify the extract by adding 1 mL of 1 : 1 nitric 81.3.4 Pre-treatment of the electrodes
acid, stir and filter through an inert membrane
filter (pore size 0.45 4m). If interfering substances 81.3.4.1 Amalgamation of the silver double
are present (see 81.4) add 0.5 g activated carbon electrode. Immerse both electrode rods in the
(analytical grade) to the acidified extract, stir etching solution for 15 s. Wash with de-ionized
vigorously and filter off over an inert membrane water, and dry carefully with filter paper.
filter (pore size 0.45 4m). Immediately dip the electrode rods in pure mercury
for approximately 30 s. Remove any excess mercury
Transfer the extract to a 500 mL one-mark by light tapping. The electrode rods should have a
volumetric flask and make up to the mark with bright metallic appearance. The layer of amalgam is
de-ionized water. sufficient for 15 to 20 titrations with 0.01N AgNO3.
81.3 Determination of chloride ions If there is doubt as to the condition of the electrodes
81.3.1 General. The chloride ions are determined by a test titration should be undertaken with a solution
polarographic titration using the alternating of 5 mL 0.01N NaCl in 100 mL de-ionized water
current voltage method with amperometric with 0.01N AgNO3. If the titration is slow and the
indication. A weak a.c. voltage of constant end point not clearly defined then the electrode
amplitude is applied to two amalgamated silver needs to be reamalgamated.
electrodes immersed in the titration solution When not in use the electrode should be stored in
containing chloride ions producing a specific state of de-ionized water.
polarization at the electrode surface. The
81.3.4.2 Activation of the amalgamated silver
polarization resistance at the electrodes is
electrode. Activation should be undertaken before
dependent on the concentration of the chloride ions
the first chloride determination, after each new
which react on titration with silver nitrate solution.
amalgamation or if the electrode has not been used
As the titration nears its end point, the polarization for several hours.
resistance increases considerably, reaching a
maximum at the end point. The electrodes should be activated in a titration
with 0.01N AgNO3. Titrate a solution of 5 mL 0.1N
If a constant a.c. voltage is maintained at the
NaCl and 100 mL de-ionized water with 0.1N
electrodes, any change in the polarization resistance
AgNO3 to the end point. Newly amalgamated
is indicated by a corresponding current variation.
electrodes should be left in the titrated solution
81.3.2 Apparatus for 30 min and then rinsed with de-ionized water
NOTE Other forms of polarographic equipment may be before an actual titration.
suitable.
81.3.2.1 Schmidt Eltimeter with control and
measuring devices.
54 © BSI 02-2000
BS 2972:1989
81.3.5 Chloride titration procedure. Place 200 mL of NOTE Outlying results (statistical outliers) should be
the nitric acid extract together with a magnetic determined using Dixon’s test as described in clause 13 of
BS 5497-1:1987. If more than one outlier is found, the chloride
stirring rod into the titration vessel. determination has to be repeated.
Add 2.0 mL 0.01N sodium chloride to aid detection
81.4 Impurities and interferences
of the end point. Immerse the double silver electrode
as deeply as possible into the solution and away As a check on the titration result add a known
from the inlet of the titrant. Switch on the volume of 0.01N NaCl solution to the completely
instrument and magnetic stirrer. Adjust the titrated test solution. Titrate with 0.01N AgNO3.
micro-ammeter needle to the centre of the scale and This titration has to give an identical volume of
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
when the needle has steadied titrate the solution AgNO3 to the NaCl volume that was added. If the
with 0.01N AgNO3. The end point is reached when volume of AgNO3 is less than the volume of NaCl
the needle moves clearly to the left. added then the titration is incorrect because of the
Determine the blank value with 2.0 mL 0.1N NaCl presence of impurities. In this case it is essential
that pretreatment as in 81.2 is carried out.
solution:
mL test solution – mL blank value = x mL
81.3.6 Expression of results. Calculate the chloride
content from the following expression:
500 × F
-------------------- = mg Cl/kg
200 E
where
E is the mass of insulating material (in g);
F is the stoichiometric factor for calculating
chloride content (in mg/kg) = 355 when
using 0.01N AgNO3 solution.
© BSI 02-2000 55
BS 2972:1989
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
further 2 g of the sample and report both values.
56 © BSI 02-2000
BS 2972:1989
Publications referred to
© BSI 02-2000
BS 2972:1989
Revisions
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We would be grateful if anyone finding an inaccuracy or ambiguity while using
Licensed Copy: Kerry Pritchard, Brown & Root, 15-Feb-01, Uncontrolled Copy. © BSI
this British Standard would inform the Secretary of the technical committee
responsible, the identity of which can be found on the inside front cover.
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