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
28-Feb-2005
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-Mar-2005
Due Date
01-Mar-2005
Completion Date
01-Mar-2005

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SLOVENSKI STANDARD
SIST EN ISO 4263-1:2005
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
SIST EN ISO 4263-1:2005 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 4263-1:2005
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SIST EN ISO 4263-1:2005
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.
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SIST EN ISO 4263-1:2005
EN ISO 4263-1:2004 (E)
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.
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SIST EN ISO 4263-1:2005
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
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SIST EN ISO 4263-1:2005
ISO 4263-1:2003(E)
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ii © ISO 2003 — All rights reserved
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SIST EN ISO 4263-1:2005
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 2003 — All rights reserved iii
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SIST EN ISO 4263-1:2005
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
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SIST EN ISO 4263-1:2005
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.
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 2003 — All rights reserved 1
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SIST EN ISO 4263-1:2005
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
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SIST EN ISO 4263-1:2005
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 2003 — All rights reserved 3
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SIST EN ISO 4263-1:2005
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
Bend over mandrel of diameter 26
4 water
Grind end of tube
Figure 1 — Oxidation cell
4 © ISO 2003 — All rights reserved
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SIST EN ISO 4263-1:2005
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 2003 — All rights reserved 5
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SIST EN ISO 4263-1:2005
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
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SIST EN ISO 4263-1:2005
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 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 at approximately

100 °C or with 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 oil completely from the test tube and rinse all

glassware with heptane (4.2) to remove traces of oil. 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 may 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 of 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 device and/or any other devices used and rinse any surfaces that

have contacted the oil with heptane (4.2) to remove traces of oil. 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.
© ISO 2003 — All rights reserved 7
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SIST EN ISO 4263-1:2005
ISO 4263-1:2003(E)
8 Procedure

8.1 Adjust the heating bath to a temperature that will maintain the temperature in the oil in the oxidation

cells (5.1) at 95 °C ± 0,2 °C throughout the duration of the test, with oxygen passing through the cells at

3 l/h ± 0,5 l/h.

NOTE The temperature of the heating bath (5.2) will be above 95 °C due to the cooling effect of the oxygen flow, but

the specific temperature will depend on 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.

8.2 Measure the temperature in each cell containing 360 ml of fluid (which may be 300 ml of oil plus 60 ml

of water), 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 a 0,1 °C subtraction

to allow for emergent-stem heating.

8.3 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 the test fluid type, necessitates a check on the level and uniformity of temperature control. All temperature

measurements are carried out on new, undepleted test portions and/or dummy cells. Immediately the

temperature control has been established, remove the temperature-measurement devices.

8.4 Fill the empty oxidation test tube with 300 ml of mineral oil (up to the graduation mark). 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 in the test tube, and place the condenser over the

oxygen-delivery tube and test tube. If used, a sampling tube and holder 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.

8.5 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 dr
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