British Standard

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 | BS 144 : 1997
BRITISH STANDARD |
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Specification for |
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Coal tar creosote for |
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wood preservation |
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Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

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ICS 71.100.50; 79.020 |
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NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW
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BS 144 : 1997

Committees responsible for this

British Standard
The preparation of this British Standard was entrusted to Technical Committee
B/515, Wood preservation, upon which the following bodies were represented:

British Telecommunications plc

British Wood Preserving and Damp-proofing Association
Chemical Industries Association
Creosote Council

Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

Department of the Environment (Building Research Establishment)
Timber Research and Development Association
Timber Trade Federation
Wood Panel Industries Federation

The following bodies were also represented in the drafting of the standard, through
subcommittees and panels:

Association of Consulting Scientists

ITRI Ltd.
Ministry of Defence

This British Standard, having

been prepared under the
direction of the Sector Board for
Building and Civil Engineering,
was published under the
authority of the Standards Board
and comes into effect on
15 July 1997
 BSI 1998

First published, as BS 144, August Amendments issued since publication

1921
Second edition July 1936 Amd. No. Date Text affected
Third edition June 1954
Fourth edition March 1973
Fifth edition, as Parts 1 and 2, 9947 April 1998 Indicated by a sideline in the margin
April 1990
Sixth edition, as BS 144, July 1997

The following BSI references

relate to the work on this
standard:
Committee reference B/515
Draft for comment 96/120287 DC

ISBN 0 580 25301 5

 BS 144 : 1997

Contents

Page
Committees responsible Inside front cover
Foreword ii
Specification
1 Scope 1
2 References 1
3 Composition 1
4 General requirements 1
Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

5 Methods of treatment of timber 1

Annexes
A (normative) Method for the determination of liquidity 3
B (normative) Method for the determination of density 3
C (normative) Method for the determination of distillation range 4
D (normative) Method for the determination of extractable phenols 9
E (normative) Method for the determination of kinematic viscosity 10
F (normative) Method for the determination of water content 12
G (normative) Method for the determination of matter insoluble in toluene 12
H (normative) Method for the determination of naphthalene content by gas
chromatography 13
I (informative) Guidance on the methods of treatment of timber 15
Tables
1 Requirements for creosote types 1, 2, 3 and 4 2
B.1 Multiplication (m) and addition (a) factors for conversion of corrected
hydrometer readings at t ÊC to density at 38 ÊC (creosote types 1 and 2) 5
B.2 Multiplication (m) and addition (a) factors for conversion of corrected
hydrometer readings at t ÊC to density at 20 ÊC (creosote type 3) 6
B.3 Multiplication (m) and addition (a) factors for conversion of corrected
hydrometer readings at t ÊC to density at 55 ÊC (creosote type 4) 7
C.1 Corrections for barometric pressure 8
Figures
E.1 BS/IP/RF U-tube reverse flow viscometer 11
I.1 Example spacing of incisions 17
List of references 20

 BSI 1997 i
BS 144 : 1997

Foreword

This revision of BS 144 has been prepared under the direction of Technical Committee
B/515, Wood preservation.
This British Standard was first published in 1921, with revisions in 1954, 1973 and 1990.
The 1990 revision brought all types of creosote under one standard (low viscosity
creosote not requiring heat for application had previously been covered by BS 3051).
The 1990 revision specified three types of creosote to cover all applications; it also
incorporated the provisions of BS 913, which was withdrawn. This revision reflects the
subsequent advances in technology and particular attention has been paid to
environmental issues.

Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

Four types of creosote are specified in this revision, together with methods for
determining conformity to the specifications. Methods of application previously
specified in BS 144 : Part 2 : 1990 are now given in an informative annex.
Materials conforming to this specification and used as a wood preservative require
Government approval under the Control of Pesticides Regulations 1986 (SI 1510)
before they can be sold, supplied, stored, advertised or used in the United Kingdom.
This revision supersedes BS 144 : Part 1 : 1990 and BS 144 : Part 2 : 1990, which are
withdrawn.
CAUTION. Attention is drawn to the Health and Safety at Work etc. Act 1974, and the
need for ensuring that the methods specified in this British Standard are carried out
with suitable precautions.
The procedures described in this British Standard are intended to be carried out by
appropriately qualified and experienced persons or other suitably trained and/or
supervised personnel. Normal safety precautions should be taken throughout
performing the methods.
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 and ii, pages 1 to
20, an inside back cover and a back cover.

ii  BSI 1997
 BS 144 : 1997

Specification

1 Scope 3 Composition
This British Standard specifies requirements for four All types of creosote shall consist of blends of
types of coal tar creosote for wood preservation. distillates of coal tar and shall be free from
Type 1 creosote is intended for treatment of timber petroleum oils or oils not derived from coal tar.
by pressure impregnation.
Type 2 creosote is also intended for pressure 4 General requirements
impregnation, but has a more closely defined
distillation range and a more restricted residue 4.1 When tested in accordance with the methods
listed in table 1, the creosote, when manufactured,
Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

content than creosote of type 1. Type 2 creosote is

especially suitable for treatment of poles for shall be in accordance with the limiting requirements
overhead power and telecommunication lines, and given in that table. Samples for the assessment of
for structural timbers where bleeding in service conformity to these requirements shall be taken in
could present a problem. accordance with BS EN 1014-1.
Type 3 creosote is intended for treatment of timber 4.2 Requirements for creosote in use within
by immersion and brushing. treatment plants shall be as in table 1 except for:
Type 4 creosote is intended for treatment of timber
by pressure impregnation at temperatures > 100 ÊC. water content (max.): 3.0 % (V/V);
This creosote excludes the lower boiling fractions insoluble matter content (max.): 0.6 % (m/m).
allowable in the other three creosote types and is
especially suitable where volatility leading to odour
is a problem. 5 Methods of treatment of timber
NOTE. Creosote of types 1, 2 and 3 may be used for the Guidance on methods of treatment of timber for use
hot-and-cold open tank process. with these preparations is given in annex I.

2 References
2.1 Normative references
This British Standard incorporates, by dated or
undated reference, provisions from other
publications. These normative references are made
at the appropriate places in the text and the cited
publications are listed on page 20. For dated
references, only the edition cited applies; any
subsequent amendments to or revisions of the cited
publication apply to this British Standard only when
incorporated in the reference by amendment or
revision. For undated references, the latest edition of
the cited publication applies, together with any
amendments.
2.2 Informative references
This British Standard refers to other publications
that provide information or guidance. Editions of
these publications current at the time of issue of this
Standard are listed on the inside back cover, but
reference should be made to the latest editions.

 BSI 1997 1
 BS 144 : 1997

Table 1. Requirements for creosote types 1, 2, 3 and 4

Property Type 1 Type 2 Type 3 Type 4 Test method

Liquidity
Temperature ( ÊC) at which the
product is completely liquid, after:
32 32 Ð 50 Annex A
2h
Ð Ð 0

Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

4h
Min. Max. Min. Max. Min. Max. Min. Max.
Density (kg/m3) at:
55 ÊC Ð Ð Ð Ð Ð Ð 1003 1144
38 ÊC 1003 1108 1003 1108 Ð Ð Ð Ð Annex B
20 ÊC Ð Ð Ð Ð 910 1120 Ð Ð
Distillation
Recovery of dehydrated creosote Annex C
(% (m/m)) at:
205 ÊC Ð 6 Ð 5 Ð 15 Ð Ð
230 ÊC Ð 40 5 30 Ð 40 Ð Ð
270 ÊC Ð Ð Ð Ð 30 Ð Ð Ð
315 ÊC Ð 78 40 78 40 90 Ð 18
355 ÊC 60 Ð 73 90 65 Ð 65 95
Min. Max. Min. Max. Min. Max. Min. Max.
Extractable phenols content
(ml/100 g of dehydrated creosote) in
the distillate up to 315 ÊC (as
obtained in annex D):
Types 1, 2 and 4, density 5 20 5 20 Ð Ð 5 18 Annex D
range 1003 kg/m3 to 1045 kg/m3
Types 1, 2 and 4, density 0 20 0 20 Ð Ð 0 18
range 1046 kg/m3 to 1144 kg/m3
Type 3 Ð Ð Ð Ð 1 20 Ð Ð
Flash point (ÊC, Pensky-Martens 61 Ð 61 Ð 61 Ð 61 Ð BS EN 22719
closed tester)
Viscosity (mm2/s), kinematic at 40 ÊC Ð Ð 4 20 Ð Ð Ð Ð Annex E
Water content (% (V/V)) Ð 1.5 Ð 1.5 Ð 1.5 Ð 1.5 Annex F
Insoluble matter content (% (m/m)) Ð 0.4 Ð 0.4 Ð 0.4 Ð 0.4 Annex G
Naphthalene content (% (m/m)) Ð Ð Ð 15 Ð Ð Ð Ð Annex H
Benzo[a]pyrene content (mg/kg) Ð 500 Ð 500 Ð 50 Ð 500 DD ENV 1014-3
Water extractable phenols content Ð 3 Ð 3 Ð 3 Ð 3 BS EN 1014-4
| (% (m/m))

2  BSI 1998
 BS 144 : 1997

Annexes

Annex A (normative) Annex B (normative)

Method for the determination of liquidity Method for the determination of density
A.1 Principle B.1 Principle
The sample is maintained at the specified temperature Density is determined by means of a density
(50 ÊC, 32 ÊC or 0 ÊC) for 2 h or 4 h and then examined hydrometer.
for the presence of separated solid matter. B.2 Apparatus
A.2 Apparatus B.2.1 Hydrometer, conforming to series L50 of BS 718,
Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

A.2.1 Conical flask, capacity 100 ml. calibrated for determination of density at 20 ÊC in g/ml,
for use in liquids of low surface tension, and
A.2.2 Thermometer, partial immersion thermometer of constructed of soda-lime glass.
range 2 0.5 ÊC to 55 ÊC, graduated at each 0.1 ÊC and NOTE. Hydrometers calibrated in kg/m3 are also available in
accurate to ± 0.2 ÊC. series L50 of BS 718, and these may be used instead. If such a
NOTE. A thermometer conforming to BS 593 is suitable. hydrometer is used, it should be read to the nearest kg/m3
(see B.3); the corrections described in B.4 should be multiplied
A.2.3 Constant temperature baths. Depending on the by 1000, and the factor 1000 from the equation in B.4.2 omitted.
type of creosote being tested, baths able to maintain Examine the hydrometer before use to see that it is
temperatures of (50 ± 0.1) ÊC, (32 ± 0.1) ÊC or clean and dry and that there has been no displacement
(0 ± 0.1) ÊC. of the paper scale during use.
NOTE. Any displacement of the paper scale can be detected by
A.3 Procedure reference to the means provided for this purpose: e.g., a horizontal
Pour about 50 ml of the laboratory sample (see line may be etched on the stem of the hydrometer and the
BS EN 1014-1) into the conical flask. Fit the corresponding datum marked on the paper scale. If the scale has
been displaced, recertification of the hydrometer is necessary.
thermometer by means of a cork into the neck of the
flask, with the bulb of the thermometer immersed in B.2.2 Hydrometer vessel, free from local irregularities
the creosote. Place the flask in the appropriate producing distortion and several millimetres greater in
constant temperature bath. diameter than the hydrometer bulb.
Ensure that the surface of the creosote is below that of NOTE. A 1 l measuring cylinder conforming to BS 604 is suitable.
the water in the bath. Swirl the flask until the creosote B.2.3 Partial immersion thermometer, of range
reaches the appropriate temperature. Leave the flask in 2 0.5 ÊC to 60 ÊC, graduated in 0.1 ÊC and accurate to
the bath for 2 h or 4 h as appropriate, then withdraw ± 0.2 ÊC.
the flask and examine the surface of the creosote for NOTE. A thermometer conforming to BS 593 is suitable.
solid matter. Rotate the flask slowly, holding it
horizontally, and examine the sides for solid matter. B.3 Procedure
When the sample is free from solid matter, place the Warm the laboratory sample (see BS EN 1014-1) to
flask in the second bath, maintained at (32 ± 0.1) ÊC for approximately 38 ÊC for types 1 and 2, 20 ÊC for type 3
types 1 and 2 creosote, (0 ± 0.1) ÊC for type 3, and and 55 ÊC for type 4 creosote. Fill the clean hydrometer
(50 ± 0.1) ÊC for type 4. Re-examine the sample for vessel with the liquefied laboratory sample to a depth
solids when the contents have reached the bath sufficient to allow the hydrometer to float.
temperature, and again after having maintained the NOTE. Pour the sample down the side of the vessel, to avoid
formation of air bubbles.
sample at the bath temperature for 2 h for
types 1, 2 and 4, or 4 h for type 3. Gently stir the sample, avoiding formation of air
bubbles. Hold the hydrometer by the top of the stem,
A.4 Acceptance criteria insert it carefully into the sample, and release it when
The sample shall be deemed to pass the liquidity test if approximately in the position of equilibrium, i.e. when
it remains completely liquid for the specified period at it rises or falls only to a small degree.
the specified temperature. Lightly press the top of the hydrometer stem, to
The sample shall be deemed to fail the liquidity test if immerse it further by a few millimetres. Release the
any solid matter is observed, either after cooling to the hydrometer. After a few oscillations, when the
specified temperature or at any time up to the end of hydrometer is steady, note the reading.
the specified period at that temperature. Observe the meniscus. If the stem is clean the
meniscus shape will remain unchanged during the
hydrometer oscillations. If the meniscus shape changes,
clean the hydrometer and repeat the procedure.
Record the hydrometer reading to the
nearest 0.001 g/ml and the temperature of the creosote
to the nearest 0.1 ÊC. If the bottom of the meniscus is
not visible, take the reading at the level where the
meniscus merges into the stem of the hydrometer.

 BSI 1997 3
BS 144 : 1997

B.4 Calculation C.2.2 Thermometer, with a range of 2 2 ÊC to 400 ÊC,

as described in BS 593.
B.4.1 Correction of hydrometer reading
Calculate the corrected hydrometer reading, Rt, as C.2.3 Separating funnels, capacity 50 ml, as described
follows: in BS 2021.
C.2.4 Fortin's barometer.
Rt = R + C + 0.0007
C.3 Corrections
where
R is the hydrometer reading; C.3.1 General

Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

Apply the corrections described in C.3.2 and C.3.3 to
C is the certification correction;
the specified distillation temperatures before
0.0007 is the meniscus height correction (to be commencing the distillation.
used for opaque creosotes only).
C.3.2 Barometer readings
NOTE. The value of Rt is the corrected hydrometer reading for C.3.2.1 Read the barometer to obtain the atmospheric
the sample at t ÊC, the temperature of the creosote in the test. pressure in mbar or mmHg, and record the ambient
B.4.2 Calculation of density temperature. Continue as described in either C.3.2.2
for mbar or C.3.2.3 for mmHg.
Calculate the density d, at the required temperature
NOTE. If atmospheric pressure is measured in other units, the
(55 ÊC, 38 ÊC or 20 ÊC), as follows: following conversion factors can be used:
1 mbar = 100 N/m2 = 100 Pa;
d = 1000 (Rtm + a) 1 mmHg = 133.322 N/m2.
where
C.3.2.2 Correct the barometer readings for
d is the density (kg/m3); temperature as described in BS 658, and if the
Rt is the corrected hydrometer reading corrected reading differs from 1013 mbar, apply
(see B.4.1); corrections to the specified distillation temperature by
adding the value given in table C.1 for each millibar
m is the multiplication factor (see note); above 1013 mbar, or subtracting for each millibar
a is the addition factor (see note). below 1013 mbar.

NOTE. m and a are obtained from table B.1 for types 1 and 2,
from table B.2 for type 3, and table B.3 for type 4 creosote.

B.5 Expression of results

Express the density of the sample, to the nearest
kg/m3, at the specified temperature.

Annex C (normative)
Method for the determination of
distillation range
C.1 Principle
A sample of creosote is dehydrated and distilled, and
the fractions collected at specified temperatures.
C.2 Apparatus
C.2.1 Distillation apparatus, described in BS 658.
Assemble in accordance with BS 658, except as stated
in a) to d).
a) Distillation flasks:
1) capacity 250 ml, untared;
2) capacity 150 ml, tared, held in the vertical
position by means of a clamp at the extreme
upper end of the neck.
b) Condensers, types 1 and 2.
c) Draught screen, type 2, from which the shelf has
been removed.
d) Crow receivers, capacity 50 ml, tared.

4  BSI 1997
 Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI
 BSI 1997

Table B.1 Multiplication (m) and addition (a) factors for conversion of corrected hydrometer readings at t ÊC to density at 38 ÊC
(creosote types 1 and 2)
t ÊC 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9
34 1.00318 1.00309 1.00299 1.00290 1.00281 1.00271 1.00262 1.00253 1.00243 1.00234
2 0.00667 2 0.00650 2 0.00634 2 0.00617 2 0.00600 2 0.00584 2 0.00567 2 0.00550 2 0.00533 2 0.00517
35 1.00225 1.00215 1.00206 1.00197 1.00188 1.00178 1.00169 1.00160 1.00150 1.00141
2 0.00500 2 0.00483 2 0.00466 2 0.00450 2 0.00433 2 0.00416 2 0.00400 2 0.00383 2 0.00366 2 0.00350
36 1.00132 1.00122 1.00113 1.00104 1.00094 1.00085 1.00076 1.00067 1.00057 1.00048
2 0.00333 2 0.00316 2 0.00300 2 0.00283 2 0.00266 2 0.00250 2 0.00233 2 0.00216 2 0.00200 2 0.00183
37 1.00039 1.00030 1.00020 1.00011 1.00002 0.99992 0.99983 0.99974 0.99964 0.99955
2 0.00166 2 0.00150 2 0.00133 2 0.00116 2 0.00100 2 0.00083 2 0.00067 2 0.00050 2 0.00033 2 0.00017
38 0.99946 0.99937 0.99928 0.99918 0.99909 0.99900 0.99890 0.99881 0.99872 0.99863
0.00000 0.00017 0.00033 0.00050 0.00066 0.00083 0.00100 0.00116 0.00133 0.00149
39 0.99853 0.99844 0.99835 0.99826 0.99816 0.99807 0.99798 0.99789 0.99780 0.99770
0.00166 0.00183 0.00199 0.00216 0.00232 0.00249 0.00266 0.00282 0.00299 0.00315
40 0.99761 0.99752 0.99743 0.99733 0.99724 0.99715 0.99706 0.99697 0.99687 0.99678
0.00332 0.00348 0.00365 0.00381 0.00398 0.00414 0.00431 0.00448 0.00464 0.00481
41 0.99669 0.99660 0.99650 0.99641 0.99632 0.99623 0.99614 0.99604 0.99595 0.99586
0.00497 0.00513 0.00530 0.00547 0.00563 0.00580 0.00596 0.00613 0.00629 0.00646
NOTE. The upper figure is the multiplication factor.

BS 144 : 1997
5
6

BS 144 : 1997
Table B.2 Multiplication (m) and addition (a) factors for conversion of corrected hydrometer readings at t ÊC to density at 20 ÊC
(creosote type 3)
t ÊC 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9
15 1.00466 1.00456 1.00447 1.00438 1.00428 1.00419 1.00410 1.00400 1.00391 1.00382
2 0.00835 2 0.00818 2 0.00801 2 0.00785 2 0.00768 2 0.00751 2 0.00734 2 0.00718 2 0.00701 2 0.00684
16 1.00372 1.00363 1.00354 1.00344 1.00335 1.00326 1.00316 1.00307 1.00298 1.00288
2 0.00667 2 0.00651 2 0.00634 2 0.00617 2 0.00600 2 0.00584 2 0.00567 2 0.00550 2 0.00533 2 0.00517
17 1.00279 1.00270 1.00260 1.00251 1.00242 1.00232 1.00223 1.00214 1.00204 1.00195
2 0.00500 2 0.00483 2 0.00467 2 0.00450 2 0.00433 2 0.00416 2 0.00400 2 0.00383 2 0.00366 2 0.00350
18 1.00186 1.00176 1.00167 1.00158 1.00149 1.00139 1.00130 1.00121 1.00111 1.00102
2 0.00333 2 0.00316 2 0.00300 2 0.00283 2 0.00266 2 0.00250 2 0.00233 2 0.00216 2 0.00200 2 0.00183
19 1.00093 1.00084 1.00074 1.00065 1.00056 1.00046 1.00037 1.00028 1.00019 1.00009
2 0.00166 2 0.00150 2 0.00133 2 0.00117 2 0.00100 2 0.00083 2 0.00067 2 0.00050 2 0.00033 2 0.00017
20 1.00000 0.99991 0.99982 0.99972 0.99963 0.99954 0.99944 0.99935 0.99926 0.99917
0.00000 0.00017 0.00033 0.00050 0.00067 0.00083 0.00100 0.00117 0.00133 0.00150
21 0.99907 0.99898 0.99889 0.99880 0.99870 0.99861 0.99852 0.99843 0.99833 0.99824
0.00166 0.00183 0.00200 0.00216 0.00233 0.00250 0.00266 0.00283 0.00300 0.00316
22 0.99815 0.99806 0.99797 0.99787 0.99778 0.99769 0.99760 0.99750 0.99741 0.99732
0.00333 0.00350 0.00366 0.00383 0.00400 0.00416 0.00433 0.00450 0.00467 0.00483
23 0.99723 0.99713 0.99704 0.99695 0.99686 0.99677 0.99667 0.99658 0.99649 0.99640
0.00500 0.00517 0.00533 0.00550 0.00567 0.00584 0.00600 0.00617 0.00634 0.00651
24 0.99631 0.99621 0.99612 0.99603 0.99594 0.99585 0.99575 0.99566 0.99557 0.99548
0.00667 0.00684 0.00701 0.00718 0.00734 0.00751 0.00768 0.00785 0.00801 0.00818
25 0.99539 0.99529 0.99520 0.99511 0.99502 0.99493 0.99484 0.99474 0.99465 0.99456
0.00835 0.00852 0.00868 0.00885 0.00902 0.00919 0.00935 0.00952 0.00969 0.00986
NOTE. The upper figure is the multiplication factor.
 BSI 1997

Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

 Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI
 BSI 1997

Table B.3 Multiplication (m) and addition (a) factors for conversion of corrected hydrometer readings at t ÊC to density at 55 ÊC
(creosote type 4)
t ÊC 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9
51 1.00315 1.00306 1.00297 1.00288 1.00279 1.00270 1.00261 1.00252 1.00243 1.00234
2 0.00667 2 0.00650 2 0.00633 2 0.00616 2 0.00599 2 0.00582 2 0.00565 2 0.00548 2 0.00531 2 0.00514
52 1.00222 1.00213 1.00204 1.00195 1.00186 1.00177 1.00168 1.00159 1.00150 1.00141
2 0.00500 2 0.00483 2 0.00466 2 0.00449 2 0.00432 2 0.00415 2 0.00398 2 0.00381 2 0.00364 2 0.00347
53 1.00129 1.00120 1.00111 1.00102 1.00093 1.00084 1.00075 1.00066 1.00057 1.00048
2 0.00333 2 0.00316 2 0.00299 2 0.00282 2 0.00265 2 0.00248 2 0.00231 2 0.00214 2 0.00197 2 0.00180
54 1.00036 1.00027 1.00018 1.00009 1.00000 0.99991 0.99982 0.99973 0.99964 0.99955
2 0.00166 2 0.00149 2 0.00132 2 0.00115 2 0.00098 2 0.00081 2 0.00064 2 0.00047 2 0.00030 2 0.00013
55 0.99943 0.99934 0.99925 0.99916 0.99907 0.99898 0.99889 0.99880 0.99871 0.99862
0.00000 0.00017 0.00034 0.00051 0.00068 0.00085 0.00102 0.00119 0.00136 0.00153
56 0.99850 0.99841 0.99832 0.99823 0.99814 0.99805 0.99796 0.99787 0.99778 0.99769
0.00166 0.00183 0.00200 0.00217 0.00234 0.00251 0.00268 0.00285 0.00302 0.00319
57 0.99757 0.99748 0.99739 0.99730 0.99721 0.99712 0.99703 0.99694 0.99685 0.99676
0.00332 0.00349 0.00366 0.00383 0.00400 0.00417 0.00434 0.00451 0.00468 0.00485
58 0.99664 0.99655 0.99646 0.99637 0.99628 0.99619 0.99610 0.99601 0.99592 0.99583
0.00497 0.00514 0.00531 0.00548 0.00565 0.00582 0.00599 0.00616 0.00633 0.00650
59 0.99571 0.99562 0.99553 0.99544 0.99535 0.99526 0.99517 0.99508 0.99499 0.99490
0.00663 0.00680 0.00697 0.00714 0.00731 0.00748 0.00765 0.00782 0.00799 0.00816
NOTE. The upper figure is the multiplication factor.

BS 144 : 1997
7
BS 144 : 1997

C.3.2.3 Correct the barometer readings for Apply heat, and distil at a rate of (5 ± 0.5) ml/min. If for
temperature as described in BS 658, and if the reading any reason the distillation rate falls outside the
differs from 760 mmHg, apply corrections to the specified limits at any time after the first 5 ml of
specified distillation temperature by adding the value distillate has been collected, discontinue the test and
given in table 4 for each millimetre of mercury start again on another portion of the original sample.
above 760 mmHg, or subtracting for each millimetre of NOTE. The specified distillation rate corresponds to
mercury below 760 mmHg. approximately 90 drops/min (i.e. three drops in 2 s), but this figure
should only be taken as a guide so that the rate in millimetres per
minute may be kept under close observation.
Table C.1 Corrections for barometric pressure

Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

If solids are deposited in the condenser during the
Specified Corrections distillation, warm the condenser so that such solids are
temperature ÊC
ÊC
collected in the fraction with which they distil.
Per millibar Per millimetre of
mercury Change the receiver at each corrected specified
temperature (see tables 1 and 4), without stopping the
205 0.076 0.057 distillation. Remove the heat when the thermometer
230 0.080 0.060 indicates the highest corrected specified temperature.
270 0.087 0.065 The final fraction includes the oil that drains from the
condenser within 5 min after the heat has been
315 0.095 0.071 removed.
355 0.100 0.075 Weigh each receiver containing distillate fraction. Note
the mass of each fraction (f1, f2, f3, f4, and f5) and
C.3.3 Thermometers calculate the accumulative distillate as a percentage by
If necessary, make the appropriate adjustments mass of the dehydrated creosote (Mc).
indicated by the thermometer test certificate at any of Reserve the distillate fractions (f1, f2, f3, and f4) for
the specified distillation temperatures (see table 1). testing in accordance with annex D.
C.4 Preparation of test portion of dehydrated C.6 Calculation
creosote Calculate the percentage by mass of each fraction as
Transfer about 120 g of the sample (see BS EN 1014-1) follows:
into the 250 ml untared distillation flask, to which has let f1 be the mass of the fraction distilled up
been added fragments of porous inert material. Using to 205 ÊC;
the type 1 condenser, distil the sample and collect the let f2 be the mass of the fraction distilled
distillate in a separating funnel (C.2.3), stopping the between 205 ÊC and 230 ÊC;
distillation when water ceases to distil. Allow the
contents of the separating funnel to settle, run the let f3 be the mass of the fraction distilled
lower water layer off, and return the oil layer to the between 230 ÊC and 270 ÊC;
distillation flask when the flask has cooled to let f4 be the mass of the fraction distilled
about 40 ÊC. Mix the contents of the flask thoroughly, between 270 ÊC and 315 ÊC;
ensuring that the oil is homogeneous. let f5 be the mass of the fraction distilled
C.5 Procedure between 315 ÊC and 355 ÊC.
Weigh, to an accuracy of 0.1 g, approximately 100 g of Calculate the cumulative distillate up to each of the
the dehydrated creosote (see C.4) directly into the specified temperatures as a percentage by mass of the
tared 150 ml distillation flask. Record this mass as Mc. dehydrated creosote (Mc) as required in table 1, using
Add fragments of porous inert material and assemble the generalized formula:
the distillation apparatus, with the side arm of the flask cumulative percentage to a specific temperature =
extending at least 25 mm beyond the cork in the upper
end of the type 2 condenser.
100 ∑ fn
Mc
for n = 1 to 5, as appropriate.
C.7 Expression of results
Express the cumulative distillate as a percentage by
mass of the dehydrated creosote (Mc) at the specified
temperature.

8  BSI 1997
 BS 144 : 1997

Annex D (normative) Stopper the funnel, shake vigorously for 1 min to 2 min,
and allow to stand. After separation (see note 1), pour
Method for the determination of the alkaline layer into a beaker. Repeat this operation
extractable phenols with successive 25 ml portions of sodium hydroxide
solution (D.2.4) until all the phenols have been
D.1 Principle removed from the oil layer (see notes 1 and 2).
The phenols are extracted from the distillate up to After separation, add the alkaline layers to the first
315 ÊC (obtained from the distillation described in sodium hydroxide washing.
annex C as f1, f2, f3, and f4) with sodium hydroxide.
The neutral oils and bases are removed by boiling. The During the extraction procedure, ensure that the
Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

phenols are liberated by hydrochloric acid and contents of the separating funnel are completely liquid.
measured. If necessary, immerse the funnel in warm water (40 ÊC
to 70 ÊC).
NOTE. The phenols, as recovered, contain water derived from the
reagents used in the test. No correction is made for this water. Take the combined sodium hydroxide washings and
boil for 20 min (using, if necessary, a fragment of inert
D.2 Reagents
material of approximately 2 mm3, to prevent bumping),
NOTE. All reagents should be of recognized analytical grade and and roughly maintain the initial volume by adding
water conforming to grade 3 of BS EN ISO 3696 should be used
throughout.
water. Cool the sodium hydroxide washings to
laboratory temperature and, if clear, transfer them
D.2.1 Hydrochloric acid (HCl), concentrated, 425 g/l. directly to the phenols flask (see note 4). If the
D.2.2 Sodium chloride (NaCl), powdered solid. solution contains suspended matter, filter it through
glass wool moistened with sodium chloride
D.2.3 Sodium chloride solution, saturated. solution (D.2.3) and collect in the 200 ml phenols
flask (D.3.1) (see note 4). Wash the glass wool with a
D.2.4 Sodium hydroxide solution (NaOH), 100 g/l.
further 25 ml of sodium chloride solution and add to
D.2.5 Toluene [C6H5CH3]. the filtered sodium hydroxide washings.
D.2.6 Methyl orange indicator solution, Add a few drops of methyl orange indicator
4-[4±dimethylaminophenylazo]benzenesulfonic acid solution (D.2.6) to the washings, and slowly add
sodium salt, 1 g/l. concentrated hydrochloric acid (D.2.1) until the methyl
orange just indicates distinct acidity, mixing the two
D.3 Apparatus layers by swirling. While adding the hydrochloric acid,
D.3.1 Phenols flask, capacity 200 ml or 150 ml (see keep the contents of the flask cool by immersing it
notes 2 to 5 of D.5), with graduated neck conforming to periodically in cold water.
BS 676. Add just sufficient powdered sodium chloride (D.2.2)
to saturate the aqueous layer and leave a few particles
D.3.2 Separating funnel, capacity 250 ml, stoppered, undissolved. Shake to ensure thorough mixing and
conforming to BS 2021. then stand to allow separation, the phenols forming the
D.3.3 Measuring cylinder, capacity 100 ml, upper liquid layer. Bring the phenols into the graduated
conforming to BS 604. portion of the flask by adding the saturated sodium
chloride solution (D.2.3). After setting (preferably
D.3.4 Thermometer, of range 2 10 ÊC to 110 ÊC, overnight), measure the volume of phenols (see
conforming to BS 593. note 5). Record the volume as Vp.
D.3.5 Glass wool. NOTE 1. Complete removal of the phenols can be verified by
slightly acidifying the final washings with concentrated
D.4 Test portion hydrochloric acid (D.2.1) and examining for separated phenols.
The test portion (see note) shall be obtained by NOTE 2. It may be assumed that 25 ml of sodium hydroxide
solution (D.2.4) is sufficient to remove about 5 ml of phenols.
combining distillate fractions f1 + f2 + f3 + f4, collected
below 315 ÊC (see annex C). NOTE 3. If necessary, the upper layer of the flask may be diluted
with toluene (D.2.5) to secure a satisfactory separation.
NOTE. A known mass (approximately 100 g) of dehydrated
creosote (Mc) will have been distilled to produce the combined NOTE 4. If it is expected that the sample for test contains only a
fractions (f1 + f2 + f3 + f4) which constitute this test portion. small amount of phenols, it is preferable to use about half the
specified volumes of sodium hydroxide solution for the successive
D.5 Procedure washings and to collect the sodium hydroxide washings (after
filtration through the glass wool if necessary) in the 150 ml
If necessary, warm the test portion (see D.4) until phenols flask.
completely liquid, and transfer it to the separating NOTE 5. For some creosotes, measurement of the liberated
funnel (D.3.2). With 50 ml of sodium hydroxide phenols is difficult because of their viscous nature. This may be
solution (D.2.4) (see notes 1 and 2), rinse the receivers overcome by adding a measured volume of toluene (D.2.5) to the
originally containing the test samples into the phenols flask immediately before the final addition of saturated
sodium chloride solution. From the observed volume of the
separating funnel. If the combined samples contain separated upper layer in the phenols flask, subtract the volume of
solids which have separated, warm the separating toluene added.
funnel just sufficiently to redissolve the solids.

 BSI 1997 9
BS 144 : 1997

D.6 Expression of results E.4 Procedure

Express the volume of phenols (Vp), in millimetres, E.4.1 Filling the viscometer
in 100 g of the original sample of dehydrated creosote NOTE. See figure E.1.
(Mc), as follows: Vertically mount the thermometer (E.2.4) in the
Vp 3 100 bath (E.2.3), so that the top of the mercury column is
Mc within 2 mm of the surface of the water. Mount the
clean, dry viscometer (E.2.1) inside the viscometer
D.7 Precision holder (E.2.5) in the bath, in the alignment described
D.7.1 Repeatability in the certificate of calibration. Allow the viscometer to

Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

Duplicate results for the volume of extractable phenols reach bath temperature. Stop tube L with a rubber
obtained by the same operator shall be considered bung fitted with a stopcock or similar device so that
suspect if they differ by more than 0.8 ml. the air can be prevented from escaping. With the
stopcock open, pour the creosote sample (E.3) into the
D.7.2 Reproducibility filling tube N to a point just below the upper filling
Single results for the volume of extractable phenols mark H, without wetting the glass above H. Allow the
obtained at separate laboratories shall be considered sample to flow through the capillary tube R, ensuring
suspect if they differ by more than 2.9 ml. that the creosote column remains unbroken, until it
has reached a position about 5 mm below the lower
filling mark G. Stop the flow of creosote at this point
Annex E (normative) by closing tube L.
Method for the determination of Add more of the sample to the filling tube N to bring
kinematic viscosity the upper surface of the creosote to just below the
mark H. Keep the viscometer in the bath for at
E.1 Principle least 30 min, to allow the sample to reach bath
The kinematic viscosity of a sample of creosote at temperature and for any air bubbles to rise to the
40 ÊC is determined using a U-tube reverse flow surface. With the stopcock, carefully adjust the lower
viscometer. level of the creosote so that its ring of contact with the
glass coincides with the bottom of mark G. Next add
E.2 Apparatus further sample to tube N, until the ring of contact of
E.2.1 U-tube reverse flow viscometers, type BS/IP/RF, the creosote coincides with the bottom of mark H.
conforming to BS 188 : 1977, size 2 (viscosity range Allow time for this additional amount of sample to
2 mm2/s to 10 mm2/s, nominal factor reach bath temperature.
C = 0.01 mm2/s2) and size 3 (viscosity range 6 mm2/s E.4.2 Measurement
to 30 mm2/s, nominal factor C = 0.03 mm2/s2), with Remove the rubber bung from tube L or open the
certificate of calibration. stopcock to allow the creosote to flow under its own
E.2.2 Test sieve, nominal aperture size 75 mm, head. Measure the time for the uppermost ring of
conforming to BS 410. contact of the sample with the glass to rise from the
bottom of mark E to the bottom of mark F. Record the
E.2.3 Water bath, thermostatically controlled, able to thermometer readings before, during, and after the
adjust to (40 ± 0.1) ÊC. timed flow.
NOTE. The temperature control should be such that the bath does NOTE. As some of the sample may remain on the walls of the
not vary by more than 0.01 ÊC during the period of measurement, viscometer between the timing marks, repeat determinations of
over the viscometer or between viscometers. The depth of the flow time may be made only after emptying, cleaning and drying
bath should be such that, when the viscometer and sample are in the viscometer.
position, no part of the sample is less than 20 mm below the
surface of the water, or less than 20 mm above the bottom of the
bath. E.5 Expression of results
E.2.4 Thermometer, total immersion type. Details of The kinematic viscosity of the creosote sample is
suitable thermometers are given in BS 2000 : calculated from the following equation:
Part 0 : Addendum 1. h = Ct
E.2.5 Viscometer holder, to hold the viscometer firmly where
in the thermostatic bath, in the alignment described in h is the kinematic viscosity (mm2/s);
the certificate of calibration. C is the viscometer constant;
E.2.6 Timing device, graduated in divisions of 0.2 s or t is the mean flow time (s).
less, accurate to 0.07 % over 15 min.
E.6 Repeatability
E.3 Preparation of test portion Duplicate results for the kinematic viscosity, obtained
Warm the creosote sample (see BS EN 1014-1) to 45 ÊC by the same operator with the same viscometer, shall
and filter a minimum of 20 ml through the test be considered suspect if the difference is greater
sieve (E.2.2). than 0.35 % of the mean.

10  BSI 1997
 Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

 BSI 1997
Figure E.1 BS/IP/RF U-tube reverse flow viscometer

11
BS 144 : 1997
BS 144 : 1997

Annex F (normative) Annex G (normative)

Method for the determination of water Method for the determination of matter
content insoluble in toluene
F.1 Principle G.1 Principle
The sample is azeotropically distilled with a suitable A sample of creosote is mixed with toluene and the
solvent, and the water collected and measured. soluble matter filtered out. The remainder is washed,
dried and weighed.
F.2 Reagent

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G.2 Reagent
F.2.1 Solvent, either:
a) toluene [C6H5CH3]; or G.2.1 Toluene [C6H5CH3].
b) xylene [C6H4(CH3)2]. G.3 Apparatus
F.3 Apparatus G.3.1 Beakers, capacity 250 ml, with glass covers.
F.3.1 Measuring cylinder, capacity 100 ml, conforming G.3.2 Filter crucibles, capacity 30 ml, glass or
to BS 604. porcelain, porosity grade P16, conforming to
BS 1752 : 1983.
F.3.2 Dean and Stark condensing and collecting
system, conforming to BS 756 : 1952, type 1, with a 2 ml G.3.3 Measuring cylinder, capacity 100 ml,
receiver. conforming to BS 604.
F.3.3 Round-bottomed flask, capacity 500 ml. G.3.4 Water bath, able to heat to boiling.
F.4 Procedure G.3.5 Laboratory oven, (105 ± 5) ÊC.
Fill the measuring cylinder (F.3.1) to the 100 ml mark G.3.6 Desiccator, with silica gel desiccant.
with thoroughly mixed sample (see
BS EN 1014 : Part 1) at laboratory temperature (or at G.3.7 Analytical balance.
the lowest temperature of complete liquidity if above G.3.8 Stainless steel filter, mesh size 150 mm,
laboratory temperature), and transfer it to the conforming to BS 410.
flask (F.3.3). Wash the measuring cylinder with
successive quantities of solvent (F.2.1), using 100 ml G.4 Procedure
altogether, and add the washings to the flask. Add a Dry a filter crucible (G.3.2) in the oven at 105 ÊC, cool
fragment of porous inert material and connect the flask in the desiccator and weigh to the nearest 0.1 mg.
to the Dean and Stark condensing and collecting Repeat until successive weighings do not differ by
system (F.3.2). more than 0.2 mg. Record the mass of the crucible
Heat the flask so that the condensate falls from the (m1).
end of the condenser at a rate of 2 drops/sec Pour 25 g to 30 g of thoroughly mixed sample (see
to 5 drops/sec. Continue the distillation until condensed BS EN 1014-1) through the stainless steel filter (G.3.8)
water is no longer visible in any part of the apparatus into a beaker (G.3.1), weigh to the nearest 0.1 g and
(except at the bottom of the graduated tube), and the record the mass of the sample (m2). Add 100 ml of
volume of collected water remains constant. Record toluene (G.2.1) to the beaker, place a glass cover on
the volume of water in the graduated tube. the beaker, and heat on the boiling water bath.
If a ring of condensed water persists in the condenser Cautiously stir the contents of the beaker with the
tube, clean the condenser and repeat the glass rod. When the sample has dissolved, cover the
determination. beaker and leave on the water bath for about 10 min to
allow the greater part of the insoluble matter to settle.
F.5 Expression of results
Heat approximately 200 ml of toluene (G.2.1) on the
The water content, as a percentage by volume, is equal water bath (80 ÊC to 100 ÊC) for washing purposes.
to the volume, in millimetres, of water in the graduated
tube. Decant the supernatant solution in the beaker through
the filter crucible, using gentle suction to assist
filtration. With the hot toluene, quantitatively transfer
the insoluble matter to the crucible and rinse out the
beaker. Wash the filter and its contents three or four
times using the remainder of the hot toluene.
Dry the crucible in the oven at 105 ÊC, cool in the
desiccator and weigh to the nearest 0.1 mg. Repeat
until successive weighings do not differ by more
than 0.2 mg. Record the final mass of the crucible (m3).

12  BSI 1997
 BS 144 : 1997

G.5 Expression of results H.3 Apparatus

Calculate the matter insoluble in toluene as a H.3.1 Gas chromatograph, fitted with a flame
percentage by mass of the sample using the following ionization detector and heated injection port with
equation: sample splitter, and the following:
a) a column temperature range of 130 ÊC to 200 ÊC;
(m3 2 m1) 3 100 b) the injection port temperature set at 200 ÊC
m2 to 250 ÊC;
c) a silica capillary column, approximately 25 m in
length and 0.2 mm ID, coated with methyl silicone
Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

where
gum (OV1);
m1 is the mass of the crucible (g); d) a potentiometric strip chart recorder with
m2 is the mass of the test portion (g); minimum chart width of 200 mm and maximum
m3 is the mass of the crucible and residue after response time of 1 s.
NOTE. An electronic integrator may be used either in addition or
drying (g). as an alternative to the chart recorder.
H.3.2 Micro-pipette, syringe type, suitable for
Annex H (normative) accurately injecting 1 ml portions into the gas
chromatograph.
Method for the determination of
H.3.3 Micro-pipette, syringe type, able to accurately
naphthalene content by gas measure 100 ml.
chromatography
H.3.4 Analytical balance.
H.1 Principle H.3.5 One-mark volumetric flasks, capacity 10 ml,
A toluene solution of the creosote sample is analysed conforming to BS 1792.
by gas chromatography using a flame ionization
H.4 Calibration solutions
detector, and the response compared with that of a
standard naphthalene solution. Prepare duplicate calibration solutions of
approximately the same composition by the following
H.2 Reagents and materials procedure.
NOTE. All reagents should be checked for purity by passing a Add approximately 0.1 g of naphthalene (H.2.5) to a
sample through the chromatograph under the conditions of the tared 10 ml one-mark volumetric flask (H.3.5), stopper
determination (see H.6). If a response is obtained on the
chromatogram that is likely to cause significant errors in the the flask, and weigh to the nearest 0.0002 g. Add
determination on the test sample, then the reagent or material carefully, from a syringe, 10 ml
should be rejected. of 1,2,3,4-tetrahydronaphthalene (H.2.6), replace the
H.2.1 Carrier gas, nitrogen (N2), oxygen-free. stopper, and re-weigh. Dilute to the mark with
toluene (H.2.3).
H.2.2 Detector gases, hydrogen (H2) and compressed H.5 Column performance solution
air, to be used as directed by the manufacturers of the
gas chromatograph. Take approximately 0.01 g of naphthalene (H.2.5),
weigh accurately and transfer quatitatively to a 10 ml
H.2.3 Toluene [C6H5CH3], giving no peaks that one-mark volumetric flask (H.3.5). Take
coincide with those of naphthalene or tetralin when approximately 0.10 g of benzo[b]thiophene (H.2.4),
1 ml (see note) is analysed by gas chromatography. weigh accurately and transfer quantitatively to the
NOTE. Some sample splitters may require a different injection same 10 ml one-mark volumetric flask (H.3.5). Add
volume to 1 ml. In these cases, account should be taken using the toluene (H.2.3), first to dissolve, then to make up to
procedure given in H.6.1.3. the mark.
H.2.4 Benzo[b]thiophene (thionaphthalene), of a H.6 Procedure
purity such that, when used in the column NOTE. Throughout this procedure all solutions are analysed by
performance solution (H.5), and the solution is injecting 1 ml samples into the gas chromatograph (see also the
analysed by gas chromatography, there are no note to H.2.3).
additional peaks between the main, single peaks of H.6.1 Setting up the gas chromatograph
naphthalene and benzo[b]thiophene. H.6.1.1 Oven conditions
H.2.5 Naphthalene [C10H8], minimum melting For all analyses, maintain the column oven at 130 ÊC
point 79.6 ÊC. until the benzo[b]thiophene has been eluted. Then raise
the oven temperature to 200 ÊC (either manually or by
H.2.6 1,2,3,4-tetrahydronaphthalene (tetralin) a temperature programmer) and maintain at this
[C6H4(CH2)3CH2], showing no peaks that coincide with temperature until the rest of the sample has been
those of naphthalene by gas chromatography. eluted. Reset the oven to 130 ÊC, allowing sufficient
time for the temperature to equilibrate before running
the next sample.

 BSI 1997 13
BS 144 : 1997

H.6.1.2 Carrier gas Measure the heights of the naphthalene

Adjust the carrier gas flow to give a retention time for and 1,2,3,4-tetrahydronaphthalene peaks from the
naphthalene of 15 min to 20 min. chromatograms (or take the equivalent values from an
integrator). Calculate the calibration factor fn for each
H.6.1.3 Detector signal solution, from the formula:
If using a strip chart recorder, adjust the detector
signal to give a naphthalene peak height of 50 % to 99 % Ht m
of full-scale deflection. fn = 3 n
Hn mt
H.6.1.4 Column performance

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NOTE. The criteria in a), b), and c) should be checked during the where
adjustments to the chromatograph described in H.6.1.1, H.6.1.2
and H.6.1.3. Ht is the peak height (or integrator reading)
Satisfy the following before the column is used for of 1,2,3,4-tetrahydronaphthalene;
analysis: Hn is the peak height (or integrator reading) of
a) that peaks to be measured are symmetrical, i.e. naphthalene;
show no obvious tailing; mt is the mass of 1,2,3,4-tetrahydronaphthalene
b) that the number of theoretical plates measured on in 10 ml of solution (g);
the naphthalene peak is not less than 5000. The mn is the mass of naphthalene in 10 ml of
theoretical plate number (n) is calculated from the solution (g).
equation:
n = 16 (retention time/peak width)2 Determine the mean of the two factors.
where both retention time and peak width are
measured in length terms directly from the recorder
chart; H.6.3 Analysis
c) that the separation between naphthalene and If the approximate naphthalene content is not known,
benzo[b]thiophene is such that the trough ratio is weigh 0.20 g of the test sample (see BS EN 1014-1) into
less than 0.2. The trough ratio is determined by a one-mark volumetric flask, dilute to 10 ml with
dividing the height of the trough between two toluene (H.2.3) and analyse 1 ml of the solution by
partially resolved peaks by the height of the smaller chromatography under the same conditions as for the
of the two peaks, both measurements being made calibration (H.6.2).
from the baseline. NOTE. If the test sample requires warming to dissolve solid
matter before analysis, care should be taken that volatile
H.6.2 Calibration constituents are not lost.
Analyse in turn 1 ml of each of the duplicate calibration Measure the peak height for naphthalene and compare
solutions by chromatography (H.4), applying the this with the peak heights obtained from the
conditions described in H.6.1 to obtain separate calibration solutions. Calculate the approximate
chromatograms. naphthalene content.
Weigh a test portion containing 0.05 g to 0.1 g of
naphthalene into a tared 10 ml one-mark volumetric
flask and dilute to the mark with toluene. Inject 1 ml of
this solution into the chromatograph to obtain the first
chromatogram. Weigh the flask and add 100 ml
of 1,2,3,4-tetrahydronaphthalene as in the calibration.
Shake and re-weigh the flask, and inject 1 ml of this
solution into the chromatograph to obtain the second
chromatogram.

14  BSI 1997
 BS 144 : 1997

H.6.4 Measurement of peak heights Annex I (informative)

Draw in the peak base for each relevant peak on the
chromatogram, and measure the vertical distance
Guidance on the methods of treatment of
between the peak base and the apex of the peak. timber
NOTE. The peak base is defined as the interpolation line drawn Introduction
between the start and the finish of the peak, and represents the
base line that the chromatogram would have followed if the This annex gives guidance on the methods that can be
sample component forming the peak had not been present. used for the treatment of timber with creosote.
Record the peak heights for naphthalene The method to select depends on the end use of the
and 1,2,3,4-tetrahydronaphthalene in the second treated timber and the penetration and retention of
Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

chromatogram, and for naphthalene and any coincident creosote required by the specifier.
peak at the 1,2,3,4±tetrahydronaphthalene retention NOTE. Guidance on the treatment of timber with preservatives
time in the first chromatogram. and an introduction to the European Standards for wood
preservation is given in BS 1282 and DD239 (in preparation).
H.7 Expression of results
I.1 Condition and preparation of timber for
The naphthalene content of the test sample, as a
treatment
percentage by mass, is given by the following formula:
Naphthalene content = I.1.1 Moisture content
(Hn1 + Hn2) mt Unless otherwise specified, or when using the Boulton
3 3 100fn process (see I.2.6.5), the average moisture content of
2ms (Ht2 2 Ht1)
the timber should not exceed 28 % (m/m) on an oven
dry basis.
where
The Boulton process can be used on green or
fn is the calibration factor; unseasoned timber, to ensure a moisture content of
mt is the mass of 1,2,3,4-tetrahydronaphthalene 28 % (m/m) or lower before continuing with a full cell
added (g); or empty cell process.
ms is the mass of sample taken (g); NOTE. If timber is frozen, the penetration power of preservative is
limited, so treatment should not be carried out in this condition.
Hn1 is the height of the naphthalene peak (or
integrator reading) in the first chromatogram I.1.2 Incising
(mm); If incising the timber is specified, incisions should be
Hn2 is the height of the naphthalene peak (or made parallel to the general direction of the grain.
integrator reading) in the second Incisions (usually of up to 20 mm in length) should
chromatogram (mm); penetrate to a depth of approximately 20 mm, and
should be spaced 25 mm apart across the timber, in
Ht1 is the height of the peak (or integrator rows extending across all faces of the timber. The
reading) at the 1,2,3,4-tetrahydronaphthalene distance between each row along the timber should
retention time in the first chromatogram be 60 mm, and incisions in adjacent rows should not
(mm); be in direct line but staggered at intervals of
Ht2 is the height of the approximately 6 mm (i.e. incisions in every fourth row
1,2,3,4-tetrahydronaphthalene peak (or are in direct line, see figure I.1).
integrator reading) in the second NOTE 1. Sawn timbers rated as resistant to preservative (e.g.
chromatogram (mm). Douglas fir), of thickness 75 mm or more, and intended for
exterior use, can benefit from incising before treatment.
If Ht1 = 0, the formula simplifies to: NOTE 2. For definitions of resistant or extremely resistant timber,
(H + Hn2) m refer to BS EN 350±1 and BS EN 350-2.
Naphthalene content = n1 3 t 3 100fn
2ms Ht2

 BSI 1997 15
BS 144 : 1997

I.2 Processing by pressure impregnation with expressed rather than the treatment process. The result
creosote types 1, 2 or 4 is described in terms of the preservative penetration
into the wood, and the retention of the wood
I.2.1 General
preservative in the defined analytical zone.
Many different schedules for applying creosote under NOTE 1. It is anticipated that penetration and retention
pressure have been devised; each requires the timber requirements may be routinely achieved through a defined
to be contained in a pressure cylinder and uses hot treatment process, provided that it has been established that the
creosote with varying combinations of time, defined process is able to produce treated timber with the
required penetration and retention values.
temperature, pressure and vacuum. Details of the most
NOTE 2. Guidance on methods for sampling treated timber to

Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

commonly used processes in the UK are given
determine penetration and retention values is presented in
in I.2.6.2, I.2.6.3 and I.2.6.4. An associated process BS EN 351-2.
that may be used to condition green or unseasoned
timber prior to pressure impregnation, the Boulton I.2.5.2 Penetration
process, is described in I.2.6.5. Listed in BS EN 351-1 are nine penetration classes that
Full cell processes are normally used where high can be used to specify penetration, starting from
absorption of creosote is required or where P1 (no penetration requirement) to P9 (full sapwood
impermeable species are being treated. After treatment, penetration and a minimum of 6 mm penetration of
the timber cells are nearly full of creosote, which may exposed heartwood).
give rise to exudation of free creosote on the surface I.2.5.3 Retention
of the timber when in service.
The average retention for the charge, determined at the
Empty cell processes are normally used when analytical zone (according to BS EN 351-1), should be
permeable species are being treated, and the high not less than that specified. Retention values are based
absorption resulting from a full cell process is not upon the critical value of the preservative for the
necessary. After treatment, the timber cells contain hazard class concerned (see BS EN 599-1).
almost no creosote, minimizing exudation of creosote
on the surface. I.2.6 Treatment schedules
I.2.2 Stacking in the cylinder I.2.6.1 General
The timber should be stacked in the cylinder so that The timber should be treated with coal tar creosote of
the creosote can reach all surfaces. If necessary, the type 1, type 2 or type 4, using one of the procedures
timber should be separated by sticks or laths. described in I.2.6.2 to I.2.6.4, subject to any additional
NOTE 1. Consideration of stacking is particularly important when requirements of the user.
planed timber is to be treated. The Boulton process (see I.2.6.5) is essentially a
NOTE 2. Only timbers of the same species and similar conditioning process, and is particularly applicable to
cross-sectional areas should be treated in the same charge, and treatment of unseasoned timber. Immediately following
differing timbers should be separated unless the most intense
schedule can be applied without detriment to the more easily treatment by this process, timber can be further
treated timbers. treated using one of the processes detailed in I.2.6.2
to I.2.6.4.
I.2.3 Applied pressure and temperature
NOTE. The Boulton process is a very severe treatment process,
The applied pressure should be a gauge pressure not and unless extreme caution is exercised, breakdown of the timber
lower than 10 bar and not higher than 14 bar. During structure may occur. The process should only be used with prior
the pressure period, the minimum temperature for agreement with the customer.
type 1 and type 2 creosote should be 65 ÊC and the I.2.6.2 Full cell (Bethel) process
maximum temperature should be 100 ÊC. In the Bethel process, timber is enclosed in a pressure
For type 4 creosote the minimum temperature should cylinder, and a vacuum of at least 2 0.75 bar applied.
be 90 ÊC and the maximum 125 ÊC. Hot creosote is introduced into the cylinder until the
I.2.4 Pressure period cylinder is full, and the vacuum is then released.
The pressure period should be measured from the time Next, a pressure of sufficient magnitude (see I.2.3) is
the specified maximum working pressure (I.2.3) is applied and maintained long enough to ensure that the
reached. Pressure should be maintained until the requirements regarding penetration and retention
required penetration and retention has been achieved. (see I.2.5) are met.
The pressure is released and the cylinder emptied of
I.2.5 Penetration and retention creosote. Finally, a vacuum of not less than 2 0.75 bar
I.2.5.1 General is applied so that the timber is substantially free from
The method that should be used by specifiers to surplus creosote before removal from the cylinder.
describe the quality of treatment required in
preservative-treated timber is given in BS EN 351. This
method requires the result of the treatment to be

16  BSI 1997
 Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI
 BSI 1997

Dimensions in millimetres (approx.)

Figure I.1 Example spacing of incisions

BS 144 : 1997
17
BS 144 : 1997

I.2.6.3 Empty cell (Rueping) process allowed to cool. On cooling, the remaining air in the
In the Rueping process, timber is enclosed in a timber contracts and the vapour pressure decreases,
pressure cylinder, and an air pressure greater than creating a partial vacuum that draws the creosote into
atmospheric pressure but not exceeding 4 bar applied. the wood.
While the gauge pressure is maintained, hot creosote is Caution. Naked flames should not be used for
introduced into the cylinder until the cylinder is full. heating. Smoking and other potential sources of
The pressure is increased to a sufficient magnitude and ignition should be avoided, because the creosote may
maintained for long enough to ensure that the be heated above its flash point.
requirements regarding retention and penetration NOTE 1. Practically all of the creosote absorption takes place

Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

(see I.2.5) are met. during the cooling period. For this reason, equivalent results are
not obtained if the timber is merely immersed in the hot
The pressure is then released and the cylinder emptied preservative for steeping.
of creosote. A final vacuum of not less than 2 0.75 bar NOTE 2. Permeable species often absorb much more creosote
is applied for a sufficient period to ensure that the air than necessary. Excess creosote can be removed by reheating the
in the cylinder has expanded and forced out any free charge to 85 ÊC to 95 ÊC for about 1 h, then removing the timber
creosote from the cells of the timber, reducing the while still hot. During reheating, up to 50 % of the retained
creosote is expelled.
creosote retention.
NOTE. With most permeable timber, creosote retention can be I.3.3 Variations
raised by lowering the initial air pressure. I.3.3.1 It is permissible to vary the hot-and-cold open
I.2.6.4 Empty cell (Lowry) process tank method in a number of ways. For example,
The procedure for the Lowry process is the same as cooling can be achieved more quickly by transferring
for the Rueping process (I.2.6.3), except that the air in the timber to a tank of cold preservative, or the timber
the cylinder is maintained at atmospheric pressure can be preheated for 1 h or 2 h by any convenient
until the cylinder is full. alternative means, such as with hot air, before
NOTE. Creosote retention by the Lowry process is normally higher transferring into cold creosote.
than with the Rueping process. I.3.3.2 A convenient but less efficient variation of the
I.2.6.5 Boulton process (boiling under vacuum) hot-and-cold open tank method, used to treat small
In the Boulton process, timber is enclosed in a numbers of fence posts, is the butt-treatment process.
pressure cylinder, and sufficient hot creosote The fence posts are placed upright in a drum with only
introduced to immerse the timber but ensuring that an their ends immersed in the creosote, therefore covering
air space is left. A vacuum is applied to the cylinder the part of the post which will be in or near the
and a sufficiently high temperature maintained so that ground, and then heated and cooled as described
the water in the timber boils under the vacuum. before.
The boiling water vapour is condensed and measured I.4 Processing by brushing and immersion
in a suitable receiver. When sufficient water has been I.4.1 Treatment materials
extracted to achieve the required moisture content in The treatment material should be coal tar creosote
the timber, the process is halted by releasing the conforming to type 3.
vacuum and emptying the creosote from the cylinder. I.4.2 Brushing
NOTE. This treatment can be followed immediately by pressure
NOTE 1. Brushing is the easiest but generally the least effective
impregnation using any of the processes detailed in I.2.6.2 method of applying wood preservatives.
to I.2.6.4.
NOTE 2. In situ brush treatment of outdoor timber is best carried
I.3 Processing by hot-and-cold open tank with out between late spring and early autumn, after a period of dry
creosote types 1, 2 or 3 weather, when the surface of the timber is warm and dry. The
timber is then in its most absorbent state, and the higher
I.3.1 Treatment materials prevailing temperatures aid penetration. It is advisable to re-treat
The treatment material should be coal tar creosote the timber periodically.
conforming to either type 1, type 2 or type 3. The creosote should be applied liberally and the timber
I.3.2 General method allowed to absorb as much as possible, particularly
into the sapwood and end grain. It is essential to cover
The hot-and-cold open tank process can be carried out the whole of the surface thoroughly and to ensure that
in any convenient open tank or drum suitable for the the creosote penetrates into all the splits and surface
size and quantity of wood to be treated. It is essential checks. More than one coating should be applied and
to provide some means of lifting the timber in and out the timber allowed to dry between applications.
of the tank, and to ensure that the timber is completely
submerged in the creosote during treatment. The I.4.3 Immersion
timber is immersed in the creosote and then heated The timber should be submerged in cold preservative
safely to (90 ± 5) ÊC (see caution), causing air to be for the period required by the appropriate commodity
extracted from the timber by expansion (the vapour specification.
pressure within the wood also increases, expelling NOTE. The efficiency of this method largely depends on the
species, sapwood content and period of immersion. Fairly deep
further air). The temperature is maintained for at penetration may be obtained with some species of timber if left in
least 1 h, depending on the size and permeability of the the preservative for several days or even weeks. Resistant timbers,
timber, after which the creosote and timber are however, will merely show surface penetration.

18  BSI 1997
 Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

blank
19
BS 144 : 1997

List of references

Normative references

BSI publications
BRITISH STANDARDS INSTITUTION, London

BS EN 1014 : Wood preservatives Ð Creosote and creosoted timber ÐMethods of

sampling and analysis

Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

BS EN 1014-1 : 1995 Procedure for sampling creosote
DD ENV 1014-3 : 1996 Determination of the benzo[a]pyrene content of creosote
BS EN 1014-4 : 1996 Determination of the water extractable phenols content of creosote
BS EN 22719 : 1994 Methods of test for petroleum and its products ÐPetroleum
products and lubricants Ð Determination of flash point Ð
Pensky-Martens closed cup method
BS EN ISO 3696 : 1995 Water for analytical laboratory use Ð Specification and test
methods
BS 188 : 1977 Methods for determination of the viscosity of liquids
BS 410 : 1986 Specification for test sieves
BS 593 : 1989 Specification for laboratory thermometers
BS 604 : 1982 Specification for graduated glass measuring cylinders
BS 658 : 1989 Specification for apparatus for the determination of distillation
range (including flasks and receivers)
BS 718 : 1991 Specification for density hydrometers
BS 756 : 1952 Specification for Dean and Stark apparatus
BS 1752 : 1983 Specification for laboratory sintered or fritted filters including
porosity grading
BS 1792 : 1982 Specification for one-mark volumetric flasks
BS 2000 : Methods of test for petroleum and its products
BS 2000 : Part 0 : Standard reagents and thermometers
Addendum 1 : 1987
BS 2021 : 1980 Specification for separating and dropping funnels for laboratory
use

20  BSI 1997
 BS 144 : 1997

Informative references

BSI publications
BRITISH STANDARDS INSTITUTION, London

BS EN 350 : Durability of wood and wood-based products Ð Natural

durability of solid wood
BS EN 350-1 : 1994 Guide to the principles of testing and classification of natural
Licensed Copy: Giorgio Cavalieri, ALSTOM, 15-Mar-01, Uncontrolled Copy. © BSI

durability of wood
BS EN 350-2 : 1994 Guide to natural durability and treatability of selected wood
species of importance in Europe
BS EN 351 : Durability of wood and wood-based products Ð
Preservative-treated solid wood
BS EN 351-1 : 1996 Classification of preservative penetration and retention
BS EN 351-2 : 1996 Guidance on sampling for the analysis of preservative±treated
wood
BS EN 599 : Durability of wood and wood-based products Ð Performance of
preventive wood preservatives as determined by biological tests
BS EN 599-1 : 1997 Specification according to hazard class
BS 1282 : 1975 Guide to the choice, use and application of wood preservatives
DD 2391) Code of practice for preservation of timber

1) In preparation.

 BSI 1997
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