DRAFT FDES

DES 6612 -2
carbonated

4050
ETHIOPIAN First edition

STANDARD 2004-xx-xx

Bitumens for building and civil

engineering —
Part 2: Specification for mixtures of
bitumen with pitch, tar and Trinidad lake
asphalt

ICS : 75.140; 91.100.50; 93.080.20

Descriptors: Bitumens for building and civil engineering, specification for mixtures of
bitumen with pitch, tar and Trinidad lake asphalt, classification, pitch-bitumen mixtures

Reference number
Price based on 14 pages. ES 6612 - 2: 2004
DES 6612 - 2: 2004

Foreword

This Ethiopian Standard has been prepared under the direction of the Construction Materials Building and
Civil Engineering Technical Committee and published by the Quality and Standards Authority of Ethiopia
(QSAE).

In the preparation of this Committee Draft reference has been made to the following:

- BS 3690 Part 3:1990, British Standard Specification for Bitumens for building and civil engineering — Part
2: Specification for mixtures of bitumen with pitch, tar and Trinidad lake asphalt , published by the British
Standards Institute (BSI).

Acknowledgement is made for the use of information from the above publication.

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DRAFT ETHIOPIAN STANDARD DES 6612 - 2: 2004

Bitumens for building and civil engineering — Part 2: Specification

for mixtures of bitumen with pitch, tar and Trinidad lake asphalt

1 Scope

This Ethiopian Standard 6612 Part 2: 2004 specifies classification, composition and properties of pitch-bitumen
mixtures, tar-bitumen mixtures and lake asphalt-bitumen mixtures that are suitable for use in road and industrial
applications in the UK.

Each mixture is classified into a number of grades for each of which the appropriate designation and properties are
specified.

Advice on handling and packaging, and on samplin and testing is given in Annex A and Annex B.

2 Normative references

The following Draft Standards/ Ethiopian Standards contain provisions which, through reference in this text, constitute
the provisions of this Ethiopian Standard. At the time of publication the editions indicated were valid. All standards are
subject to revision and parties to agreements based on this Ethiopian Standard are encouraged to investigate the
possibility of applying the most recent editions of the Ethiopian Standards indicated below. Registers of currently valid
standards are maintained in the Quality and Standards Authority of Ethiopia.

BS 76, Specification for tars for road purposes.

3)
BS 594, Hot rolled asphalt for roads and other paved areas .

BS 598, Sampling and examination of bituminous mixtures for roads and other paved areas.

BS 598-3, Methods for design and physical testing.

3)
BS 1446, Specification for mastic asphalt (natural rock asphalt fine aggregate) for roads and footways .
3)
BS 1447, Specification for mastic asphalt (limestone fine aggregate) for roads and footways .

BS 2000, Methods of test for petroleum and its products.

BS 2000-45, Loss on heating of bitumen and flux oil.

BS 2000-47, Solubility of bituminous binders.

BS 2000-49, Penetration of bituminous materials.

BS 2000-58, Softening point of bitumen (ring and ball).

BS 2000-223, Ash from petroleum products containing mineral matter.

BS 6612, Bitumens for building and civil engineering.

BS 6612-1, Specification for bitumens for roads and other paved areas.

BS 3690-2, Specification for bitumens for industrial purposes3).

 DES 6612 - 2: 2004

BS 4306, Method for determination and application of precision data in relation to methods of test for petroleum
products.

BS 4699, Methods for determination of density or relative density of petroleum and petroleum products (pyknometer
methods).
3)
BS 4987, Coated macadam for roads and other paved areas .

ISO 3838, Crude petroleum and liquid or solid petroleum products — Determination of density or relative density —
Capillary — stoppered pyknometer and graduated bicapillary pycnometer methods.

ASTM D5, Standard test method for penetration of bituminous materials.

IP 45, Loss on heating bitumen and flux oil.

IP 47, Solubility of bituminous binders.

IP 49, Standard method of test for penetration of bituminous materials.

IP 58, Softening point of bitumen (ring and ball).

IP 223, Ash from petroleum products containing mineral matter.

Institute of Petroleum Model Code of Safe Practice Part 11, Bitumen Safety Code. Road Note 39 Recommendations
3)
for road surface dressing .
3)
Specification for Highway works . Standard methods for testing tar and its products (7th edition).

STPTC PT3-79 Pitch softening point: Ring and ball method.

STPTC RT2-79 Viscosity (efflux time in the standard tar viscometer).

STPTC RT10-79 Segas test and accelerated Segas test.

3)
Referred to in the foreword only.

3 Definitions:

For the purposes of this Part of this standard, the following definitions apply

3.1
bitumen
a viscous liquid, or a solid, consisting essentially of hydrocarbons and their derivatives, which is soluble in
trichloroethylene and is substantially non-volatile and softens gradually when heated. It is black or brown in colour and
possesses waterproofing and adhesive properties. It is obtained by refinery processes from petroleum, and is also
found as a natural deposit or as a component of naturally occurring asphalt, in which it is associated with mineral
matter

3.2
pitch
the black or dark brown solid or semi-solid residue remaining after the partial evaporation or fractional distillation of
crude tars produced wholly or substantially as a by-product in the carbonization of coal at temperatures exceeding 600
°C (see also 2.3)

3.3
refined tar
road tar as defined in BS 76

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3.4
pitch-bitumen mixture
a binder consisting of a homogeneous mixture containing specified proportions by mass of penetration grade bitumen
and pitch

3.5
tar-bitumen mixture
a binder consisting of a homogeneous mixture containing specified proportions by mass of penetration grade bitumen
and refined tar

3.6
refined lake asphalt
a naturally occurring mixture of bitumen and finely divided mineral matter which is found in well-defined surface
deposits and from which unwanted components such as water and vegetable matter have been removed

3.7
lake asphalt-bitumen mixture
a homogeneous mixture of refined Trinidad lake asphalt and bitumen, with or without the addition of flux oil, used in
the manufacture of asphalts and other coated materials.

4 Classification
The mixtures specified in this Part of this standard shall be designated by numbers representing the mid-point of the
penetration or viscosity range as appropriate. Pitch-bitumen mixtures, penetration grade tar-bitumen mixtures and lake
asphalt-bitumen mixtures shall have the suffix “pen” whereas lower viscosity tar-bitumen mixtures shall have the suffix
“secs”.

5 Pitch-bitumen mixtures
Pitch-bitumen mixtures shall be homogeneous mixtures containing 20 % to 25 % by mass of pitch with the remainder
being penetration grade bitumen complying with BS 6612-1. The bitumen shall have a penetration value not greater
than 150, and the softening point of the pitch when determined in accordance with Annex C shall be between 55 °C
and 80 °C.

The mixtures shall comply with the requirements given for the appropriate grade in Table 1 when tested by the
methods shown in that table.

6 Tar-bitumen mixtures

6.1 Tar-bitumen mixtures for surface dressing

6.1.1 Composition.

Tar-bitumen mixtures for surface dressing shall be homogeneous mixtures containing 30 % to 55 % by mass of
refined tar, with the remainder being penetration grade bitumen complying with BS 6612-1. The refined tar component
of the mixtures shall contain not less than 25 % by mass of pitch with a softening point of 80 °C when determined in
accordance with Annex C, or a correspondingly greater amount of pitch with a softening point below 80 °C or lesser
amounts of pitch with a softening point above 80 °C.

The mixtures shall comply with the requirements given for the appropriate grade in Table 2 when tested by the
methods shown in that table.

6.1.2 Storage stability.

The mixtures shall transform completely, without stirring, into a mobile, uniform liquid with no separation of solid
matter when heated to a temperature of 140 °C.
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After cooling, the mixtures shall have a uniform appearance and no visible layer of oil shall form on the surface after it
has remained without agitation for 24 h at 15 °C to 20 °C in a sealed container.

6.2 Tar-bitumen mixtures for coated macadam.

Tar-bitumen mixtures for coated macadam shall be homogeneous mixtures containing 10 ± 3 % by mass of refined
tar, with the remainder being penetration grade bitumen complying with BS 6612-1.

The mixtures shall comply with the requirements given for the appropriate grade in Table 3 when tested by the
methods shown in that table.

7 Lake asphalt-bitumen mixtures

Lake asphalt-bitumen mixtures shall be homogeneous mixtures containing approximately equal proportions by mass
of refined lake asphalt complying with the requirements given in Table 4 and penetration grade bitumen complying
with BS 6612-1.

The mixtures shall comply with the requirements given for the appropriate grade in Table 5 when tested by the
methods shown in that table.

8 Sampling

Samples shall be taken in accordance with Annex B.

Table 1 — Properties of pitch-bitumen mixtures

Grade
Property Test method Identical with 50 pen 70 pen
Penetration at 25 °C BS 2000-49 ASTM D5 50 ±10 70 ±10
IP 49
Softening Point °C (min.) BS 2000-58 IP 58 47 44
(max.) 58 54
Loss on heating for 5 h at 163 °C BS 2000-45 IP 45
a) Loss by mass % (max.) 1.0 1.0
b) Drop in penetration % (max.) 30 30
Solubility in trichloroethylene BS 2000-47 IP 47 95.0 96.0
% by mass (min.)
Stability index (max.) BS 598-3 1.2 1.2

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Table 2 — Properties of tar-bitumen mixtures for surface dressing

Grade
Technically
Property Test method
identical with 100 secs 200 secs

Viscosity (STVa) at 40 °C 10 mm cup BS 76 ES 76 STPTC RT2 -79 100 ±20 10 to 200 ±40 6 to
Segas test evt bincrease °C Storage See 5.1.2 STPTC RT1 0-79 20 See 5.1.2 16 See 5.1.2
stability

aStandard tar viscometer. The determination of viscosity shall be carried out in accordance with B.1 a) of
ES 76:1974.
b Equiviscous temperature.

Table 3 — Properties of tar-bitumen mixtures for coated macadam

Property Test method Identical with Grade
100 pen 200 pen
Penetration at 25 °C BS 2000-49 ASTM D5 100 ±20 200 ±30
IP 49
Softening point °C (min.) BS 2000-58 IP 58 41 33
(max.) 51 42

Table 4 — Properties of refined lake asphalt

Property Test method Identical with Requirements
Penetration at 25 °C BS 2000-49 ASTM D5 2 ±2
IP 49
Softening point °C (min.) BS 2000-58 IP 58 93
(max.) 99
Loss on heating for 5 h at 163 °C (max.) BS 2000-45 IP 45 2.0
% by mass
Solubility in trichloroethylene (min.) BS 2000-47 IP 47 52
% by mass (max.) 55
Ash content (min.) BS 2000-223 IP 223 35
% by mass (max.) 39
Density at 25 °C (min.) BS 4699 ISO 3838 1.39
g/mL (max.) 1.44

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Table 5 — Properties of lake asphalt-bitumen

Property Test method Identical with Requirements
Penetration at 25 °C ES 2000-49 ASTM D5 2 ±2
IP 49
Softening point °C (min.) BS 2000-58 IP 58 93
(max.) 99
Loss on heating for 5 h at 163 °C (max.) BS 2000-45 IP 45 2.0
% by mass
Solubility in trichloroethylene (min.) BS 2000-47 IP 47 52
% by mass (max.) 55
Ash content (min.) BS 2000-223 IP 223 35
% by mass (max.) 39
Density at 25 °C (min.) BS 4699 ISO 3838 1.39
g/mL (max.) 1.44

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Annex A

Handling and packaging

Pitch-bitumen and tar-bitumen mixtures are normally supplied hot in bulk either by road tanker or rail car. Lake asphalt
is normally supplied in drums. Supplier’s recommendations should be sought with regard to appropriate handling
procedures. Reference should also be made to the latest versions of “Standard methods for testing tar and its
products”1), and the “Institute of Petroleum Model code of Safe Practice, Part 11, Bitumen Safety Code”2). Both of
these publications include specific information on safe handling procedures for the mixtures.

Excessive or prolonged heating of bitumen mixtures, particularly of tar-bitumen mixtures for surface dressing, can lead
to loss of volatile components and consequent non-compliance with the specification.
1)
Obtainable from the Standardization of Tar Products Test Committee, Wingerworth, Chesterfield, Derbyshire S42
6JS.
2)
Obtainable from the Institute of Petroleum, 61 New Cavendish Street, London W1M8AR.

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Annex B

Sampling and testing

B.1 Sampling locations

B.1.1 General.

If it is desired to sample for the purpose of establishing compliance with this standard, samples of the bitumen
mixtures should be taken as follows.

B.1.2 Pitch-bitumen and tar-bitumen mixtures.

Samples should be taken from whichever of the following locations is appropriate:

a) from the tanker or rail car in the case of bulk delivery by road or rail, immediately before discharge;

b) from the storage tank (or the feed pipe to the mixer) of a manufacturer of asphalts, macadams or other coated
materials, immediately before mixing;

c) from the tank or the spray-bar of a binder distributor used for surface dressing, immediately before spraying.

The procedures involved in handling the binder for surface dressing may lead to some loss of volatile components
from the tar-bitumen mixtures without necessarily impairing the performance of the surface dressing. Where a sample
of a tar-bitumen mixture for surface dressing that has been taken from one of the locations listed in B.1.2 c) has a
viscosity (STV) at 40 °C that is as given in Table 6, experience has shown that the original viscosity of the mixture
complied with the requirements of this Part of this standard.

Table 6 — Viscosity limits

B.1.3 Refined lake asphalt.

Samples should be broken from the material in the package.

B.1.4 Lake asphalt-bitumen mixtures.

Samples should be taken from the tank used for blending the refined lake asphalt and bitumen or from the feed pipe of
the tank to the mixer, immediately after the refined lake asphalt and bitumen have been thoroughly mixed together.

B.2 Sampling procedure.

When sampling bitumen mixtures the purchaser should obtain a sample of not less than 5 kg which should represent
the material delivered by the supplier. The sample should be immediately divided into three approximately equal sub-
samples which should be placed in clean and dry metal containers capable of being securely closed. Each sub-
sample should be clearly labelled with the names of the supplier and purchaser, details of the type and grade of
bitumen mixture, time and date of sampling and identification of the sampling location.

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The purchaser should use only one of the sub-samples for his own tes ts, the remaining two sub-samples should be
retained by him to be used in case of dispute.

NOTE 1 It is recommended that routine checking of bitumen mixtures should be based mainly on the penetration test for those
mixtures given in Table 1, Table 3 and Table 5, the viscosity test for mixtures given in Table 2 and the penetration and softening
point tests in the case of refined lake asphalt. The other specified properties are relevant but experience indicates that checking
these properties on a routine basis is only necessary when there are reasons to suspect the quality of the material.

NOTE 2 To ensure valid comparison between the test results of purchaser and supplier, it is essential that the purchaser should
test the material within 7 days after sampling.

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Annex C

Method for the determination of the softening point of pitch (ring and ball
method)

NOTE This method is technically identical with STPTC PT3-79. Editorial changes have been made to bring the method into line
with the rest of this Part of this standard. STPTC PT3-79 supersedes PT3-67 which currently appears in ES 76. It is intended that
this test be carried out in accordance with the general principles and apparatus requirements laid down in the STPTC handbook.

C.1 Principle.

To determine the softening point of pitches having expected softening points equal to or greater than 30 °C using ring
and ball apparatus.

The test assembly is prepared with a disc of the test sample cast in a horizontal brass ring upon which rests a steel
ball. The test assembly is heated at a specified rate in a glycerol- or water-bath until the test sample becomes
sufficiently soft to allow the steel ball enveloped in the pitch to fall to a specified level.

NOTE There are no special hazards involved in this method, but see foreword.

C.2 Reagents

C.2.1 Glycerol, for use with samples having an expected softening point greater than 85 °C.

C.2.2 Distilled water, or equivalent, which has been freshly boiled and cooled, for use with pitcheshaving an expected
softening point within the range 30 °C to 85 °C.

C.3 Apparatus

C.3.1 Stainless steel dish, or similar, of approximately 55 mm diameter and 35 mm depth.

C.3.2 Oven, capable of being maintained at a temperature 50 °C above the expected ring and ball softening point of
the sam ple.

C.3.3 Grinder, capable of coarsely grinding the sample to particles approximately 3 mm in size.

C.3.4 Knife.

C.3.5 Tongs.

C.3.6 Vacuum desiccator.

C.3.7 Ring and ball apparatus, see Figure 1 (a) comprising the following.

a) Two brass tapered rings, see Figure 1 (b), with the following dimensions:

1) depth 6.4 ± 0.1 mm;

2) internal diameter at bottom 15.9 ± 0.1 mm;

3) internal diameter at top 17.5 ± 0.1 mm;

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 DES 6612 - 2: 2004

4) external diameter above shoulder 20.6 ± 0.1 mm;

5) external diameter below shoulder 18.5 ± 0.1 mm.

b) Two steel balls, 9.53 mm diameter and each weighing 3.5 ± 0.05 g.

c) Two ball centring guides, see Figure 1 (c).

d) Bath, in the form of a heat-resistant glass squat-form beaker of 800 mL capacity.

e) Thermometers, of the following ranges as appropriate and complying with the appropriate requirements of Table 7:

1) range 0 °C to 120 °C for pitches expected to give results between 30 °C and 120 °C;

2) range 50 °C to 210 °C for pitches expected to give a result greater than 120 °C.

f) Ring support, see Figure 1 (d), consisting of two brass plates, the upper carrying two rings. The support is attached
to a brass plate which rests on top of the beaker and has a central hole through which the thermometer is located. The
depth of the pitch ring below the shoulder is the same as the thickness of the ring support plate. The lower plate is
approximately 25 mm wide and approximately 75 mm long, fixed so that its upper surface is 25 ± 0.5 mm below the
surface of the ring support plate and its lower surface is not less than 13 mm above the base of the beaker.

g) Bunsen burner, fitted with a governor if the gas supply is liable to fluctuate.

h) Tripod and draught screen. The apparatus is supported on a tripod on a square of open mesh wire gauze and the
whole assembly is protected from draughts by means of an appropriately dimensioned screen.

i) Moulding plate, see Figure 1 (e).

C.4 Procedure

C.4.1 Melting of sample.

Place 50 g of the ground sample in the dish and place in the oven set at approximately 50 °C above the expected ring
and ball softening point of the pitch. At the same time place the rings in the oven. Leave both the pitch and rings in the
oven for 2 h at this temperature.

Remove both the pitch and rings. Invert the heated rings and place one within each of the sets of guide pins on the
moulding plate, having treated it to prevent adhesion of the pitch and immediately pour the molten pitch in a steady
stream into the ring s.

The molten pitch after 2 h in the oven should have a smooth shiny surface with no skin on top. If the surface of the
molten pitch is covered with froth, this suggests that there is moisture present in the sample. In this case discard the
melt and stand a freshly ground sample in a vacuum dessicator for 24 h, prior to using it to prepare a further molten
sample.

The quantity of pitch used for each ring shall be such that, after a cooling period of 20 min a slight excess of pitch
remains above the level of the ring.

At the end of the cooling period remove this excess with a knife with out applying heat. Fill the two rings from a single
melting and test them together. While the sample is being melted, prepare the apparatus.

C.4.2 Apparatus.

Measure approximately 600 Ml of the appropriate heating liquid into the beaker at a temperature at least 45 °C below
the expected softening point of the pitch. The liquid level shall be at least 50 mm above the top of the rings. Fit the
filled rings into the support and place the assembly centrally in the beaker. Insert the appropriate thermometer so that
it lies along the axis of the beaker and so that the bottom of the bulb is level with the bottom of the rings and central
with the central hole of the supporting plate.

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Set the ball centring guides on top of each ring.

Place the steel balls in the liquid in the beaker but not in position in the centring guides. Set up the apparatus on the
tripod so that the ring support plate is horizontal and allow to stand for 15 min. Using tongs, place the balls in the
centring guides on the upper surface of the pitch in the rings.

C.4.3 Determination.

Place the Bunsen burner under and midway between the centre and the edge of the beaker and on a diameter at
right-angles to that which includes the rings and the thermometer. Heat so that the temperature is raised 5 °C/min.

Maintain this rate with ± 0.5 °C over each 1 min period after the first 3 min. It shall not be merely the average of the
period of the test.

Reject any test in which the heating does not comply with these requirements.

Record the temperature at which the pitch surrounding each steel ball touches the lower plate of the support and
report the mean of the two figures to the nearest 0.2 °C. If, for the two balls, the temperatures differ by more than 1 °C,
discard the result and repeat the test. If, for any reason, the test has to be repeated, carry out the whole procedure
given in C.4.1 and C.4.2 again with a fresh 50 g sample of the pitch.

C.5 Expression of results

C.5.1 Softening point.

Give the softening point as the mean of the two temperatures recorded as described in C.4.3 and express the result to
the nearest 0.2 °C.

C.5.2 Repeatability and reproducibility.

Duplicate results (each the mean of two figures) by the same operator shall be accepted if they do not differ by more
than 0.5 °C up to 85 °C and by more than 2.0 °C above that temperature. Single results (the mean of the two figures)
submitted by each of two laboratories shall be accepted if they do not differ by more than 2.8 °C up to 85 °C and by
more than 3.8 °C above that temperature.

NOTE These figures were obtained in tests using a less well-defined pitch melting technique and before the introduction of the use
of the ball centring guide. The precision now obtained from this method of determination is expected to be better than the figures
given. Further information on the use of these precision figures may be obtained from ES 4306.

C.6 Test report.

Report the following information:

a) sample description and reference number;

b) test method;

c) the softening point of the pitch to the nearest 0.2 °C;

d) any abnormalities in the sample or the procedure likely to affect the result.

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Table 7 — STPTC thermometer specifications

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NOTE All dimensions are in millimetres.

Figure 1 — Apparatus for ring and ball test

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