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© BSI 2009
ICS 29.040.10
Publication history
First published April 1923
First revision May 1927
Second revision April 1933
Third revision January 1951
Fourth revision April 1959
Fifth revision December 1972
Sixth revision September 1984
Seventh revision October 1997
Eighth revision July 1998
Ninth (latest) revision February 2009
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Contents
Foreword ii
1 Scope 1
2 Normative references 1
3 Terms and definitions 2
4 Identification and delivery 3
5 Sampling 3
6 Properties of the oils 3
7 Test methods 4
Annexes
Annex A (normative) Analysis method for determination of
passivators in mineral oils by high performance liquid
chromatography (HPLC) 8
Bibliography 16
List of figures
Figure A.1 – UV spectra of TTAA and BTA 13
List of tables
Table 1 – Uninhibited mineral insulating oils 6
Table 2 – Inhibited mineral insulating oils 7
Table A.1 – Examples of separation condition 12
Table A.2 – Repeatability 15
Table A.3 – Reproducibility 15
Summary of pages
This document comprises a front cover, an inside front cover,
pages i to ii, pages 1 to 16, an inside back cover and a back cover.
Foreword
Publishing information
This British Standard is published by BSI and came into effect on
28 February 2009. It was prepared by Technical Committee GEL/10, Fluids
for electrotechnical applications. A list of organizations represented on
this committee can be obtained on request to its secretary.
Supersession
This British Standard supersedes BS 148:1998, which is withdrawn.
BS 148:1998 was the specification for unused and reclaimed mineral
insulating oil for transformers and switchgear. The specification for
unused mineral insulating oil is now covered in BS EN 60296. Due to
the continued market requirement for reclaimed oil to an agreed
specification, BS 148 is now dedicated to reclaimed mineral insulating
oil only.
Presentational conventions
The provisions of this standard are presented in roman (i.e. upright)
type. Its requirements are expressed in sentences in which the
principal auxiliary verb is “shall”.
Commentary, explanation and general informative material is presented
in smaller italic type, and does not constitute a normative element.
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British standard BS 148:2009
1 Scope
This British Standard specifies requirements for reclaimed oxidation
inhibited and uninhibited mineral insulating oils, as delivered, for use
in transformers, switchgear and similar electrical equipment in which
oil is required as an insulant or for heat transfer.
Oils with and without additives are within the scope of this standard.
This standard does not differentiate between the methods used to
reclaim used mineral insulating oil; thus it is also applicable to oils
having undergone a re‑refining process.
This standard does not apply to mineral insulating oils used as
impregnates in cables or capacitors, or to hydrocarbon insulating
liquids obtained by synthesis.
NOTE 1 Oils conforming to the requirements of this standard, and
containing no additives, are considered to be compatible with one
another and can be mixed in any proportion. This does not necessarily
apply to oils containing additives, and where the user wishes to mix such
oils a check should be made to ensure that the mixture conforms to the
requirements of this standard.
NOTE 2 Reclaimed mineral insulating oil is produced by the processing,
to a greater or lesser extent, of service degraded used mineral insulating
oil. Such oil will have been originally supplied in compliance with either
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BS 148:1998 (or earlier editions) or BS EN 60296. Due to the variability
of service conditions and the changes in original specification since the
first edition of BS 148, reclaimers may reserve the right to reject used oil
if it is considered unsuitable as a feedstock to produce a reclaimed oil in
accordance with this specification.
2 Normative references
The following referenced documents are indispensable for the
application of this document. For dated references, only the edition
cited applies. For undated references, the latest edition of the
referenced document (including any amendments) applies.
BS 2000‑15, Methods of test for petroleum and its products – Part 15:
Petroleum products – Determination of pour point
BS 5263, Method for sampling liquid dielectrics
BS 5984, Method for detection and determination of specified
anti‑oxidant additives in insulating oils
BS EN 60156, Insulating liquids – Determination of the breakdown
voltage at power frequency – Test method
BS EN 60247, Insulating liquids – Measurement of relative permittivity,
dielectric dissipation factor (tan d) and d.c. resistivity
BS EN 60814, Insulating liquids – Oil-impregnated paper and
pressboard – Determination of water by automatic coulometric Karl
Fischer titration
BS EN 61125, Unused hydrocarbon-based insulating liquids – Test
methods for evaluating the oxidation stability
BS EN 61198, Mineral insulating oils – Methods for the determination
of 2‑furfural and related compounds
BS EN 61619, Insulating liquids – Contamination by polychlorinated
biphenyls (PCBs) – Method of determination by capillary column gas
chromatography
1) In preparation.
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British standard BS 148:2009
5 Sampling
Sampling shall be carried out in accordance with BS 5263.
NOTE As a general rule, oil samples should be taken where the oil --`,,,```,,,,```````,`````````,`-`-`,,`,,`,`,,`---
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Reclaimed uninhibited oil shall meet the limiting values in Table 1 and
reclaimed inhibited oil shall meet the limiting values in Table 2.
NOTE 3 Precision data given in the specified methods are to be
used solely as a guide to the expected agreement between duplicate
measurements of the property and are not to be regarded as tolerances
applicable to the limits specified in Table 1 and Table 2.
7 Test methods
7.1 Appearance
To test appearance, a representative sample of the oil shall be examined
in transmitted light under an oil depth of approximately 100 mm and at
ambient temperature.
7.2 Density
Density shall be measured using any recognized standard test method
or, in the event of a dispute, the method specified in BS EN ISO 3675.
Density shall be measured at 20 °C.
NOTE Density values can be converted to 20 °C using Table 59 D
of Petroleum measurement paper No.3: Computer implementation
procedures for correcting densities and volumes to 20 °C [1].
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British standard BS 148:2009
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7.12 Breakdown voltage
Breakdown voltage shall be determined by the method described in
BS EN 60156.
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British standard BS 148:2009
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Passivator content 7.8 Not detectable C)
Water content, mg/kg 7.9
bulk delivery G 20
drum delivery G 30
D)
Anti‑oxidant additives , % 7.10 > 0.08 and < 0.40
Oxidation stability, 500 h 7.11
total acidity, mg KOH per g of oil G 1.2
sludge, % by mass G 0.8
Breakdown voltage, as delivered, kV 7.12 H 30
Dielectric dissipation factor, at 90 °C 7.13 G 0.005
and 40 Hz to 62 Hz
Total PCB content mg/kg 7.14 To be agreed E)
Total furans mg/kg 7.15 < 0.2
A)
The corresponding viscosity value at 20 °C is approximately 40 mm2/s.
B)
A maximum limit for density is specified in an attempt to minimize the risk of ice crystals floating in the oil where
oil‑insulated equipment is exposed to very low temperatures.
C)
Subject to agreement between purchaser and supplier, a metal passivator may be incorporated in the oil to a
maximum concentration of 100 mg/kg as measured by the method given in Annex A.
D)
Methods for the detection and quantitative determination of some anti‑oxidant additives are described in BS 5984.
E)
To be agreed between supplier and purchaser but not more than 10 mg/kg.
NOTE 1 The purchaser might wish to agree with the supplier limits for sulfur content and resistivity at 90 °C.
NOTE 2 A pour point depressant should only be included in the oil formulation if this is agreed between
supplier and purchaser.
NOTE 3 In the present context, “bulk” refers to shipments made in breather‑protected vehicles or containers
and does not apply to oil carried in ships or barges or by pipeline.
A.1 General
This test method covers the determination of passivators
N‑bis(2‑ethylhexyl)‑aminomethyl-tolutriazol (TTAA), Benzotriazole
(BTA) and 5‑methyl‑1H‑benzotriazole (TTA) in mineral oils by high
performance liquid chromatography (HPLC) in used and unused
insulating mineral oils.
NOTE 1 This method is based on an existing method for determination
of BTA, which can be detected in the same chromatographic run of TTAA,
as described in this Annex.
NOTE 2 This test method uses the commercial product of TTAA for
calibration. Its inherent uncertainty is related to the degree of purity
supplied.
NOTE 3 TTAA is commercially available as Ciba® IRGAMET® 39. To
the best of the committee’s knowledge, this is the only commercial
product available at time of publication. This information is given for
the convenience of users of this document and does not constitute an
endorsement by BSI or the committee of this product.
This test method covers the determination of TTAA for routine analysis.
TTAA is an amine derivate of tolutriazole, liquid at room temperature,
added in mineral insulating oils mainly as a metal passivator, for
its capability to inhibit the corrosive reactions involving surfaces of
copper (and other metals) and of metal-reactive compounds present
in the oil. TTAA is usually added to mineral oils in concentrations of
0.005% to 0.02%.
Other triazole derivates are used in insulating mineral oils, such as BTA
and TTA, which have a lower solubility in oil. BTA is more widely used
than TTA, mainly to modify the electrical behaviour of copper surfaces.
TTAA is a mixture of 2 isomers:
N,N‑bis(2‑ethylesil)‑4‑methyl‑1H‑benzotriazol‑1‑methylamine and
N,N‑bis(2‑ethylesil)-5-methyl-1H-benzotriazol-1-methylamine. The two
isomers are not usually separated in the conditions described in this
method, but they might give two partially overlapping peaks if a high
efficiency column is used (C18, 250 mm); in this case the total area of
two peaks shall be considered.
Heavily oxidized oils might partially affect the analysis, giving relevant
interferences from UV‑absorbing polar compounds. In the case of
doubt, the standard addition method can be used for more accurate
determinations.
This method can be used for monitoring TTAA content in passivated
used and unused insulating mineral oils.
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British standard BS 148:2009
A.2 Principles
A.2.1 Summary
A weighed portion of the sample oil is diluted with pentane and
passed under a vacuum through a silica gel solid phase extraction
(SPE) cartridge, previously rinsed with methanol and pentane. The
residue of non-polar oil constituents retained by the solid phase is
eluted with a further volume of pentane and discarded. The cartridge
is then dried by flushing it with air under a vacuum.
The analytes are eluted with a known volume of methanol and
filtered through a 0.45 μm PTFE filter.
The solution is injected into an HPLC system equipped with a
reverse‑phase column, and the TTAA is detected with a UV detector
at a wavelength of 260 nm to 270 nm.
NOTE In order to obtain the optimal separation and detection condition
with individual chromatographic systems, this method allows a large
flexibility in choice of stationary phase and mobile phase separation.
A.2.2 Interferences
TTA has been found to co-elute with TTAA in the conditions described
in this method. TTAA decomposes to TTA during some stage of the
chromatographic run, the UV spectra of the two compounds (recorded
from the chromatogram) being identical.
NOTE It is recommended that the effective co-elution of TTAA and TTA
under the selected separation conditions is verified.
A.3 Equipment
A.3.1 Apparatus
A.3.1.1 Balance, top loading, with automatic tare, capable of weighing
to 0.001 g, capacity of 100 g minimum.
A.3.1.2 Vacuum manifold for SPE, for vacuum elution of silica cartridges.
A.3.1.3 Silica SPE cartridges sorbent substrate silica; sorbent weight:
500 to 1 000 mg; pH range: 2 to 8; particle size: 20 μm to 200 μm.
NOTE The choice of the sorbent weight should be carefully correlated
with the weight of the sample analysed and to the load capacity of the
cartridge. While optimizing the method, a check for analyte recovery is
recommended.
A.3.1.4 PFTE filters, 0.45 μm, Luer plug fitting.
A.3.2.4 Solutions
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British standard BS 148:2009
NOTE 2 Stock solutions of 1 000 mg/kg have been found to be stable for
at least 3 months. If a longer lasting stock is desired, the stability should
be checked by comparison with a fresh solution.
A.4 Sampling
Take laboratory samples in accordance with IEC 60475.
A.5.1.2 UV detection
Detect the TTAA with a UV detector.
NOTE It is recommended that a wavelength of 264 nm is used for
UV detection of TTAA , corresponding to the maximum absorbance (see
Figure A.1). However, a lower wavelength may be used if necessary.
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A.5.2 Calibration
Establish the linear range for the particular instrument being used
and the selected separation procedure.
NOTE The method should show a linear response in a concentration
range of 5 mg/kg to 500 mg/kg.
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British standard BS 148:2009
Key
X axis nm
Y axis AU (absorption unit)
TTAA
BTA
A.6 Analysis
© BSI 2009 • 13
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A.6.3 Calculations
The model obtained during the calibration being y = bx + m, calculate
the result as:
peak area − m
mg/kg (ttaa) =
b
A.7 Report
Report the concentration of TTAA in mg/kg to the nearest whole figure.
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British standard BS 148:2009
A.9.2 Repeatability
Duplicate determinations carried out by one laboratory shall be
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Concentration r (repeatability)
mg/kg %
10 10
> 50 5
A.9.3 Reproducibility
Duplicate determinations carried out by different laboratories shall be
considered suspect at the 95% confidence level if they differ by more
than the value reported in Table A.3 (expressed in percentage of the
average value).
Concentration R (reproducibility)
mg/kg %
10 15
> 50 8
Bibliography
Standards publications
For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including
any amendments) applies.
BS EN 60296, Fluids for electrotechnical applications – Unused mineral
insulating oils for transformers and switchgear
Other publications
[1] THE INSTITUTE OF PETROLEUM. Petroleum measurement paper
No. 3: Computer implementation procedures for correcting
densities and volumes to 20 ºC. October 1988. 3)
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3) Available from Energy Institute, 61 New Cavendish St, London W1G 7AR.
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