EN ISO 4263-1:2004

Petroleum and related products - Determination of the ageing behaviour of inhibited oils and fluids - TOST test - Part 1: Procedure for mineral oils (ISO 4263-1:2003)

ISO 4263-1:2003 specifies a method for the determination of the ageing behaviour of rust- and oxidation- inhibited mineral oils having a density less than that of water, used as turbine oils (categories TSA, TGA, TSE, TGE of ISO 6743-5, hydraulic oils (categories HL, HM, HR, HV, HG of ISO 6743-4), and circulating oils (category CKB of ISO 6743-6). Oils containing synthetic components can be tested by this procedure, but no precision statement is available yet for such fluids.
This test method is widely used in specifications and is considered of value in comparing the oxidation stability of oils that are 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.

Mineralölerzeugnisse und verwandte Produkte - Bestimmung des Alterungsverhaltens von inhibierten Ölen und Flüssigkeiten - TOST- Verfahren - Teil 1: Verfahren für Mineralöle (ISO 4263-1:2003)

Dieser Teil von ISO 4263 legt ein Verfahren fest zur Bestimmung des Alterungsverhaltens von Mineralölen, die als Turbinenöl (Kategorien TSA, TGA, TSE, TGE nach ISO 6743-5, siehe Literaturhinweis [4]), als Druckflüssigkeit (Kategorien HL, HM, HR, HV, HG nach ISO 6743-4, siehe Literaturhinweis [3]) oder als Umlauföl (Kategorie CKB nach ISO 6743-6, siehe Literaturhinweis [5]) eingesetzt werden, Wirkstoffe zur Erhöhung der Alterungsbeständigkeit und des Korrosionsschutzes enthalten und deren Dichte niedriger ist als die von Wasser. Öle, die synthetische Bestandteile enthalten, können ebenfalls mit diesem Prüfverfahren untersucht werden, allerdings liegen für solche Flüssigkeiten keine Präzisionsangaben vor.
ANMERKUNG 1   Für die Anwendung dieses Teils von ISO 4263 wird die Bezeichnung "% (m/m)" für den Massenanteil in Prozent  verwendet.
ANMERKUNG 2   Andere mögliche Zerfallserscheinungen, wie die Bildung von unlöslichem Schlamm, die Korrosion der Katalysatorwendeln oder die Abnahme des pH-Wertes, sind ein Anzeichen für Oxidationsvorgänge im Öl, sie lassen aber keine Rückschlüsse auf die Öllebensdauer zu. Die Korrelation dieser Vorkommnisse mit Feldanwendungen wird noch untersucht.
Dieses Prüfverfahren ist in Spezifikationen weit verbreitet. Die dabei ermittelten Ergebnisse werden zum Vergleich der Oxidationsstabilität von mit Wasser verunreinigten Ölen herangezogen. Wegen der großen Anzahl individueller Anwendungen in der Praxis kann eine Übereinstimmung der nach diesem Prüfverfahren erhaltenen Ergebnisse mit der aktuellen Leistungsfähigkeit des Öles stark variieren und sich erst im Betriebseinsatz herausstellen.
Die Präzision dieses Teils von ISO 4263 wurde nur mit wirkstoffhaltigen Turbinenölen bestimmt und gilt für eine Oxidationsstabilität im Bereich von 700 h bis 3 900 h.

Pétrole et produits connexes - Détermination du comportement au vieillissement des fluides et huiles inhibées - Essai TOST - Partie 1: Méthode pour les huiles minérales (ISO 4263-1:2003)

L'ISO 4263-1:2003 spécifie une méthode permettant d'évaluer le comportement au vieillissement des huiles minérales contenant des additifs antioxydants et antirouille dont la masse volumique est inférieure à celle de l'eau, et utilisées comme huiles pour turbines (catégories TSA, TGA, TSE, TGE de l'ISO 6743-5), comme fluides hydrauliques (catégories HL, HM, HR, HV, HG de l'ISO 6743-4), et comme huiles de graissage par circulation (catégorie CKB de l'ISO 6743-6). Il est possible de tester par cette méthode des huiles contenant des composés synthétiques, mais il n'existe aucune donnée de fidélité disponible à ce jour pour de tels produits.
Il est largement fait appel à cette méthode d'essai dans les spécifications. Celle-ci est considérée comme très utile lorsqu'il s'agit de comparer la stabilité à l'oxydation d'huiles sujettes à la pollution par l'eau. Cependant, en raison du grand nombre d'applications différentes, la corrélation entre les résultats de cet essai et les performances réelles en service peut varier fortement et de ce fait l'expérience reste le meilleur moyen pour l'évaluer.

Nafta in sorodni proizvodi - Določanje staranja inhibiranih olj in tekočin - Preskus TOST - 1. del: Postopek za mineralna olja (ISO 4263-1:2003)

General Information

• Status: Published
• Publication Date: 21-Dec-2004
• Withdrawal Date: 29-Jun-2005
• ICS: 75.100 - Lubricants, industrial oils and related products
• Technical Committee: CEN/TC 19 - Petroleum products, lubricants and related products
• Drafting Committee: CEN/TC 19/WG 28 - Fire-resistant hydraulic fluids
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 22-Dec-2004
• Completion Date: 22-Dec-2004
• Mandate: M/238 - Mandate to CEN for standardization in the field of fire-resistant hydraulic fluids used for power transmission and control (hydrostatic and hydrokinetic)
• Ref Project: SIST EN ISO 4263-1:2005 - Petroleum and related products - Determination of the ageing behaviour of inhibited oils and fluids - TOST test - Part 1: Procedure for mineral oils (ISO 4263-1:2003)

Overview

EN ISO 4263-1:2004 / ISO 4263-1:2003 defines the TOST (Thin‑Film Oxygen‑Supply Test) procedure for assessing the ageing behaviour and oxidation stability of rust- and oxidation-inhibited mineral oils (density < water). It is intended for turbine oils (ISO 6743-5 categories TSA, TGA, TSE, TGE), hydraulic oils (ISO 6743-4 categories HL, HM, HR, HV, HG) and circulating oils (ISO 6743-6 category CKB). The test exposes oil samples to oxygen, heat and water in the presence of steel and copper catalyst coils at 95 °C and records the oxidation life as the hours required for the acid number to reach 2.0 mg KOH/g.

Key Topics

• Test principle: oil reacted with oxygen and water at 95 °C in glass oxidation cells with steel/copper catalyst coils; periodic sampling and acid-number measurement until the 2.0 mg KOH/g endpoint.
• Apparatus & consumables: borosilicate oxidation cell, thermostatically controlled heating bath (95 °C ±0.2 °C), oxygen supply (≥99.5% purity), catalyst wires (steel 1.60 mm ±0.05 mm, copper 1.63 mm ±0.05 mm), flowmeter and glassware.
• Reagents & solvents: laboratory-grade water (ISO 3696), heptane, acetone, isopropanol; cleaning solutions (chromosulfuric acid alternatives recommended because of chromium disposal issues).
• Measurements & results: acid number methods referenced (ISO 6618, ISO 6619, ISO 7537); oxidation life expressed in hours. Test may be stopped at a fixed time (e.g. 1 000 h) if required.
• Precision & limitations: precision was established only for inhibited turbine oils (oxidation lives 700–3 900 h). Oils with synthetic components can be tested but no precision statement is yet available. Correlation to field performance varies with application.
• Safety: warnings on oxygen handling and hazardous cleaning agents; appropriate safety and waste disposal practices required.

Applications

• Quality control and product development: lubricant manufacturers use the TOST test to compare oxidation stability and to screen inhibitor packages under water-contamination stress.
• Specifications and procurement: OEMs, spec writers and end-users reference EN ISO 4263-1 in supplier specifications for turbine, hydraulic and circulating oils.
• Laboratory testing & certification: independent test labs perform TOST testing to generate comparative oxidation-life data for datasheets and conformity assessment.
• Maintenance planning: used as an indicator of relative oxidative durability where oil is prone to water contamination, helping inform oil-change intervals and contamination controls.

Related Standards

• ISO 4263 series (Parts 2–4) - alternate procedures for other fluid types
• ISO 6743 series - fluid category definitions (turbine, hydraulic, circulating oils)
• ISO 3170, ISO 3696, ISO 6618, ISO 6619, ISO 7537 - referenced sampling, water quality and acid-number test methods

This standard is published by CEN/ISO and is widely cited in lubricant specifications where oxidation stability, TOST test, and ageing behaviour of inhibited oils are important selection criteria.

Standards Content (Sample)

SLOVENSKI STANDARD
01-marec-2005
1DIWDLQVRURGQLSURL]YRGL'RORþDQMHVWDUDQMDLQKLELUDQLKROMLQWHNRþLQ3UHVNXV
7267GHO3RVWRSHN]DPLQHUDOQDROMD,62
Petroleum and related products - Determination of the ageing behaviour of inhibited oils
and fluids - TOST test - Part 1: Procedure for mineral oils (ISO 4263-1:2003)
Mineralölerzeugnisse und verwandte Produkte - Bestimmung des Alterungsverhaltens
von inhibierten Ölen und Flüssigkeiten - TOST- Verfahren - Teil 1: Verfahren für
Mineralöle (ISO 4263-1:2003)
Pétrole et produits connexes - Détermination du comportement au vieillissement des
fluides et huiles inhibées - Essai TOST - Partie 1: Méthode pour les huiles minérales
(ISO 4263-1:2003)
Ta slovenski standard je istoveten z: EN ISO 4263-1:2004
ICS:
75.100 Maziva Lubricants, industrial oils and
related products
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
EN ISO 4263-1
NORME EUROPÉENNE
EUROPÄISCHE NORM
December 2004
ICS 75.100
English version
Petroleum and related products - Determination of the ageing
behaviour of inhibited oils and fluids - TOST test - Part 1:
Procedure for mineral oils (ISO 4263-1:2003)
Pétrole et produits connexes - Détermination du Mineralölerzeugnisse und verwandte Produkte -
comportement au vieillissement des fluides et huiles Bestimmung des Alterungsverhaltens von inhibierten Ölen
inhibées - Essai TOST - Partie 1: Méthode pour les huiles und Flüssigkeiten - TOST- Verfahren - Teil 1: Verfahren für
minérales (ISO 4263-1:2003) Mineralöle (ISO 4263-1:2003)
This European Standard was approved by CEN on 21 December 2004.
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, 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
© 2004 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 4263-1:2004: E
worldwide for CEN national Members.

Foreword
The text of ISO 4263-1:2003 has been prepared by Technical Committee ISO/TC 28 "Petroleum
products and lubricants” of the International Organization for Standardization (ISO) and has
been taken over as EN ISO 4263-1:2004 by 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 June 2005, and conflicting national
standards shall be withdrawn at the latest by June 2005.

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, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

Endorsement notice
The text of ISO 4263-1:2003 has been approved by CEN as EN ISO 4263-1:2004 without any
modifications.
INTERNATIONAL ISO
STANDARD 4263-1
First edition
2003-03-15
Petroleum and related products —
Determination of the ageing behaviour of
inhibited oils and fluids — TOST test —
Part 1:
Procedure for mineral oils
Pétrole et produits connexes — Détermination du comportement au
vieillissement des fluides et huiles inhibés — Essai TOST —
Partie 1: Méthode pour les huiles minérales

Reference number
ISO 4263-1:2003(E)
©
ISO 2003
ISO 4263-1:2003(E)
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ii © ISO 2003 — All rights reserved

ISO 4263-1:2003(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 . 6
7 Preparation of materials and apparatus . 6
8 Procedure . 8
9 Calculation. 9
10 Expression of results. 9
11 Precision . 9
12 Test report . 10
Annex A (normative) Liquid-in-glass thermometer specifications . 11
Annex B (normative) Procedure for packaging and storage of catalyst coils . 12
Annex C (informative) Method for the determination of the insolubles content of mineral oils . 13
Annex D (informative) Appearance rating of catalyst coil wires . 15
Annex E (informative) Determination of metals content . 16
Bibliography . 17

ISO 4263-1:2003(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 4263-1 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

iv © ISO 2003 — All rights reserved

INTERNATIONAL STANDARD ISO 4263-1:2003(E)

Petroleum and related products — Determination of the ageing
behaviour of inhibited oils and fluids — TOST test —
Part 1:
Procedure for mineral oils
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 rust- and oxidation-
inhibited mineral oils having a density less than that of water, used as turbine oils (categories TSA, TGA, TSE,
TGE of ISO 6743-5, see [4] in the Bibliography), hydraulic oils (categories HL, HM, HR, HV, HG of
ISO 6743-4, see [3] in the Bibliography), and circulating oils (category CKB of ISO 6743-6, see [5] in the
Bibliography). Oils containing synthetic components can be tested by this procedure, but no precision
statement is available yet for such fluids.
NOTE 1 For the purposes of this part of ISO 4263, the term "% (m/m)" is used to represent the mass fraction of a
material.
NOTE 2 Other signs of oil deterioration, such as the formation of insoluble sludge, catalyst coil corrosion or decrease in
pH value, may occur, which indicate oxidation of the oil, but are not reflected in the calculated oxidation lifetime. The
correlation of these occurrences with field service is under investigation.
This test method is widely used in specifications and is considered of value in comparing the oxidation stability
of oils that are 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 part of ISO 4263 for oxidation life was only determined on inhibited turbine oils, and
applies to oxidation lives of 700 h to 3 900 h.
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.
1)
ISO 3170:— , Petroleum liquids — Manual sampling
ISO 3696:1987, Water for analytical laboratory use — Specification and test methods

1) To be published. (Revision of ISO 3170:1988)
ISO 4263-1:2003(E)
ISO 6618:1997, Petroleum products and lubricants — Determination of acid or base number — Colour-
indicator titration method
ISO 6619:1988, Petroleum products and lubricants — Neutralization number — Potentiometric titration
method
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 in the presence of water and a steel and
copper catalyst coil. Small aliquots of the oil are withdrawn at regular intervals and the acid number is
measured (see Note 2 in Clause 1). The test is continued until an acid number 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. 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 as defined in
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 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
2 © ISO 2003 — All rights reserved

ISO 4263-1:2003(E)
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 when 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 to the strong oxidizing cleaning solution,
whenever the condition of the glassware permits this.
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 a 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 at
300 ml ± 1 ml, which applies to the test tube alone 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 oil test portion
in the oxidation cell at 95 °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, of minimum capacity 3 l/h and 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 calibrated to better than ± 0,1 °C. For metal-block heating
baths, a temperature-measurement system, with possibly more than one device of the same readability and
accuracy, is required.
ISO 4263-1:2003(E)
Dimensions in millimetres
Key
1 glass condenser 5 catalyst coil
2 oxygen-delivery tube 6 radius of bottom of cell
3 oil sample
a
Bend over mandrel of diameter 26
4 water
b
Grind end of tube
Figure 1 — Oxidation cell
4 © ISO 2003 — All rights reserved

ISO 4263-1:2003(E)
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 a thin stainless steel wire.
5.5 Wire-coiling mandrel. A 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
a) Bracket finished b) Development of bracket
Material: 18-8 stainless steel (0,792 mm)
Figure 2 — Thermometer bracket
ISO 4263-1:2003(E)
Dimensions in millimetres
Material: bronze
Key
1 lead
2 pitch
3 double thread
Figure 3 — 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 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 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.
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 catalysts
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
6 © ISO 2003 — All rights reserved

ISO 4263-1:2003(E)
with the abrasive cloth (4.8) until a fresh metal surface is exposed. Wipe with dry absorbent cotton until all the
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 Catalyst storage
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 e
...