1、 DEUTSCHE NORM May 2006DIN EN ISO 4263-4 ICS 75.100 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) English version of DIN EN ISO 4263-4:2006-05 Minerallerzeugnisse und verwandte
2、Produkte Bestimmung des Alterungsverhaltens von inhibierten len und Flssigkeiten TOST-Verfahren Teil 4: Verfahren fr Industriegetriebele (ISO 4263-4:2006) Englische Fassung DIN EN ISO 4263-4:2006-05 Document comprises 21 pages No part of this standard may be reproduced without prior permission of DI
3、N Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany, has the exclusive right of sale for German Standards (DIN-Normen). English price group 11 www.din.de www.beuth.de !,nlw“11.06 9757384DIN EN ISO 4263-4:2006-05 2 National foreword This standard has been published
4、 in accordance with a decision taken by CEN/TC 19 to adopt, without alteration, International Standard ISO 4263-4 as a European Standard. The responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Technical Committee NMP 68
5、1 Gasfrmige und flssige Kraft- und Brennstoffe, Schmierstoffe und verwandte Produkte mit minerallstmmiger, synthetischer oder biologischer Herkunft of the Fachausschuss Minerall- und Brennstoffnormung (FAM). DIN EN ISO 4263 consists of the following Parts, under the general title Petroleum and relat
6、ed products Determination of 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 The DIN Standards corresp
7、onding to the International Standards referred to in clause 2 of the EN are as follows: ISO 2977 DIN ISO 2977 ISO 3104 DIN EN ISO 3104 ISO 3170 DIN EN ISO 3170 ISO 3405 DIN EN ISO 3405 ISO 3696 DIN EN ISO 3696 ISO 4259 DIN EN ISO 4259 ISO 12185 DIN EN ISO 12185 DIN EN ISO 4263-4:2006-05 3 National A
8、nnex NA (informative) Bibliography DIN EN ISO 3104, Petroleum products Transparent and opaque liquids Determination of kinematic viscosity and calculation of dynamic viscosity DIN EN ISO 3170, Petroleum liquids Manual sampling DIN EN ISO 3405, Petroleum products Determination of distillation charact
9、eristics at atmospheric pressure DIN EN ISO 4259, Petroleum products Determination and application of precision data in relation to methods of test DIN EN ISO 12185, Crude petroleum and petroleum products Determination of density Oscillating U-tube method DIN ISO 2977, Petroleum products and hydroca
10、rbon solvents Determination of aniline point and mixed aniline point DIN ISO 3696, Water for analytical laboratory use Specification and test methods EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 4263-4 February 2006 ICS 75.100 English Version Petroleum and related products - Determinatio
11、n of the ageing behaviour of inhibited oils and fluids - TOST test - Part 4: Procedure for industrial gear oils (ISO 4263-4:2006) Ptrole et produits connexes - Dtermination du comportement au vieillissement des fluides et huiles inhibs - Essai TOST - Partie 4: Mthode pour les huiles pour engrenages
12、industriels (ISO 4263-4:2006) Minerallerzeugnisse und verwandte Produkte - Bestimmung des Alterungsverhaltens von inhibierten len und Flssigkeiten - TOST-Verfahren - Teil 4: Verfahren fr Industriegetriebele (ISO 4263-4:2006) This European Standard was approved by CEN on 9 January 2006. CEN members a
13、re 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
14、 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 s
15、tatus 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, Slova
16、kia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2006 CEN All rights of exploitation in any form and by any means reserved worldwide
17、 for CEN national Members. Ref. No. EN ISO 4263-4:2006: EEN ISO 4263-4:2006 (E) 2 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
18、 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 Aug
19、ust 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,
20、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. EN ISO 4263-4:2006 (E) 3 C
21、ontents Page Foreword .2 1 Scope4 2 Normative references4 3 Terms and definitions .5 4 Principle .5 5 Reagents and materials 5 6 Apparatus.6 7 Sampling 6 8 Preparation of apparatus Cleaning of glassware8 9 Procedure.8 10 Expression of results9 11 Precision 9 12 Test report10 Annex A (normative) Liqu
22、id-in-glass thermometer specifications11 Annex B (normative) Method for the determination of the insoluble content (precipitation number) 12 Annex C (informative) Method for the determination of the sediment content by filtration .14 Annex D (informative) Method for the determination of the variatio
23、n of the additives content .15 Annex E (informative) Method for the determination of the infra-red oxidation 16 Bibliography18 EN ISO 4263-4:2006 (E) 4 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 addres
24、s 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 de
25、termination of the ageing behaviour of gear oils of categories CKC, CKD, CKS and CKT as defined in ISO 6743-65. 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
26、(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
27、 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 op
28、aque 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 Specifica
29、tion 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 EN ISO 4263-4:2006 (E) 5 3 Terms and definitions For the purpo
30、ses 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 filtra
31、tion amount of insoluble matter, expressed in milligrams per 100 ml, retained on a filtration membrane of 1,2 m 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 g
32、ear 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 additiv
33、es 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 highl
34、y soluble mineral content. 5.2 Heptane (C7H16), of reagent grade and of minimum purity 99,75 %. 5.3 Acetone, (CH3COCH3), of general purpose reagent grade (GPR). 5.4 Air, dried, oil-free, at constant pressure. Supply from air cylinders or from a compressed air circuit is possible; this should be util
35、ized 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 contain
36、ing 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 Chromos
37、ulfuric 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 t
38、he 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 environm
39、ent). EN ISO 4263-4:2006 (E) 6 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 stron
40、g 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 glas
41、s, 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
42、 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 t
43、he 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 t
44、otal 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
45、 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
46、 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 dia
47、meter 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 grade anhydrous calcium sulfate or equivalent. The quantity of desiccant shall be sufficient t
48、o last for the entire test. 7 Sampling Unless otherwise specified, samples shall be obtained in accordance with the procedures described in ISO 3170. EN ISO 4263-4:2006 (E) 7 Dimensions in millimetres Key 1 slotted cork stopper a60 to 80 mm. 2 glass air-supply tube bInternal diameter. 3 borosilicate
49、 test tube 4 test sample, 300 ml Figure 1 Oxidation cell EN ISO 4263-4:2006 (E) 8 8 Preparation of apparatus Cleaning of glassware 8.1 Cleaning new glassware Wash new air-delivery tubes and oxidation cells with hot detergent solution (see 5.5.3) and rinse thoroughly with potable water (5.1). Clean the interior of the oxidation cells, and both interiors and exteriors of the air-delivery tubes by either soaking for 24 h in a 10 % solution of the surfactant clean
