Petroleum and related products - Determination of the ageing behaviour of inhibited oils and fluids - TOST test - Part 4: Procedure for industrial gear oils (ISO 4263-4:2006)

This part of ISO 4263 specifies a method for the determination of the ageing behaviour of gear oils of categories CKC, CKD, CKS and CKT as defined in ISO 6743-6[5]. The ageing is accelerated by the presence of air and elevated temperatures, and the degradation of the oil is assessed by the change in kinematic viscosity at 100 °C, the insoluble content (precipitation number), and possibly the acid number increase, the sediment content by filtration, the additives content variation and the infra-red oxidation.

Mineralölerzeugnisse und verwandte Produkte - Bestimmung des Alterungsverhaltens von inhibierten Ölen und Flüssigkeiten - TOST-Verfahren - Teil 4: Verfahren für Industriegetriebeöle (ISO 4263-4:2006)

Dieser Teil von ISO 4263 legt ein Verfahren fest zur Bestimmung des Alterungsverhaltens von Getriebeölen der Klassen CKC, CKD, CKS und CKT, wie sie in ISO 6743-6 [5] definiert sind. Die Alterung wird beschleunigt durch die Anwesenheit von Sauerstoff und durch erhöhte Temperaturen, und die Zerfallserscheinungen in der Flüssigkeit werden verfolgt über die Änderung der kinematischen Viskosität bei 100 °C, über den Gehalt an unlöslichen Anteilen (Ausfällungszahl). Bei Bedarf werden für die Ergebnisbeurteilung auch der Anstieg der Säurezahl, der Sedimentgehalt durch Filtration, Veränderungen im Additivgehalt und die infrarote Oxidation eingesetzt.

Pétrole et produits connexes - Détermination du comportement au vieillissement des fluides et huiles inhibés - Essai TOST - Partie 4: Méthode pour les huiles pour engrenages industriels (ISO 4263-4:2006)

L'ISO 4263-4:2006 spécifie une méthode permettant d'évaluer le comportement au vieillissement des huiles pour engrenages des catégories CKC, CKD, CKS et CKT, définies dans l'ISO 6743-6. Le vieillissement est accéléré par la présence d'air et par des températures élevées, et la dégradation de l'huile est suivie par l'évolution de la viscosité cinématique à 100 °C, par la teneur en produits insolubles (indice de précipitation) et, éventuellement, par l'accroissement de l'indice d'acide, la teneur en sédiments par filtration, l'évolution de la teneur en additifs et l'oxydation par infrarouge.

Nafta in sorodni proizvodi - Določanje staranja inhibiranih olj in tekočin - Preskus TOST - 4. del: Postopek za olja industrijskih naprav (ISO 4263-4:2006)

General Information

Status
Published
Publication Date
30-Apr-2006
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-May-2006
Due Date
01-May-2006
Completion Date
01-May-2006

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SLOVENSKI STANDARD
SIST EN ISO 4263-4:2006
01-maj-2006

1DIWDLQVRURGQLSURL]YRGL'RORþDQMHVWDUDQMDLQKLELUDQLKROMLQWHNRþLQ3UHVNXV

7267GHO3RVWRSHN]DROMDLQGXVWULMVNLKQDSUDY ,62

Petroleum and related products - Determination of the ageing behaviour of inhibited oils

and fluids - TOST test - Part 4: Procedure for industrial gear oils (ISO 4263-4:2006)

Mineralölerzeugnisse und verwandte Produkte - Bestimmung des Alterungsverhaltens
von inhibierten Ölen und Flüssigkeiten - TOST-Verfahren - Teil 4: Verfahren für
Industriegetriebeöle (ISO 4263-4:2006)

Pétrole et produits connexes - Détermination du comportement au vieillissement des

fluides et huiles inhibés - Essai TOST - Partie 4: Méthode pour les huiles pour
engrenages industriels (ISO 4263-4:2006)
Ta slovenski standard je istoveten z: EN ISO 4263-4:2006
ICS:
75.100 Maziva Lubricants, industrial oils and
related products
SIST EN ISO 4263-4:2006 en

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

---------------------- Page: 1 ----------------------
SIST EN ISO 4263-4:2006
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SIST EN ISO 4263-4:2006
EUROPEAN STANDARD
EN ISO 4263-4
NORME EUROPÉENNE
EUROPÄISCHE NORM
February 2006
ICS 75.100
English Version
Petroleum and related products - Determination of the ageing
behaviour of inhibited oils and fluids - TOST test - Part 4:
Procedure for industrial gear oils (ISO 4263-4:2006)

Pétrole et produits connexes - Détermination du Mineralölerzeugnisse und verwandte Produkte -

comportement au vieillissement des fluides et huiles Bestimmung des Alterungsverhaltens von inhibierten Ölen

inhibés - Essai TOST - Partie 4: Méthode pour les huiles und Flüssigkeiten - TOST-Verfahren - Teil 4: Verfahren für

pour engrenages industriels (ISO 4263-4:2006) Industriegetriebeöle (ISO 4263-4:2006)

This European Standard was approved by CEN on 9 January 2006.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European

Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national

standards may be obtained on application to the Central Secretariat or to any CEN member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by translation

under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official

versions.

CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,

Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,

Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
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EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels

© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 4263-4:2006: E

worldwide for CEN national Members.
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SIST EN ISO 4263-4:2006
EN ISO 4263-4:2006 (E)
Foreword

This document (EN ISO 4263-4:2006) has been prepared by Technical Committee ISO/TC 28

"Petroleum products and lubricants" in collaboration with Technical Committee CEN/TC 19

"Petroleum products, lubricants and related products", the secretariat of which is held by NEN.

This European Standard shall be given the status of a national standard, either by publication of

an identical text or by endorsement, at the latest by August 2006, and conflicting national

standards shall be withdrawn at the latest by August 2006.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of

the following countries are bound to implement this European Standard: Austria, Belgium,

Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary,

Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,

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

Endorsement notice

The text of ISO 4263-4:2006 has been approved by CEN as EN ISO 4263-4:2006 without any

modifications.
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SIST EN ISO 4263-4:2006
INTERNATIONAL ISO
STANDARD 4263-4
First edition
2006-02-01
Petroleum and related products —
Determination of the ageing behaviour of
inhibited oils and fluids — TOST test —
Part 4:
Procedure for industrial gear oils
Pétrole et produits connexes — Détermination du comportement au
vieillissement des fluides et huiles inhibés — Essai TOST —
Partie 4: Méthode pour les huiles pour engrenages industriels
Reference number
ISO 4263-4:2006(E)
ISO 2006
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SIST EN ISO 4263-4:2006
ISO 4263-4:2006(E)
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© ISO 2006

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ii © ISO 2006 – All rights reserved
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SIST EN ISO 4263-4:2006
ISO 4263-4:2006(E)
Contents Page

Foreword............................................................................................................................................................ iv

1 Scope ..................................................................................................................................................... 1

2 Normative references ........................................................................................................................... 1

3 Terms and definitions........................................................................................................................... 2

4 Principle................................................................................................................................................. 2

5 Reagents and materials ....................................................................................................................... 2

6 Apparatus .............................................................................................................................................. 3

7 Sampling................................................................................................................................................ 3

8 Preparation of apparatus — Cleaning of glassware ......................................................................... 5

9 Procedure .............................................................................................................................................. 5

10 Expression of results ........................................................................................................................... 6

11 Precision................................................................................................................................................ 6

12 Test report ............................................................................................................................................. 7

Annex A (normative) Liquid-in-glass thermometer specifications ............................................................... 8

Annex B (normative) Method for the determination of the insoluble content

(precipitation number).......................................................................................................................... 9

Annex C (informative) Method for the determination of the sediment content by filtration..................... 11

Annex D (informative) Method for the determination of the variation of the additives content............... 12

Annex E (informative) Method for the determination of the infra-red oxidation........................................ 13

Bibliography ..................................................................................................................................................... 15

© ISO 2006 – All rights reserved iii
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SIST EN ISO 4263-4:2006
ISO 4263-4:2006(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies

(ISO member bodies). The work of preparing International Standards is normally carried out through ISO

technical committees. Each member body interested in a subject for which a technical committee has been

established has the right to be represented on that committee. International organizations, governmental and

non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the

International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. Draft International Standards

adopted by the technical committees are circulated to the member bodies for voting. Publication as an

International Standard requires approval by at least 75 % of the member bodies casting a vote.

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent

rights. ISO shall not be held responsible for identifying any or all such patent rights.

ISO 4263-4 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 2006 – All rights reserved
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SIST EN ISO 4263-4:2006
INTERNATIONAL STANDARD ISO 4263-4:2006(E)
Petroleum and related products — Determination of the ageing
behaviour of inhibited oils and fluids — TOST test —
Part 4:
Procedure for industrial gear 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 gear oils of

[5]

categories CKC, CKD, CKS and CKT as defined in ISO 6743-6 . The ageing is accelerated by the presence

of air and elevated temperatures, and the degradation of the oil is assessed by the change in kinematic

viscosity at 100 °C, the insoluble content (precipitation number), and possibly the acid number increase, the

sediment content by filtration, the additives content variation and the infra-red oxidation.

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 2977:1997, Petroleum products and hydrocarbon solvents — Determination of aniline point and mixed

aniline point

ISO 3104:1994, Petroleum products — Transparent and opaque liquids — Determination of kinematic

viscosity and calculation of dynamic viscosity
ISO 3170:2004, Petroleum liquids — Manual sampling

ISO 3405:2000, Petroleum products — Determination of distillation characteristics at atmospheric pressure

ISO 3696:1987, Water for analytical laboratory use — Specification and test methods

ISO 3734:1997, Petroleum products — Determination of water and sediment in residual fuel oils — Centrifuge

method

ISO 12185:1996, Crude petroleum and petroleum products — Determination of density — Oscillating U-tube

method
© ISO 2006 – All rights reserved 1
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SIST EN ISO 4263-4:2006
ISO 4263-4:2006(E)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
insoluble content
precipitation number

number of millilitres of precipitate formed when 10 ml of lubricating oil are mixed with 90 ml of precipitation

naphtha, and centrifuged under the conditions of the test
3.2
sediment by filtration

amount of insoluble matter, expressed in milligrams per 100 ml, retained on a filtration membrane of 1,2 µm

pore size after filtration under vacuum
4 Principle

A test portion is reacted, in the absence of light, in the presence of air, and at a temperature appropriate to the

type of industrial gear oil under test: 95 °C for CKC type; 121 °C for CKD type; 150 °C for CKS and CKT types.

At the end of a 312 h period, the increase in kinematic viscosity at 100 °C, the insoluble content (precipitation

number), the increase in acid number (if required), the sediment content by filtration, the additives depletion

and the infra-red oxidation, are determined.
5 Reagents and materials

5.1 Water, unless otherwise specified, in accordance with the requirements of grade 2 as defined in

ISO 3696:1987. Potable water means tap water, unless normal piped supplies are contaminated with

particulate or highly soluble mineral content.
5.2 Heptane (C H ), of reagent grade and of minimum purity 99,75 %.
7 16
5.3 Acetone, (CH COCH ), of general purpose reagent grade (GPR).
3 3
5.4 Air, dried, oil-free, at constant pressure.

Supply from air cylinders or from a compressed air circuit is possible; this should be utilized via a regulation

system to improve the consistency of the air flow.
5.5 Cleaning solutions
5.5.1 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 sulphuric acid (8 g/l) have been found to give satisfactory cleanliness. A 10 % solution of three

parts of hydrochloric acid (1 mol/l) and one part of orthophosphoric acid (concentrated GPR grade) removes

iron oxide deposits.

WARNING — Chromosulfuric acid is a health hazard. It is toxic, a recognized carcinogen as it contains

Cr(VI) compounds, highly corrosive and potentially hazardous in contact with organic materials. When

using chromosulfuric acid cleaning solution, eye protection and protective clothing are essential.

Never pipette the cleaning solution by mouth. After use, do not pour cleaning solution down the drain,

but neutralize it with great care owing to the concentrated sulfuric acid present, and dispose of it in

accordance with standard procedures for toxic laboratory waste (chromium is highly dangerous to the

environment).
2 © ISO 2006 – All rights reserved
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SIST EN ISO 4263-4:2006
ISO 4263-4:2006(E)

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.
5.5.2 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.
5.5.3 Laboratory detergent
The detergent shall be water soluble.
6 Apparatus

6.1 Oxidation cell, consisting of a large test tube of borosilicate glass, 600 mm in length, of 41 mm inside

diameter, with a graduation mark to indicate a volume of 300 ml ± 1 ml at 20 °C, an air-delivery tube and a

slotted cork stopper. The design and dimensions shall be as illustrated in Figure 1.

New corks should be used for each test.

6.2 Heating bath, consisting of a thermostatically controlled bath capable of maintaining the test oil portion

in the oxidation cell at the specified temperature ± 0,2 °C. It shall be large enough to hold the required number

of oxidation cells (6.1) immersed in the heat-transfer medium so that the bath liquid is at least 50 mm above

the level of the oil sample. 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.

6.3 Flowmeters, capable of measuring a flow of air of 10 l/h with an accuracy of ± 0,5 l/h, one per oxidation

cell is required.
6.4 Temperature-measurement devices

6.4.1 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 ± 0,2 °C and calibrated to better than ± 0,2 °C.

6.4.2 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 ± 0,2 °C and calibrated to better than ± 0,2 °C.

6.5 Air-supply tube. Flexible polyvinylchloride (PVC) tubing of approximately 6,4 mm inside diameter and

1,5 mm wall thickness, is required to deliver air to the oxidation cell.

6.6 Air dryer. Between the air supply and the flowmeters, the air shall pass through a drying tower packed

with indicating gr
...

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