ISO 4263-3:2015
(Main)Petroleum and related products — Determination of the ageing behaviour of inhibited oils and fluids using the TOST test — Part 3: Anhydrous procedure for synthetic hydraulic fluids
Petroleum and related products — Determination of the ageing behaviour of inhibited oils and fluids using the TOST test — Part 3: Anhydrous procedure for synthetic hydraulic fluids
ISO 4263-3:2015 specifies a method for the determination of the ageing behaviour of synthetic hydraulic fluids of categories HFDU, HEES, HEPG and HETG as defined, for example, in ISO 12922[1] and ISO 15380[2]. 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 change 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 may 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.
Pétrole et produits connexes — Détermination du comportement au vieillissement des fluides et huiles inhibés au moyen de l'essai TOST — Partie 3: Méthode anhydre pour les fluides hydrauliques synthétiques
L'ISO 4263-3 :2015 spécifie une méthode permettant d'évaluer les caractéristiques de vieillissement des fluides hydrauliques synthétiques des catégories HFDU, HEES, HEPG et HETG définies par exemple dans l'ISO 12922[1] et l'ISO 15380[2]. Le vieillissement est accéléré par la présence d'oxygène et de catalyseurs métalliques à température élevée et la dégradation du fluide est suivie par l'évolution de son indice d'acide. D'autres parties de l'ISO 4263 spécifient des méthodes similaires permettant d'évaluer les caractéristiques de vieillissement des huiles minérales et de catégories spécifiques de fluides difficilement inflammables utilisés dans des applications hydrauliques et autres. NOTE D'autres signes peuvent indiquer la détérioration des fluides, comme la formation de dépôts insolubles, la corrosion du bobinage de catalyseurs, ou un changement de viscosité. Cela traduit une oxydation du fluide mais il n'en est pas tenu compte pour la prévision de la durée de résistance à l'oxydation. Une étude est en cours pour essayer d'établir une corrélation entre ces phénomènes et l'utilisation en service. La présente méthode d'essai peut servir à comparer la stabilité à l'oxydation de fluides qui ne sont pas sujets à la contamination par l'eau. Cependant, en raison du très grand nombre de types d'applications sur le terrain, la corrélation des résultats de ces essais avec les performances réelles en service peut varier beaucoup, et il est préférable de faire appel à l'expérience. La fidélité de la présente méthode d'essai n'est pas établie car aucun essai interlaboratoires n'a été effectué. Tant que de tels essais n'ont pas été faits, il se peut que la méthode soit jugée inacceptable pour le contrôle des spécifications ou en cas de litige.
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INTERNATIONAL ISO
STANDARD 4263-3
Third edition
2015-11-15
Petroleum and related products —
Determination of the ageing
behaviour of inhibited oils and fluids
using the TOST test —
Part 3:
Anhydrous procedure for synthetic
hydraulic fluids
Pétrole et produits connexes — Détermination du comportement au
vieillissement des fluides et huiles inhibés au moyen de l’essai TOST —
Partie 3: Méthode anhydre pour les fluides hydrauliques synthétiques
Reference number
ISO 4263-3:2015(E)
©
ISO 2015
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ISO 4263-3:2015(E)
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ISO 4263-3:2015(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Reagents and materials . 2
5 Apparatus . 3
6 Sampling .11
7 Preparation of materials and apparatus .12
7.1 Cleaning the catalyst wire .12
7.2 Preparation of catalyst coil .12
7.3 Storage of the catalyst coil.12
7.4 Cleaning new glassware .12
7.5 Cleaning used glassware .12
7.6 Cleaning aliquot-removal device .12
8 Procedure.13
9 Calculation .14
10 Expression of results .15
11 Precision .15
11.1 General .15
11.2 Repeatability, r .15
11.3 Reproducibility, R .16
11.4 Reproducibility with duplicate tests .16
12 Test report .16
Annex A (normative) Liquid-in-glass thermometer specifications .17
Annex B (normative) Procedure for packaging and storage of catalyst coils .18
Annex C (informative) Method for the determination of the insolubles content of mineral
oils and anhydrous synthetic fluids .19
Annex D (informative) Appearance rating of catalyst coil wires .22
Annex E (informative) Determination of metals content .23
Bibliography .24
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ISO 4263-3:2015(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
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ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
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. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
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For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical
Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information
The committee responsible for this document is ISO/TC 28, Petroleum products and related products of
synthetic or biological origin.
This third edition cancels and replaces the second edition (ISO 4263-3:2010). The main change is the
revision of the calculation in Clause 9 to include calculations for both a test oil reaching a TAN of 2,0 mg
KOH per gram and for a test oil reaching an increase of TAN of 2,0 mg KOH per gram. In addition, the
inclusion of HETG and exclusion of HFDR from the scope have been adopted.
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 using the 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
NOTE As of the date of publication of this part of ISO 4263, the titles of parts 1, 2 and 4 started with Petroleum
and related products – Determination of the ageing behaviour of inhibited oils and fluids — TOST test.
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INTERNATIONAL STANDARD ISO 4263-3:2015(E)
Petroleum and related products — Determination of the
ageing behaviour of inhibited oils and fluids using the
TOST test —
Part 3:
Anhydrous procedure for synthetic hydraulic fluids
WARNING — The use of this part of ISO 4263 can 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
[1]
hydraulic fluids of categories HFDU, HEES, HEPG and HETG as defined, for example, in ISO 12922
[2]
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 change 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 may 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.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 3170, Petroleum liquids — Manual sampling
ISO 3696:1987, Water for analytical laboratory use — Specification and test methods
ISO 7537, Petroleum products — Determination of acid number — Semi-micro colour-indicator
titration method
EN 10130:2007, Cold rolled low carbon steel flat products for cold forming — Technical delivery conditions
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 either an acid number of 2,0 mg of potassium hydroxide
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ISO 4263-3:2015(E)
(KOH) per gram is reached or until an 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 lifetime. 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 has still not either reached or increased by 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.
Potable water means tap water, unless normal piped supplies are contaminated with particulate or high
levels of 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 a 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.
4.6.2 Surfactant cleaning fluid.
A proprietary strong surfactant cleaning fluid is a preferred alternative for example a combination of
non-ionic with anionic detergent pH of 9,5 to 11,0.
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ISO 4263-3:2015(E)
4.7 Catalyst wires.
4.7.1 Low-metalloid steel wire, of diameter 1,60 mm ± 0,05 mm, made of low carbon steel to
EN 10130 DC04, soft bright annealed and free from rust.
4.7.2 Copper wire, of diameter 1,63 mm ± 0,05 mm, made of electrolytic copper wire of 99,9 %
[3]
minimum purity, conforming to EN 13601 . Soft copper wire of an equivalent grade may also be used.
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. 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. The stages of preparation of the oxygen-delivery tube are illustrated in Figure 2.
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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ISO 4263-3:2015(E)
Dimensions in millimetres (unless otherwise indicated)
Key
1 glass condenser
2 oxygen delivery tube
3 fluid sample
4 catalyst coil
5 radius of bottom cell
Figure 1 — Oxidation cell
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ISO 4263-3:2015(E)
Dimensions in millimetres
a) First stage — Delivery tube base preparation
b) Second stage — Delivery tube middle section preparation
Figure 2 — Construction of the oxygen delivery lead-in tube (continued on the next page)
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ISO 4263-3:2015(E)
Dimensions in millimetres
c) Third stage — Delivery tube final assembly
Key
a
Bend over mandrel of diameter 26 mm.
b
Grind end of tube flat.
c
Refers to the outer diameter.
Figure 2 — Construction of the oxygen delivery lead-in tube
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 3. 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.
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ISO 4263-3:2015(E)
Dimensions in millimetres
a) Bracket (finished) b) Development of bracket
Material: Thickness 0,792 mm, stainless steel
Figure 3 — Thermometer bracket
5.5 Wire-coiling mandrel, as illustrated in Figure 4, is used to produce the double spiral of copper
and steel wire. The mandrel is included in a suitable winding device.
Dimensions in millimetres
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ISO 4263-3:2015(E)
Figure 4 — Catalyst coil mandrel (continued on the next page)
Dimensions in millimetres
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ISO 4263-3:2015(E)
Figure 4 — Catalyst coil mandrel (continued on the next page)
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ISO 4263-3:2015(E)
Dimensions in millimetres
Key
c
1 M6 × 1,0 × 12,7 hexagon head steel screw Material: bronze.
(or equivalent)
d
2 M8 × 1,25 × 12,7 hexagon head steel screw Holes (2) tap M8 × 1,25 (or equivalent).
(or equivalent)
e
3 vice jaws Hole tap M5 × 0,8 (or equivalent).
f
4 M5 × 0,8 × 5 steel grub screw (or equivalent) Pitch.
g
5 catalyst wires Pitch height.
a h
Material: steel. Hole tap M6 × 1,0 (or equivalent).
b i
Material: brass. 6 TPI double thread.
Figure 4 — Catalyst coil mandrel
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 upon the size and frequency of removal of aliquots of the
test portion for analysis, a selection of devices is 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 are generally 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.
5.9 Sampling tube, stainless steel tubing, 2,11 mm outside diameter, 1,60 mm 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 5.
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ISO 4263-3:2015(E)
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.
Dimensions in millimetres (unless otherwise indicated)
Figure 5 — Sampling tube holder
6 Sampling
Unless otherwise specified, samples shall be obtained by procedures in accordance with ISO 3170.
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ISO 4263-3:2015(E)
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 4), 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 4.6.2)
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 4.6.2) 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.
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
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ISO 4263-3:2015(E)
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 Determine the acid number of the fresh unoxidized fluid only if determining the time to an increase
in TAN of 2,0 mg KOH per gram.
8.2 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 ± 0,1 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 the specific temperature will depend upon the bath medium, capacity and circulation efficiency.
It is recommended that the heating bath be always filled with oxidation cells, using dummy (ballast)
cells for positions not occupied by test cells. In this way, the heating levels will be consistent, and the
level of fluid medium in liquid baths will be maintained at the correct immersion depth.
8.3 Measure the temperature in each cell containing 360 ml of fluid, by means of the liquid-in-glass
thermometer located on the thermometer bracket (5.4.3) with the immersion line at the fluid surface,
or by means of an alternative temperature-measurement device at the same point. If the liquid-in-glass
thermometer is used, correct the temperature reading by subtracting 0,1 °C to allow for emergent-
stem heating.
8.4 When a uniform temperature of 95,0 °C ± 0,2 °C is obtained in all the test cells in the heating bath,
record the heating bath temperature and maintain it at this level throughout tests carried out under the same
conditions. Any change in condition, such as a change in the number of cells in the bath, or dramatic change
in test fluid typ
...
DRAFT INTERNATIONAL STANDARD
ISO/DIS 4263-3
ISO/TC 28 Secretariat: NEN
Voting begins on: Voting terminates on:
2013-09-26 2014-02-26
Petroleum and related products — Determination of the
ageing behaviour of inhibited oils and fluids using the
TOST test —
Part 3:
Anhydrous procedure for synthetic hydraulic fluids
Pétrole et produits connexes — Détermination du comportement au vieillissement des fluides et huiles
inhibés au moyen de l’essai TOST —
Partie 3: Méthode anhydre pour les fluides hydrauliques synthétiques
[Revision of second edition (ISO 4263-3:2010)]
ICS: 75.120
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Should this draft be accepted, a final draft, established on the basis of comments
received, will be submitted to a parallel two-month approval vote in ISO and
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STANDARD UNTIL PUBLISHED AS SUCH.
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PROVIDE SUPPORTING DOCUMENTATION. ISO 2013
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ISO/DIS 4263-3:2013(E)
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ii © ISO 2013 – All rights reserved
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ISO/DIS 4263-3
Contents Page
1 Scope . 7
2 Normative references . 7
3 Principle . 7
4 Reagents and materials . 8
5 Apparatus . 9
6 Sampling. 10
7 Preparation of materials and apparatus . 10
7.1 Cleaning the catalyst wire . 10
7.2 Preparation of catalyst coil. 11
7.3 Storage of the catalyst coil . 11
7.4 Cleaning new glassware . 11
7.5 Cleaning used glassware. 11
7.6 Cleaning aliquot-removal device . 11
8 Procedure . 11
9 Calculation . 13
10 Expression of results . 13
11 Precision . 13
11.1 General . 13
11.2 Repeatability, r . 13
11.3 Reproducibility, R . 14
11.4 Reproducibility with duplicate tests . 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 . 21
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ISO/DIS 4263-3
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, and by
Technical Committee CEN/TC 19, Gaseous and liquid fuels, lubricants and related products of petroleum,
synthetic and biological origin, in collaboration.
This third edition cancels and replaces the second edition (EN ISO 4263-3:2010). Main changes are the
revision of the calculation as in Clause 9, where the acid number of the fresh unoxidised fluid has been
introduced, and the inclusion of HETG in and the exclusion of HFDR from the scope.
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 using the 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.
iv © ISO 2013 – All rights reserved
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DRAFT INTERNATIONAL STANDARD ISO/DIS 4263-3
Petroleum and related products — Determination of the ageing
behaviour of inhibited oils and fluids using the TOST test —
Part 3: Anhydrous procedure for synthetic hydraulic fluids
WARNING — The use of this part of ISO 4263 can 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
1
fluids of categories HFDU, HEES and HEPG, HETG as defined, for example, in ISO 12922[ ] and
2
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 may 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 inter-laboratory 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
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
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7
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ISO/DIS 4263-3
(KOH) per gram of test portion is reached and the number of hours is recorded as the oxidation lifetime. 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 has still not increased by 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.
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 a 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.
4.6.2 Surfactant cleaning fluid
A proprietary strong surfactant cleaning fluid is a preferred alternative.
4.6.3 Laboratory detergent, 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.
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ISO/DIS 4263-3
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.
Dimensions in millimetres
(unless otherwise indicated)
b) First stage c) Second stage
a) Apparatus d) Final stage
Key
1 glass condenser a Bend over mandrel of diameter 26.
2 oxygen-delivery tube b Grind end of tube.
3 fluid sample c External diameter.
4 catalyst coil
5 radius of bottom cell
Figure 1 – Oxidation cell
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
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ISO/DIS 4263-3
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.
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.
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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ISO/DIS 4263-3
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.
Dimensions in millimetres
Figure 3 – Catalyst coil mandrel
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ISO/DIS 4263-3
Dimensions in millimetres
b
B
Figure 3 — Catalyst coil mandrel (continued)
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ISO/DIS 4263-3
Dimensions in millimetres
Key
″
1 1/4 Whitworth x 12,7 hexagon head steel screw (or equivalent)
″
2 5/16 Whitworth x 2,7 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)
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 upon the size and frequency of removal of aliquots of the test
portion for analysis, a selection of devices is 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 are generally 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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ISO/DIS 4263-3
Dimensions in millimetres
(unless otherwise indicated)
Figure 4 — Sampling tube holder
6 Sampling
Unless otherwise specified, samples shall be obtained by the procedures in accordance with 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.
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ISO/DIS 4263-3
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 part s
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.
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 Determine the acid number of the fresh unoxidised fluid.
8.2 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 9 °C due to the cooling effect of the oxygen flow, but
the specific temperature will depend upon the bath medium, capacity and circulation efficiency.
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ISO/DIS 4263-3
It is recommended that the heating bath be always filled with oxidation cells, using dummy (ballast) cells for
positions not occupied by test cells. In this way, the heating levels will be consistent, and the level of fluid
medium in liquid baths will be maintained at the correct immersion depth.
8.3 Measure the temperature in each cell containing 360 ml of fluid, by means of the liquid-in-glass
thermometer located on the thermometer bracket (5.4.3) with the immersion line at the fluid surface, or by
means of an alternative temperature-measurement device at the same point. If the liquid-in-glass
thermometer is used, correct the temperature reading by subtracting 0,1 °C to allow for emergent-stem
heating.
8.4 When a uniform temperature of 95,0 °C ± 0,2 °C is obtained in all the test cells in the heating bath,
record the heating bath temperature and maintain it at this level throughout tests carried out under the same
conditions. Any change in condition, such as a change in the number of cells in the bath, or dramatic
change in test fluid type, necessitates a check on the level and uniformity of temperature control. All
temperature measurements are carried out on new, un-depleted test portions and/or dummy cells.
Immediately after the temperature control has been established, remove the temperature-measurement
devices.
8.5 Fill the empty oxidation test tube with 360 ml of hydraulic fluid. Slide the catalyst coil over the oxygen
inlet tube. If the wires are uneven at one end of the coil, position the coil so that this end is down. Place the
oxygen inlet tube with the coil into the test tube, and place the condenser over the oxygen delivery tube and
test tube. If used, a sampling tube (5.9) and holder (5.11) are inserted at this time. Check the immersion
depth of the oxidation cell, and adjust to 355 mm ± 10 mm as necessary. Connect the condenser to the
cooling water and adjust the flow rate such that the temperature of the outlet water does not exceed 32 °C at
any time during the test.
NOTE As an alternative to using the sampling tube holder (5.11) and sampling tube spacer (5.12), the sampling
tube (5.9) can be secured in position by taping to the oxygen-delivery tube using a suitable adhesive tape. The sampling
tube is taped to the oxygen-delivery tube at a distance of approximately 25 mm above the top of the condenser. The bottom
of the sampling tube is positioned at (150 ± 5) mm from the bottom curved end of the oxygen-delivery tube.
8.6 Connect the oxygen-delivery tube to the oxygen supply through the flowmeter (5.3) using new
flexible tubing (5.6) no more than 600 mm in length. Before use, flush the interior of the tubing with heptane
(4.2) and blow dry with air. Adjust the rate of oxygen flow to 3,0 l/h ± 0,1 l/h.
8.7 Maintain the conditions for 30 min. Mark the level of the hydrau
...
NORME ISO
INTERNATIONALE 4263-3
Troisième édition
2015-11
Pétrole et produits connexes —
Détermination du comportement au
vieillissement des fluides et huiles
inhibés au moyen de l'essai TOST —
Partie 3:
Méthode anhydre pour les fluides
hydrauliques synthétiques
Petroleum and related products — Determination of the ageing
behaviour of inhibited oils and fluids using the TOST test —
Part 3: Anhydrous procedure for synthetic hydraulic fluids
Numéro de référence
ISO 4263-3:2015(F)
©
ISO 2015
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ISO 4263-3:2015(F)
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2015, Publié en Suisse
Droits de reproduction réservés. Sauf indication contraire, aucune partie de cette publication ne peut être reproduite ni utilisée
sous quelque forme que ce soit et par aucun procédé, électronique ou mécanique, y compris la photocopie, l’affichage sur
l’internet ou sur un Intranet, sans autorisation écrite préalable. Les demandes d’autorisation peuvent être adressées à l’ISO à
l’adresse ci-après ou au comité membre de l’ISO dans le pays du demandeur.
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Tel. +41 22 749 01 11
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ii © ISO 2015 – Tous droits réservés
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ISO 4263-3:2015(F)
Sommaire Page
Avant-propos .iv
1 Domaine d'application . 1
2 Références normatives . 1
3 Principe . 2
4 Produits et réactifs . 2
5 Appareillage . 3
6 Échantillonnage .11
7 Préparation des produits et de l’appareillage .12
7.1 Nettoyage des fils de catalyseur .12
7.2 Préparation de la bobine de catalyseur .12
7.3 Conservation de la bobine de catalyseurs .12
7.4 Nettoyage de la verrerie neuve .12
7.5 Nettoyage de la verrerie après utilisation .12
7.6 Nettoyage des dispositifs de prélèvement des parties aliquotes .13
8 Mode opératoire.13
9 Calculs .14
10 Expression des résultats.15
11 Fidélité .15
11.1 Généralités .15
11.2 Répétabilité, r .16
11.3 Reproductibilité, R .16
11.4 Reproductibilité avec des essais en double .16
12 Rapport d'essai .16
Annexe A (normative) Spécifications pour les thermomètres en verre .17
Annexe B (normative) Mode opératoire pour le conditionnement et la conservation
des bobines de catalyseur .18
Annexe C (informative) Méthode de détermination de la teneur en produits insolubles
des huiles minérales et des fluides synthétiques anhydres .19
Annexe D (informative) Cotation visuelle des fils de la bobine de catalyseur .22
Annexe E (informative) Détermination de la teneur en métaux.23
Bibliographie .24
© ISO 2015 – Tous droits réservés iii
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ISO 4263-3:2015(F)
Avant-propos
L'ISO (Organisation internationale de normalisation) est une fédération mondiale d'organismes
nationaux de normalisation (comités membres de l'ISO). L'élaboration des Normes internationales est
en général confiée aux comités techniques de l'ISO. Chaque comité membre intéressé par une étude
a le droit de faire partie du comité technique créé à cet effet. Les organisations internationales,
gouvernementales et non gouvernementales, en liaison avec l'ISO participent également aux travaux.
L'ISO collabore étroitement avec la Commission électrotechnique internationale (CEI) en ce qui
concerne la normalisation électrotechnique.
Les procédures utilisées pour élaborer le présent document et celles destinées à sa mise à jour sont
décrites dans les Directives ISO/IEC, Partie 1. Il convient, en particulier de prendre note des différents
critères d’approbation requis pour les différents types de documents ISO. Le présent document a été
rédigé conformément aux règles de rédaction données dans les Directives ISO/IEC, Partie 2 (voir www.
iso.org/directives).
L’attention est appelée sur le fait que certains des éléments du présent document peuvent faire l’objet de
droits de propriété intellectuelle ou de droits analogues. L’ISO ne saurait être tenue pour responsable
de ne pas avoir identifié de tels droits de propriété et averti de leur existence. Les détails concernant
les références aux droits de propriété intellectuelle ou autres droits analogues identifiés lors de
l’élaboration du document sont indiqués dans l’Introduction et/ou dans la liste des déclarations de
brevets reçues par l’ISO (voir www.iso.org/brevets).
Les appellations commerciales éventuellement mentionnées dans le présent document sont données
pour information, par souci de commodité, à l’intention des utilisateurs et ne sauraient constituer un
engagement.
Pour une explication de la signification des termes et expressions spécifiques de l’ISO liés à
l’évaluation de la conformité, ou pour toute information au sujet de l’adhésion de l’ISO aux principes
de l’OMC concernant les obstacles techniques au commerce (OTC), voir le lien suivant: Avant-propos —
Informations supplémentaires.
L'ISO 4263-3 a été élaborée par le comité technique ISO/TC 28, Produits pétroliers et connexes d’origine
synthétique ou biologique, carburants et lubrifiants, d'origine pétrolière, synthétique et biologique.
Cette troisième édition annule et remplace la deuxième (ISO 4263-3:2010). Les principaux changements
consistent en la révision du mode de calcul spécifié dans l’Article 9, pour inclure à la fois les calculs pour
une huile d’essai ayant un indice d’acide (TAN) de 2,0 mg KOH par gramme et pour une huile d’essai
dont l’indice d’acide (TAN) augmente de 2,0 mg KOH par gramme. Par ailleurs, l’introduction des fluides
HETG et l’exclusion des fluides HFDR du domaine d’application ont été adoptées.
L'ISO 4263 comprend les parties suivantes, présentées sous le titre général Pétrole et produits
connexes — Détermination du comportement au vieillissement des fluides et huiles inhibés au moyen de
l'essai TOST:
— Partie 1: Méthode pour les huiles minérales
— Partie 2: Méthode pour les fluides hydrauliques de catégorie HFC
— Partie 3: Méthode anhydre pour les fluides hydrauliques synthétiques
— Partie 4: Méthode pour les huiles pour engrenages industriels
NOTE À partir de la date de publication de cette partie de l’ISO 4263, les titres des Parties 1, 2 et 4 ont
commencé par Pétrole et produits connexes — Détermination du comportement au vieillissement des fluides et huiles
inhibées — Essai TOST.
iv © ISO 2015 – Tous droits réservés
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NORME INTERNATIONALE ISO 4263-3:2015(F)
Pétrole et produits connexes — Détermination du
comportement au vieillissement des fluides et huiles
inhibés au moyen de l'essai TOST —
Partie 3:
Méthode anhydre pour les fluides hydrauliques
synthétiques
AVERTISSEMENT — L'utilisation de la présente partie de l’ISO 4263 peut impliquer l'intervention
de produits, d'opérations et d'équipements à caractère dangereux. La présente partie de
l’ISO 4263 n'est pas censée aborder tous les problèmes de sécurité concernés par son usage. Il est
de la responsabilité de l'utilisateur de consulter et d'établir des règles de sécurité et d'hygiène
appropriées et de déterminer l'applicabilité des restrictions réglementaires avant utilisation.
1 Domaine d'application
La présente partie de l'ISO 4263 spécifie une méthode permettant d'évaluer les caractéristiques
de vieillissement des fluides hydrauliques synthétiques des catégories HFDU, HEES, HEPG et HETG
[1] [2]
définies par exemple dans l’ISO 12922 et l’ISO 15380 . Le vieillissement est accéléré par la présence
d'oxygène et de catalyseurs métalliques à température élevée et la dégradation du fluide est suivie
par l'évolution de son indice d'acide. D'autres parties de l'ISO 4263 spécifient des méthodes similaires
permettant d'évaluer les caractéristiques de vieillissement des huiles minérales et de catégories
spécifiques de fluides difficilement inflammables utilisés dans des applications hydrauliques et autres.
NOTE D’autres signes peuvent indiquer la détérioration des fluides, comme la formation de dépôts insolubles,
la corrosion du bobinage de catalyseurs, ou un changement de viscosité. Cela traduit une oxydation du fluide mais
il n’en est pas tenu compte pour la prévision de la durée de résistance à l’oxydation. Une étude est en cours pour
essayer d’établir une corrélation entre ces phénomènes et l’utilisation en service. La présente méthode d’essai
peut servir à comparer la stabilité à l’oxydation de fluides qui ne sont pas sujets à la contamination par l’eau.
Cependant, en raison du très grand nombre de types d’applications sur le terrain, la corrélation des résultats
de ces essais avec les performances réelles en service peut varier beaucoup, et il est préférable de faire appel
à l’expérience. La fidélité de la présente méthode d’essai n’est pas établie car aucun essai interlaboratoires n’a
été effectué. Tant que de tels essais n’ont pas été faits, il se peut que la méthode soit jugée inacceptable pour le
contrôle des spécifications ou en cas de litige.
2 Références normatives
Les documents suivants, en totalité ou en partie, sont référencés normativement dans ce document et
sont indispensables pour son application. Pour les références datées, seule l'édition citée s'applique.
Pour les références non datées, la dernière édition du document de référence s'applique (y compris les
éventuels amendements).
ISO 3170, Produits pétroliers liquides — Échantillonnage manuel
ISO 3696:1987, Eau pour laboratoire à usage analytique — Spécification et méthodes d'essai
ISO 7537, Produits pétroliers — Détermination de l'indice d'acide — Méthode de titrage semi-micro par
indicateur coloré
ISO 10130:2007, Produits plats laminés à froid, en acier à bas carbone pour formage à froid — Conditions
techniques de livraison
© ISO 2015 – Tous droits réservés 1
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ISO 4263-3:2015(F)
3 Principe
Une prise d'essai est portée à 95 °C sous courant d’oxygène, à l'abri de la lumière, en présence d'une
bobine de fils d'acier et de cuivre faisant office de catalyseur. De petites parties aliquotes de fluide sont
soutirées à intervalles réguliers et leur indice d'acide est déterminé (voir la Note de l’Article 1). L'essai
est poursuivi soit jusqu'à ce que l'indice d'acide atteigne une valeur de 2,0 mg d’hydroxyde de potassium
(KOH) par gramme, soit jusqu'à ce qu’une augmentation d'indice d'acide de 2,0 mg d’hydroxyde de
potassium (KOH) par gramme de prise d’essai soit atteinte et le nombre d'heures d'essai écoulé à ce
moment est noté comme durée de résistance à l'oxydation. Pour certaines exigences, l'essai peut être
interrompu après un nombre d'heures préalablement fixé (par exemple 500 h ou 1 000 h), alors que
l'indice d'acide n’a pas encore atteint ou augmenté de 2,0 mg de KOH par gramme de prise d’essai.
4 Produits et réactifs
4.1 Eau, qui sauf indication contraire, doit être conforme aux exigences de la qualité 2 définie dans
l'ISO 3696. L'expression «eau potable» se réfère à l'eau du robinet, sauf si la distribution normale par
réseau est polluée par des particules solides ou si elle contient une teneur élevée en minéraux solubles.
4.2 Heptane (C H ), de pureté minimale de 99,75 %.
7 16
4.3 Acétone (CH COCH ), de qualité pour usage général.
3 3
4.4 Propan-2-ol (CH CHOHCH ), de qualité pour usage général.
3 3
4.5 Oxygène, de pureté minimale de 99,5 %. Distribué par un dispositif de régulation de pression apte
à maintenir le débit spécifié pendant toute la durée de l'essai.
Pour une alimentation à partir d'une bouteille d'oxygène, il convient d'utiliser un système de régulation
à deux étages couplé à un robinet à aiguille pour améliorer la stabilité de la régulation du débit de gaz.
AVERTISSEMENT — Utiliser l'oxygène seulement avec des équipements certifiés pour le service
oxygène. Ne pas laisser d'huile ou de graisse entrer en contact avec l'oxygène, nettoyer et
inspecter chaque régulateur, manomètre et équipement de contrôle. Rechercher régulièrement
la présence éventuelle de fuites sur le réseau d'alimentation en oxygène. Si une fuite est
suspectée, fermer immédiatement l'alimentation et solliciter une assistance qualifiée.
4.6 Solutions de nettoyage.
4.6.1 Solution acide fortement oxydante.
La solution de nettoyage fortement oxydante de référence sur laquelle sont fondées les valeurs de
fidélité est l'acide sulfochromique (voir l'avertissement ci-après). Cependant l'expérience montre
que d'autres solutions, exemptes de chrome, telle que le persulfate d'ammonium à 8 g/l dans l'acide
sulfurique concentré, conduisent à un état de propreté satisfaisant. L'utilisation d'une solution à 10 %
de trois parties d'acide chlorhydrique (1 mole/l) et d'une partie d'acide orthophosphorique (concentré,
de qualité pour usage général), permet d'éliminer les dépôts d'oxydes de fer.
AVERTISSEMENT — L'acide sulfochromique est dangereux pour la santé. Il s'agit d'un
carcinogène reconnu en raison des composés du Cr-VI qu'il contient, il est toxique, très
corrosif et potentiellement dangereux lorsqu'il est en contact avec des produits organiques.
Il est indispensable de porter des vêtements et lunettes de protection lors de l'utilisation de
solutions de nettoyage à base d'acide sulfochromique. Ne jamais pipeter la solution de nettoyage
à la bouche. Après usage, ne pas verser la solution de nettoyage directement à l'égout, mais la
neutraliser avec de grandes précautions en raison de l'acide sulfurique présent, puis rejeter
conformément aux procédures normales relatives aux déchets toxiques de laboratoire (le
chrome est très dangereux pour l'environnement).
2 © ISO 2015 – Tous droits réservés
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ISO 4263-3:2015(F)
Les solutions de nettoyage acides fortement oxydantes exemptes de chrome sont également très
corrosives et potentiellement dangereuses lorsqu'elles sont en contact avec des produits organiques,
mais elles ne présentent pas les problèmes spécifiques de rejet relatifs au chrome.
4.6.2 Fluide de nettoyage tensioactif.
L'usage d'un fluide de nettoyage tensioactif de marque déposée est préférable, par exemple la
combinaison d’un détergent non ionique avec un détergent anionique dont le pH est de 9,5 à 11,0.
4.7 Fils de catalyseur.
4.7.1 Fil en acier à faible teneur en métalloïdes, de 1,60 mm ± 0,05 mm de diamètre, en acier à bas
carbone EN 10130 DC04, recuit, poli et exempt de rouille.
4.7.2 Fil en cuivre, de 1,63 mm ± 0,05 mm de diamètre, fil de cuivre électrolytique de pureté minimale
[3]
de 99,9 %, conforme à l’EN 13601 . Un fil de cuivre doux de qualité équivalente peut aussi être utilisé.
4.8 Toile abrasive, en carbure de silicium de 150 μm (grain P100) sur support textile ou une toile
abrasive de qualité équivalente.
4.9 Coton hydrophile.
5 Appareillage
5.1 Cellule d'oxydation, composée d'un grand tube en verre borosilicaté. Sur ce tube viennent
s'adapter un condenseur du type «champignon» et un tube d'arrivée d'oxygène, tous deux également en
verre borosilicaté. La cellule doit présenter la configuration et les dimensions indiquées à la Figure 1. Les
étapes de préparation du tube d’arrivée d’oxygène sont illustrées en Figure 2.
5.2 Bain chauffant, thermostaté capable de maintenir la prise d'essai de fluide hydraulique placée
dans la cellule d'oxydation à 95,0 ± 0,2 °C. Il doit être suffisamment spacieux pour abriter le nombre
voulu de cellules d'oxydation (5.1) immergées à une profondeur de 355 ± 10 mm dans le milieu de
transfert de chaleur. Il doit être conçu de manière que les prises d'essai soient abritées de la lumière
tout au long de l'essai. Si un bain à fluide est utilisé, il doit être équipé d'un dispositif d'agitation adapté
permettant d'assurer une température uniforme en tout point du bain. Si le bain à fluide est muni d'un
couvercle, la partie de la cellule d'oxydation se trouvant à l'intérieur du bain doit avoir une longueur
totale de 390 ± 10 mm. Si un bain du type bloc métallique est utilisé, les éléments chauffants doivent être
distribués de manière à assurer une température uniforme en tout point du bloc. Les alésages du bloc
doivent avoir un diamètre minimal de 50 mm et une profondeur de 390 ± 10 mm, comprenant, le cas
échéant, l'épaisseur du couvercle isolant.
5.3 Débitmètre, de capacité minimale de 3,0 l/h et d'une précision de ± 0,1 l/h.
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ISO 4263-3:2015(F)
Dimensions en millimètres (sauf indication contraire)
Légende
1 condenseur en verre
2 tube d’arrivée d’oxygène
3 prise d’essai de fluide
4 bobine de catalyseur
5 rayon de courbure du fond du tube à essai
Figure 1 — Cellule d'oxydation
4 © ISO 2015 – Tous droits réservés
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ISO 4263-3:2015(F)
Dimensions en millimètres
a) Première étape — Préparation de la base du tube
b) Deuxième étape — Préparation de la section médiane du tube
Figure 2 — Construction du tube d’arrivée d’oxygène (suite page suivante)
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ISO 4263-3:2015(F)
Dimensions en millimètres
c) Troisième étape — Assemblage final du tube
a
Courbé sur un mandrin de diamètre 26 mm.
b
Extrémité du tube rodé à fond plat.
c
Diamètre externe.
Figure 2 — Construction du tube d’arrivée d’oxygène
5.4 Dispositifs de mesurage de température.
5.4.1 Bain chauffant, la température des bains chauffants à liquide doit être mesurée soit avec un
thermomètre en verre conforme aux spécifications données dans l'Annexe A, soit avec un dispositif
de mesurage de température équivalent dont les indications sont lisibles à ± 0,1 °C près et gradué par
incréments de 0,1 °C. Les bains du type bloc métallique doivent être dotés d'un système de mesurage de
température comportant éventuellement plusieurs dispositifs et présentant la même lisibilité et la même
précision.
5.4.2 Cellule d'oxydation, la température régnant dans la cellule d'oxydation doit être mesurée
soit avec un thermomètre en verre conforme aux spécifications données dans l'Annexe A, soit avec un
dispositif de mesurage de température équivalent dont les indications sont lisibles à ± 0,1 °C près et
étalonné à mieux que ± 0,1 °C.
5.4.3 Support de thermomètre, s'il est fait usage d'un thermomètre en verre dans la cellule
d'oxydation, celui-ci doit être suspendu à l'aide d'un support, comme illustré à la Figure 3. Le
thermomètre est maintenu dans le support soit par deux joints toriques en élastomère fluoré d'environ
5 mm de diamètre, soit au moyen d'un fil en acier inoxydable fin.
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ISO 4263-3:2015(F)
Dimensions en millimètres
a) Support (terminé) b) Agrandissement
Matériau: acier inoxydable d’épaisseur 0,792 mm
Figure 3 — Support du thermomètre
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ISO 4263-3:2015(F)
5.5 Mandrin de bobinage des fils, tel qu'illustré à la Figure 4 est utilisé pour confectionner la double
spirale de fils de cuivre et d'acier. Ce mandrin fait partie d'un dispositif de bobinage approprié.
Dimensions en millimètres
Figure 4 — Mandrin de bobinage des fils de catalyseur (suite page suivante)
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ISO 4263-3:2015(F)
Dimensions en millimètres
Figure 4 — Mandrin de bobinage des fils de catalyseur (suite page suivante)
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ISO 4263-3:2015(F)
Dimensions en millimètres
Légende
c
1 vis en acier à tête hexagonale M6 × 1,0 × 12,7 Matériau: bronze.
(ou équivalent)
d
2 vis en acier à tête hexagonale M8 × 1,25 × 12,7 2 trous taraudés M8 × 1,25 (ou équivalent).
(ou équivalent)
e
3 mâchoires d’étau Trou M5 × 0,8 (ou équivalent).
f
4 vis sans tête acier M5 × 0,8 × 5 (ou équivalent) Pas.
g
5 fils de catalyseur Hauteur du pas.
a a
Matériau: acier. Trou taraudé M6 × 1,0 (ou équivalent).
b i
Matériau: laiton. Filetage double 6 TPI.
Figure 4 — Mandrin de bobinage des fils de catalyseur
5.6 Tuyau d'alimentation en oxygène, pour alimenter la cellule d'oxydation en oxygène il est
nécessaire de disposer de tuyau souple en chlorure de polyvinyle (PVC) d'environ 6,4 mm de diamètre
intérieur et 1,5 mm d'épaisseur de paroi.
5.7 Dispositifs de prélèvement des parties aliquotes, une sélection de différents dispositifs est
nécessaire en fonction de la taille et de la fréquence prévue des prélèvements en vue d'analyse. Des
seringues en verre munies d'embouts de raccordement du type Luer et d'aiguilles en acier inoxydable
ou des pipettes à pointe longue équipées d'un dispositif de remplissage approprié, conviennent. Ces
dispositifs peuvent être insérés par un tube d'échantillonnage (5.9) installé à travers le condenseur.
La taille des parties aliquotes est généralement comprise entre 2 ml et 10 ml, et les dispositifs utilisés
doivent être en mesure d'effectuer le prélèvement à ± 0,2 ml près.
5.8 Récipients pour les prélèvements, petits flacons en verre brun de 5 ml à 10 ml munis de capsules
en polyéthylène à serrage étanche.
5.9 Tube d’échantillonnage, tube en acier inoxydable, de 2,11 mm de diamètre extérieur, 1,60 mm
de diamètre intérieur, 6,10 mm ± 2 mm de long, avec une extrémité finie à 90° et l’autre munie en option
d’un connecteur Luer femelle [si l’on utilise des seringues comme dispositifs de prélèvement des parties
aliquotes (5.7)]. Le connecteur optionnel est de préférence fait d’un élastomère, tel que le polychlorure
de fluorovinyle, afin de réaliser un bon raccord avec la seringue.
5.10 Bouchon, pour le connecteur optionnel Luer sur le tube d’échantillonnage (5.9), fait en
polytétrafluoréthylène (PTFE) ou en polychlorure de fluorovinyle.
5.11 Support de tube d’échantillonnage, pour porter le tube d’échantillonnage (5.9), fait en résine de
méthylmétacrylate, ayant les dimensions tel qu'illustré en Figure 5.
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ISO 4263-3:2015(F)
5.12 Pièce de calage pour le tube d’échantillonnage, pour positionner l’extrémité du tube
d’échantillonnage (5.9) au-dessus du support du tube d’échantillonnage (5.11), fait d’un tube de
plastique en polychlorure de vinyle, polyéthylène, polypropylène, ou polytétrafluoréthylène, ayant un
diamètre intérieur d’environ 3 mm et une longueur de 51 mm ± 1 mm.
Dimensions en millimètres (sauf indication contraire)
Figure 5 — Support de tube d'échantillonnage
6 Échantillonnage
Sauf indication contraire, les échantillons doivent être prélevés conformément à l'ISO 3170.
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ISO 4263-3:2015(F)
7 Préparation des produits et de l’appareillage
7.1 Nettoyage des fils de catalyseur
Immédiatement avant de procéder au bobinage des fils de catalyseur, nettoyer une longueur de
3,00 ± 0,01 m de fil d'acier (4.7.1) et une longueur équivalente de fil de cuivre (4.7.2) à l'aide de tampons
de coton hydrophile (4.9) imprégnés d'heptane (4.2). Frotter ensuite avec la toile abrasive (4.8) jusqu'à
découvrir une surface fraîche de métal. Enfin, essuyer avec un tampon de coton hydrophile sec jusqu'à
ce que toutes les particules de métal arraché et d'abrasif soient enlevées. Dans les opérations qui suivent,
manipuler les fils de catalyseurs avec des gants propres (en coton, en caoutchouc ou en plastique) afin
d'éviter tout contact avec la peau.
7.2 Préparation de la bobine de catalyseur
Torsader ensemble et de façon serrée les fils d'acier et de cuivre par l'une de leurs extrémités en faisant
trois tours et ensuite les enrouler simultanément côte à côte sur un mandrin fileté (5.5 et Figure 4) en
insérant le fil d'acier dans le filet le plus profond. Torsader ensemble les extrémités libres des fils d'acier
et de cuivre en faisant trois tours, puis courber les extrémités torsadées de manière à suivre la forme de
l'enroulement. Retirer la bobine du mandrin en inversant le sens de la manœuvre de bobinage. S'assurer
que la longueur totale de la bobine est de 225 ± 5 mm, au besoin en l'étirant ou en la comprimant.
7.3 Conservation de la bobine de catalyseurs
Avant usage, conserver la bobine de catalyseurs sous une atmosphère inerte sèche, selon la méthode
décrite dans l'Annexe B. Aussitôt avant utilisation, inspecter la bobine afin de s'assurer de l'absence de
produits de corrosion ou de pollution. Pour une conservation d'une durée inférieure à 24 h, un stockage
de la bobine dans de l'heptane exempt de traces d'eau et de produits corrosifs est satisfaisant.
NOTE L'heptane redistillé (4.2) stocké dans une bouteille hermétiquement fermée convient pour le stockage
de la bobine de catalyseur pendant une nuit.
7.4 Nettoyage de la verrerie neuve
Laver les tubes d'arrivée d'oxygène, les condenseurs et les tubes à essais neufs avec une solution chaude
de détergent (voir 4.6.2) puis les rincer soigneusement avec de l'eau potable (4.1). Nettoyer l'intérieur
des tubes à essais, l'extérieur des condenseurs et aussi bien l'intérieur que l'extérieur des tubes d'arrivée
d'oxygène, soit par trempage pendant 24 h dans une solution à 10 % de fluide de nettoyage tensioactif
(4.6.2), soit par lavage dans la solution acide fortement oxydante (4.6.1). Rincer soigne
...
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