SIST EN ISO 4263-3:2006

SLOVENSKI STANDARD
SIST EN ISO 4263-3:2006
01-maj-2006
1DIWDLQVRURGQLSURL]YRGL'RORþDQMHVWDUDQMDLQKLELUDQLKROMLQWHNRþLQ3UHVNXV
7267GHO3RVWRSHNEUH]YRGH]DVLQWHWLþQHKLGUDYOLþQHWHNRþLQH,62

Petroleum and related products - Determination of the ageing behaviour of inhibited oils
and fluids - TOST test - Part 3: Anhydrous procedure for synthetic hydraulic fluids (ISO
4263-3:2006)
Mineralölerzeugnisse und verwandte Produkte - Bestimmung des Alterungsverhaltens
von inhibierten Ölen und Flüssigkeiten - TOST-Verfahren - Teil 3: Wasserfreies
Verfahren für synthetische Druckflüssigkeiten (ISO 4263-3:2006)
Pétrole et produits connexes - Détermination du comportement au vieillissement des
fluides et huiles inhibés - Essai TOST - Partie 3: Méthode anhydre pour les fluides
hydrauliques synthétiques (ISO 4263-3:2006)
Ta slovenski standard je istoveten z: EN ISO 4263-3:2006
ICS:
75.120 +LGUDYOLþQLIOXLGL Hydraulic fluids
SIST EN ISO 4263-3:2006 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 4263-3:2006

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SIST EN ISO 4263-3:2006
EUROPEAN STANDARD
EN ISO 4263-3
NORME EUROPÉENNE
EUROPÄISCHE NORM
February 2006
ICS 75.120

English Version
Petroleum and related products - Determination of the ageing
behaviour of inhibited oils and fluids - TOST test - Part 3:
Anhydrous procedure for synthetic hydraulic fluids (ISO 4263-
3:2006)
Pétrole et produits connexes - Détermination du Mineralölerzeugnisse und verwandte Produkte -
comportement au vieillissement des fluides et huiles Bestimmung des Alterungsverhaltens von inhibierten Ölen
inhibés - Essai TOST - Partie 3: Méthode anhydre pour les und Flüssigkeiten - TOST-Verfahren - Teil 3: Wasserfreies
fluides hydrauliques synthétiques (ISO 4263-3:2006) Verfahren für synthetische Druckflüssigkeiten (ISO 4263-
3:2006)
This European Standard was approved by CEN on 9 January 2006.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the Central Secretariat or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,
Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 4263-3:2006: E
worldwide for CEN national Members.

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SIST EN ISO 4263-3:2006

EN ISO 4263-3:2006 (E)





Foreword


This document (EN ISO 4263-3:2006) has been prepared by Technical Committee ISO/TC 28
"Petroleum products and lubricants" in collaboration with Technical Committee CEN/TC 19
"Petroleum products, lubricants and related products", the secretariat of which is held by NEN.

This European Standard shall be given the status of a national standard, either by publication of
an identical text or by endorsement, at the latest by August 2006, and conflicting national
standards shall be withdrawn at the latest by August 2006.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of
the following countries are bound to implement this European Standard: Austria, Belgium,
Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary,
Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.


Endorsement notice

The text of ISO 4263-3:2006 has been approved by CEN as EN ISO 4263-3:2006 without any
modifications.

2

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SIST EN ISO 4263-3:2006


INTERNATIONAL ISO
STANDARD 4263-3
First edition
2006-02-01

Petroleum and related products —
Determination of the ageing behaviour of
inhibited oils and fluids — TOST test —
Part 3:
Anhydrous procedure for synthetic
hydraulic fluids
Pétrole et produits connexes — Détermination du comportement au
vieillissement des fluides et huiles inhibés — Essai TOST —
Partie 3: Méthode anhydre pour les fluides hydrauliques synthétiques




Reference number
ISO 4263-3:2006(E)
©
ISO 2006

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SIST EN ISO 4263-3:2006
ISO 4263-3:2006(E)
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©  ISO 2006
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
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ii © ISO 2006 – All rights reserved

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SIST EN ISO 4263-3:2006
ISO 4263-3:2006(E)
Contents Page
Foreword. iv
1 Scope . 1
2 Normative references . 1
3 Principle. 2
4 Reagents and materials . 2
5 Apparatus . 3
6 Sampling. 11
7 Preparation of materials and apparatus. 11
8 Procedure . 12
9 Calculation. 13
10 Expression of results . 13
11 Precision. 14
12 Test report . 14
Annex A (normative) Liquid-in-glass thermometer specifications . 15
Annex B (normative) Procedure for packaging and storage of catalyst coils. 16
Annex C (informative) Method for the determination of the insolubles content of mineral oils and
anhydrous synthetic fluids . 17
Annex D (informative) Appearance rating of catalyst coil wires . 19
Annex E (informative) Determination of metals content . 20
Bibliography . 21

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SIST EN ISO 4263-3:2006
ISO 4263-3:2006(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 4263-3 was prepared by Technical Committee ISO/TC 28, Petroleum products and lubricants.
ISO 4263 consists of the following parts, under the general title Petroleum and related products —
Determination of the ageing behaviour of inhibited oils and fluids — TOST test:
⎯ Part 1: Procedure for mineral oils
⎯ Part 2: Procedure for category HFC hydraulic fluids
⎯ Part 3: Anhydrous procedure for synthetic hydraulic fluids
⎯ Part 4: Procedure for industrial gear oils

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SIST EN ISO 4263-3:2006
INTERNATIONAL STANDARD ISO 4263-3:2006(E)

Petroleum and related products — Determination of the ageing
behaviour of inhibited oils and fluids — TOST test —
Part 3:
Anhydrous procedure for synthetic hydraulic fluids
WARNING — The use of this part of ISO 4263 may involve hazardous materials, operations and
equipment. This part of ISO 4263 does not purport to address all of the safety problems associated
with its use. It is the responsibility of the user of this part of ISO 4263 to establish appropriate safety
and health practices and determine the applicability of regulatory limitations prior to use.
1 Scope
This part of ISO 4263 specifies a method for the determination of the ageing behaviour of synthetic hydraulic
[4] [5]
fluids of categories HFDR, HFDU, HEES and HEPG as defined e.g. in ISO 12922 and ISO 15380 . The
ageing is accelerated by the presence of oxygen and metal catalysts at elevated temperature, and the
degradation of the fluid is followed by changes in acid number. Other parts of ISO 4263 specify similar
procedures for the determination of ageing behaviour of mineral oils and specified categories of fire-resistant
fluids used in hydraulic and other applications.
NOTE Other signs of fluid deterioration, such as the formation of insoluble sludge, catalyst coil corrosion or decrease
in viscosity, can occur, which indicate oxidation of the fluid, but are not reflected in the calculated oxidation lifetime. The
correlation of these occurrences with field service is under investigation.
This test method can be used to compare the oxidation stability of fluids that are not prone to contamination
with water. However, because of the large number of individual field-service applications, the correlation
between the results of this test and actual service performance can vary markedly, and is best judged on
experience.
The precision of this test method for synthetic hydraulic fluids is not known because interlaboratory data are
not available. This method might not be suitable for use in specifications or in the event of disputed results as
long as these data are not available. However, precision for inhibited turbine oils is given in Clause 11 for
guidance as an indication of the precision that could be obtained for synthetic hydraulic fluids.
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.
ISO 3170:2004, Petroleum liquids — Manual sampling
ISO 3696:1987, Water for analytical laboratory use — Specification and test methods
ISO 7537:1997, Petroleum products — Determination of acid number — Semi-micro colour-indicator titration
method
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SIST EN ISO 4263-3:2006
ISO 4263-3:2006(E)
3 Principle
A test portion is reacted, in the absence of light, at 95 °C with oxygen and a steel and copper catalyst coil.
Small aliquots of the fluid are withdrawn at regular intervals and the acid number is measured (see the Note in
Clause 1). The test is continued until an acid number increase of 2,0 mg of potassium hydroxide (KOH) per
gram of test portion is reached and the number of hours is recorded as the oxidation life. For some
requirements, the test may be discontinued at a fixed number of hours (e.g. 500 h or 1 000 h) when the value
of the acid number is still below 2,0 mg of KOH per gram of test portion.
4 Reagents and materials
4.1 Water, unless otherwise specified, in accordance with the requirements of grade 2 of ISO 3696:1987.
Potable water means tap water, unless normal piped supplies are contaminated with particulate or highly
soluble mineral content.
4.2 Heptane (C H ), of minimum purity 99,75 %.
7 16
4.3 Acetone (CH COCH ), of general purpose reagent grade (GPR).
3 3
4.4 Propan-2-ol (CH CHOHCH ), of general purpose reagent grade (GPR).
3 3
4.5 Oxygen, of minimum purity 99,5 %, supplied through a pressure-regulation system adequate to
maintain the specified flow rate throughout the test duration.
Supply from an oxygen cylinder should be via a two-stage regulation system and a needle valve to improve
the consistency of gas-flow regulation.
WARNING — Use oxygen only with equipment validated for oxygen service. Do not allow oil or grease
to come into contact with oxygen and clean and inspect all regulators, gauges and control equipment.
Check the oxygen-supply system regularly for leaks. If a leak is suspected, turn off immediately and
seek qualified assistance.
4.6 Cleaning solutions
4.6.1 Strong oxidizing acid solution
The reference strong oxidizing cleaning solution on which precision was based, is chromosulfuric acid (see
the following warning), but alternative non-chromium containing solutions, such as ammonium persulfate in
concentrated sulfuric acid (8 g/l) have been found to give satisfactory cleanliness. A 10 % solution of three
parts of hydrochloric acid (1 mol/l) and one part of orthophosphoric acid (concentrated GPR grade) removes
iron oxide deposits.
WARNING — Chromosulfuric acid is a health hazard. It is toxic, a recognized carcinogen as it contains
Cr(VI) compounds, highly corrosive and potentially hazardous in contact with organic materials. When
using chromosulfuric acid cleaning solution, eye protection and protective clothing are essential.
Never pipette the cleaning solution by mouth. After use, do not pour cleaning solution down the drain,
but neutralize it with great care owing to the concentrated sulfuric acid present, and dispose of it in
accordance with standard procedures for toxic laboratory waste (chromium is highly dangerous to the
environment).
Strongly oxidizing acid cleaning solutions that are chromium-free are also highly corrosive and
potentially hazardous in contact with organic materials, but do not contain chromium which has
special disposal problems.
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SIST EN ISO 4263-3:2006
ISO 4263-3:2006(E)
4.6.2 Surfactant cleaning fluid
A proprietary strong surfactant cleaning fluid is a preferred alternative.
4.6.3 Laboratory detergent
The detergent shall be water soluble.
4.7 Catalyst wires
4.7.1 Low-metalloid steel wire, of diameter 1,60 mm ± 0,05 mm, made of carbon steel, soft bright
annealed and free from rust.
4.7.2 Copper wire, of diameter 1,63 mm ± 0,05 mm, made of either electrolytic copper wire of 99,9 %
minimum purity or soft copper wire of an equivalent grade.
4.8 Abrasive cloth, made of silicon carbide of 150 µm (100-grit) with cloth backing, or an equivalent grade
of abrasive cloth.
4.9 Absorbent cotton
5 Apparatus
5.1 Oxidation cell, consisting of a large test tube of borosilicate glass with a graduation mark to indicate a
volume of 300 ml ± 1 ml at 20 °C. A mushroom condenser and oxygen-delivery tube, also of borosilicate glass,
fit into the test tube. The design and dimensions shall be as illustrated in Figure 1.
5.2 Heating bath, consisting of a thermostatically controlled bath capable of maintaining the hydraulic fluid
test portion in the oxidation cell at 95,0 °C ± 0,2 °C. It shall be large enough to hold the required number of
oxidation cells (5.1) immersed in the heat transfer medium to a depth of 355 mm ± 10 mm. It shall be
constructed to ensure that light is excluded from the test portions during the test. If a fluid bath is used, it shall
be fitted with a suitable stirring system to provide a uniform temperature throughout the bath. If the fluid bath is
fitted with a top, the total length of the oxidation cell within the bath shall be 390 mm ± 10 mm. If a metal-block
bath is used, the heaters shall be distributed so as to produce a uniform temperature throughout the bath, and
the holes in the block shall have a minimum diameter of 50 mm and a depth, including any insulating cover, of
390 mm ± 10 mm.
5.3 Flowmeter, capable of measuring 3,0 l/h with an accuracy of ± 0,1 l/h.
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SIST EN ISO 4263-3:2006
ISO 4263-3:2006(E)
Dimensions in millimetres (unless otherwise indicated)


b) First stage c) Second stage



a) Apparatus d) Final stage
Key
a
1 glass condenser 4 catalyst coil
Bend over mandrel of diameter 26.
b
2 oxygen-delivery tube 5 radius of bottom cell
Grind end of tube.
c
3 fluid sample
External diameter.
Figure 1 — Oxidation cell
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SIST EN ISO 4263-3:2006
ISO 4263-3:2006(E)
5.4 Temperature-measurement devices
5.4.1 Heating bath. The temperature in liquid heating baths shall be measured by either a liquid-in-glass
thermometer meeting the requirements of the specification given in Annex A, or an equivalent temperature-
measurement system readable to ± 0,1 °C and graduated in 0,1 °C increments. For metal-block heating baths,
a temperature-measurement system, with possibly more than one device of the same readability and
accuracy, is required.
5.4.2 Oxidation cell. The temperature in the oxidation cell shall be measured by either a liquid-in-glass
thermometer meeting the requirements of the specification given in Annex A, or an equivalent temperature-
measurement system readable to ± 0,1 °C and calibrated to better than ± 0,1 °C.
5.4.3 Thermometer bracket. If a liquid-in-glass thermometer is used in the oxidation cell, it shall be
suspended by means of a bracket as illustrated in Figure 2. The thermometer is held in the bracket by either
two fluoro-elastomer O-rings of approximately 5 mm diameter, or by the use of thin stainless steel wire.
5.5 Wire-coiling mandrel, as illustrated in Figure 3, is used to produce the double spiral of copper and
steel wire. The mandrel is included in a suitable winding device.
5.6 Oxygen-supply tube, flexible polyvinylchloride (PVC) tubing of approximately 6,4 mm inside diameter
and 1,5 mm wall thickness, is required to deliver oxygen to the oxidation cell.
5.7 Aliquot-removal devices. Depending on the size and frequency of removal of aliquots of the test
portion for analysis, a selection of devices are required. Glass syringes, fitted with Luer connectors and
stainless steel needles, or long pipettes fitted with suitable pipette fillers, are suitable. These may be inserted
via a sampling tube (5.9) fitted through the condenser. Aliquot sizes will generally be in the range of 2 ml to
10 ml, and the devices shall be capable of removing the required aliquot ± 0,2 ml.
5.8 Aliquot containers. Small, dark glass vials of 5 ml to 10 ml capacity, fitted with close-fitting
polyethylene caps, are required.
5.9 Sampling tube. Stainless steel tubing, 2,11 mm in outside diameter, 1,60 mm in inside diameter,
610 mm ± 2 mm long, with one end finished at 90° and the other end fitted with an optional female Luer
connector (if using syringes as aliquot-removal devices (5.7)). The optional connector is preferably of
elastomeric material such as poly(fluorovinyl chloride) to provide a good seal with the syringe.
5.10 Stopper, for the optional Luer fitting of the sampling tube (5.9), made of polytetrafluoroethylene (PTFE)
or poly(fluorovinyl chloride).
5.11 Sampling tube holder, for supporting the sampling tube (5.9), made of methyl methacrylate resin,
having the dimensions shown in Figure 4.
5.12 Sampling tube spacer, for positioning the end of the sampling tube (5.9) above the sampling tube
holder (5.11), made of plastic tubing of poly(vinyl chloride), polyethylene, polypropylene, or
polytetrafluoroethylene, having an inside diameter of approximately 3 mm and 51 mm ± 1 mm in length.
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SIST EN ISO 4263-3:2006
ISO 4263-3:2006(E)
Dimensions in millimetres


a) Bracket (finished) b) Development of bracket

Material:18/8 (0,792 mm) stainless steel
Figure 2 — Thermometer bracket
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SIST EN ISO 4263-3:2006
ISO 4263-3:2006(E)
Dimensions in millimetres
(unless otherwise indicated)



Figure 3 — Catalyst coil mandrel
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SIST EN ISO 4263-3:2006
ISO 4263-3:2006(E)
Dimensions in millimetres
(unless otherwise indicated)




Figure 3 — Catalyst coil mandrel (continued)
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SIST EN ISO 4263-3:2006
ISO 4263-3:2006(E)
Dimensions in millimetres
(unless otherwise indicated)

Key
1 1/4″ Whitworth × 12,7 hexagon head steel screw (or equivalent)
2 5/16″ Whitworth × 12,7 hexagon head steel screw (or equivalent)
3 vice jaws
4 2BA steel grub screw (or equivalent)
5 catalyst wires
a
Material: steel.
b
Material: brass.
c
Material: bronze.
d
Holes (2) tap 5/8″ Whitworth (or equivalent).
e
Hole tap 2BA (or equivalent).
f
Pitch.
g
Pitch height.
h
Hole tap 1/4″ Whitworth (or equivalent).
i
6 TPI double thread.
Figure 3 — Catalyst coil mandrel (continued)
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SIST EN ISO 4263-3:2006
ISO 4263-3:2006(E)
Dimensions in millimetres
(unless otherwise indicated)

Figure 4 — Sampling tube holder

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SIST EN ISO 4263-3:2006
ISO 4263-3:2006(E)
6 Sampling
Unless otherwise specified, samples shall be obtained by the procedures described in ISO 3170.
7 Preparation of materials and apparatus
7.1 Cleaning the catalyst wire
Immediately prior to winding a catalyst coil, clean a 3,00 m ± 0,01 m length of steel wire (4.7.1) and an equal
length of copper wire (4.7.2) with wads of absorbent cotton (4.9) soaked in heptane (4.2), and then abrade
with the abrasive cloth (4.8) until a fresh metal surface is exposed. Wipe with dry absorbent cotton until all
loose particles of metal and abrasive have been removed. In all subsequent operations, handle the catalyst
wires with clean gloves (cotton, rubber or plastic) to prevent contact with the skin.
7.2 Preparation of catalyst coil
Twist the steel and copper wires together tightly at one end for three turns and then wind them simultaneously
alongside each other on a threaded mandrel (5.5 and Figure 3), inserting the steel wire in the deeper thread.
Twist the free ends of the steel and copper wires together for three turns and bend the twisted ends to
conform to the shape of the spiral coil. Remove the coil from the mandrel by reversing the winding action.
Ensure that the overall length of the coil is 225 mm ± 5 mm by stretching or compression if necessary.
7.3 Storage of the catalyst coil
Store the catalyst coil in a dry inert atmosphere prior to use, in accordance with the procedures described in
Annex B. Inspect before use to ensure that no corrosion products or contaminating materials are present. For
storage of less than 24 h, storage of the coil in heptane that is free from traces of water and corrosive
materials, is satisfactory.
NOTE Redistilled heptane (4.2), stored in a tightly-sealed bottle, is suitable for overnight storage of the catalyst coil.
7.4 Cleaning new glassware
Wash new oxygen-delivery tubes, condensers and test tubes with hot detergent solution (see 4.6.3) and rinse
thoroughly with potable water (4.1). Clean the interiors of the test tubes, the exteriors of the condensers, and
both interiors and exteriors of the oxygen-delivery tubes by either soaking for 24 h in a 10 % solution of the
surfactant cleaning fluid (4.6.2), or by washing in strong oxidizing acid solution (4.6.1). Rinse all parts
thoroughly with potable water followed by water (4.1) and allow to dry, either in an oven or by a final rinse of
propan-2-ol (4.4) or acetone (4.3) followed by air drying at ambient temperature.
7.5 Cleaning used glassware
Immediately following the termination of a test, drain the hydraulic fluid completely from the test tube and rinse
all glassware with heptane (4.2) to remove traces of hydraulic fluid. Wash with hot detergent solution (see
4.6.3) using a long-handled brush and rinse thoroughly with potable water.
NOTE If adherent deposits are still present, these can be removed by filling the test tube with detergent solution,
inserting the oxygen-delivery tube and fitting the condenser, and replacing the tube in the heating bath at test temperature.
Often, after several hours soaking, all adhering deposits except iron oxide have loosened, and this can be removed by a
subsequent soaking in the hydrochloric/orthophosphoric acid mixture (see 4.6.1).
After all deposits have been removed, follow the cleaning procedure described in 7.4.
Store all cleaned glassware in a dry, dust-free condition until required.
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SIST EN ISO 4263-3:2006
ISO 4263-3:2006(E)
7.6 Cleaning aliquot-removal device
Completely drain the tube of the sampling tube (5.9) and/or any other devices used and rinse any surfaces
that have contacted the hydraulic fluid with heptane (4.2) to remove traces of hydraulic fluid. Soak the device
to above the contact level for 24 h in the surfactant cleaning fluid (4.6.2), or wash in strong oxidizing acid
solution (4.6.1), rinse with potable water, followed by water (4.1), and dry in the manner described in 7.4.
8 Procedure
8.1 Adjust the heating bath to a temperature that will maintain the temperature in the hydraulic fluid in the
oxidation cells (5.1) at 95,0 °C ± 0,2 °C throughout the duration of the test, with oxygen passing through the
cells at 3,0 l/h ± 0,5 l/h.
NOTE The temperature of the heating bath (5.2) will be above 95 °C due to the cooling effect of the oxygen flow, but
t
...