BS EN 14833-2005 Petroleum and related products - Determination of the hydrolytic stability of fire-resistant phosphate ester fluids《石油和相关产品 测定耐火磷酸酯液体的水解稳定性》.pdf

1、BRITISH STANDARDBS EN 14833:2005Petroleum and related products Determination of the hydrolytic stabilityof fire-resistant phosphate ester fluidsThe European Standard EN 14833:2005 has the status of a British StandardICS 75.080g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53

2、g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 14833:2005This British Standard was published under the authority of the Standards Policy and Strategy Committee on 28 July 2005 BSI 28 July 2005ISBN 0 580 46407 5Natio

3、nal forewordThis British Standard is the official English language version of EN 14833:2005.The UK participation in its preparation was entrusted to Technical Committee PTI/13, Petroelum testing and terminology, which has the responsibility to: aid enquirers to understand the text; present to the re

4、sponsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK.A list of organizations represented on this committee can be obtained on

5、request to its secretary.Cross-referencesThe British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogueunder the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI

6、Electronic Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard does not of itself confer immunity from legal obligations.Summary of pages

7、This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 9 and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. No. Date CommentsEUROPEAN STANDARDNORME EUROPENNEEURO

8、PISCHE NORMEN 14833June 2005ICS 75.080English versionPetroleum and related products - Determination of the hydrolyticstability of fire-resistant phosphate ester fluidsPtrole et produits connexes - Dtermination de larsistance lhydrolyse des fluides difficilementinflammables base desters phosphatesMin

9、erallerzeugnisse und verwandte Produkte -Bestimmung der hydrolytischen Stabilitt vonschwerentflammbaren Flssigkeiten auf der Basis vonPhosphorsureesternThis European Standard was approved by CEN on 25 May 2005.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate

10、the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in

11、three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Au

12、stria, 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 STANDARDIZ

13、ATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14833:2005: EEN 14833:2005 (E) 2ContentsPage Foreword 31 Sco

14、pe .42 Normative references .43 Terms and definitions.44 Principle.55 Reagents and materials56 Apparatus 57 Samples and sampling .68 Preparation of glassware79 Procedure 710 Calculation.711 Expression of results812 Precision813 Test report .8Bibliography.9EN 14833:2005 (E)3Foreword This European Sta

15、ndard (EN 14833:2005) has been prepared 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 endorseme

16、nt, at the latest by December 2005, and conflicting national standards shall be withdrawn at the latest by December 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

17、, 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. EN 14833:2005 (E) 41 Scope This European Sta

18、ndard specifies a method for the determination of the hydrolytic stability of phosphate ester fire-resistant hydraulic fluids. These fluids fall under category HFDR of EN ISO 6743-4 2 and categories TSD, TGD and TCD of ISO 6743-5 3. Hydrolysis results in the formation of acid, measurement of which i

19、s effected by using one of the test methods ISO 6618, ISO 6619 or ISO 7537.Results from two different test methods are not necessarily compatible and direct comparison needs caution. The method is applicable to hydrolytic stability results of up to 0,50 mg KOH/g. NOTE This test may also be applied t

20、o other non-aqueous fire-resistant fluids, such as those falling into category HFDU of EN ISO 6743-4 2. WARNING The use of this European Standard may involve hazardous materials, operations and equipment. This document does not purport to address all of the safety problems associated with its use. I

21、t is the responsibility of the user of this document to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2 Normative references The following referenced documents are indispensable for the application of this document. For date

22、d references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN ISO 3170, Petroleum liquids Manual sampling (ISO 3170:2004)EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3

23、696:1987) ISO 6618, Petroleum products and lubricants Determination of acid or base number Colour-indicator titration method ISO 6619, Petroleum products and lubricants Neutralization number Potentiometric titration methodISO 7537, Petroleum products Determination of acid number Semi-micro colour-in

24、dicator titration method3 Terms and definitions For the purposes of this European Standard, the following terms and definitions apply. 3.1 hydrolytic stability sum of the changes in acid number of a fire-resistant fluid and in acid number of water when contacted for 96 h under the conditions of this

25、 document EN 14833:2005 (E)54 Principle The sample is hydrolysed with water in the ratio 3:1 for 96 h at 85 C. Special attention is given to the fact that this static test is performed without stirring. The acid number of both fluid and water phases is determined before and after the period, and the

26、 sum of the increases recorded as the hydrolytic stability. 5 Reagents and materials 5.1 Water, conforming to grade 3 of EN ISO 3696. 6 Apparatus 6.1 GeneralTapered ground-glass and vapour-tight joints specified for the glassware in this document shall be either 29/32 or 29/43. It is important that

27、whichever series is chosen, the male and female joints are of the same length. A general schematic diagram of the apparatus is given in Figure 1. 6.2 Balance, with a capacity of 1 kg minimum, capable of weighing to the nearest 0,1 g or better. 6.3 Flask, constructed from borosilicate glass, conical,

28、 500 ml capacity and fitted with a female tapered ground-glass joint. 6.4 Adaptors6.4.1 Two-neck adaptor, fitted with a male tapered ground-glass joint at the bottom and with parallel necks each fitted with a female tapered ground-glass joint. 6.4.2 Joint adaptor, with a male tapered ground-glass jo

29、int at the bottom and screwed connecting caps to hold the temperature sensor (6.7). 6.5 Condenser, of the jacketed-coil type, fitted with a male tapered ground-glass joint at the bottom end and a female tapered ground-glass joint at the other, with a minimum length of 250 mm, and supplied with a pol

30、ytetrafluoroethylene (PTFE) collar and a polyethylene stopper fitting the female joint. 6.6 Oil bath, fitted with variable temperature control in the range 85 C to 95 C and of sufficient depth to immerse the flask (6.3) in the liquid up to the neck without resting on the bottom. NOTE A suitable hold

31、er suspended from the top of the bath giving the specified immersion, is recommended. 6.7 Temperature sensor, a liquid-in-glass total immersion thermometer of nominal range 0 C to 100 C, readable to 0,2 C or better, or a temperature measurement device or system of at least equivalent accuracy. 6.8 S

32、eparating funnel, stoppered funnel of 500 ml capacity. 6.9 Oven, controlled at 105 C 5 C for drying glassware. EN 14833:2005 (E) 6Key1 Conical Flask (6.3) 2 Two neck adaptor (6.4.1) 3 Condenser with stopper (6.5) 4 Joint adaptor (6.4.2) 5 Temperature sensor (6.7) Figure 1 Schematic drawing of the te

33、st apparatus 7 Samples and sampling 7.1 Unless otherwise specified, samples shall be taken as described in EN ISO 3170 and/or in accordance with the requirements of national standards or regulations for the sampling of the product under test. 7.2 The test portion shall be clear and bright. The prese

34、nce of any sediment or free or dispersed water shall be noted in the test report and removed by filtration or decantation prior to testing. EN 14833:2005 (E)78 Preparation of glassware Ensure that the glassware is clean and dry before use. Use suitable solvents and non-ionic detergents for prelimina

35、ry cleaning, followed by thorough rinsing with water (5.1). Dry in the oven (6.9) for 30 min and allow to cool in a covered vessel. 9 Procedure 9.1 Determine the acid number of the sample and the acid number of the water (5.1) in accordance with the titration procedure specified in ISO 6618, ISO 661

36、9 or ISO 7537. 9.2 Weigh the flask (6.3) to the nearest 0,1 g. 9.3 Add 300 g 0,1 g of sample to the flask (6.3), followed by 100 g 0,1 g of the water (5.1). Record the total mass. 9.4 Fit the PTFE collar to the curved part of the two-neck adaptor (6.4.1), and then fit the condenser (6.5). 9.5 Fit th

37、e joint adaptor (6.4.2) to the straight-through part of the two-neck adaptor, and insert the temperature sensor to a depth so that the bottom of the bulb or sensing device is 10 mm 1 mm from the bottom of the flask. 9.6 Fit the stopper in the condenser, and switch on the cooling water. 9.7 Place the

38、 assembled apparatus in the bath (6.6) up to the bottom of the neck of the flask (see NOTE under 6.6). The bath shall be controlled at a temperature that maintains the test portion plus water at a temperature of 85 C 1 C. Note the time when the temperature of the liquid in the flask reaches 84 C as

39、the start of the test. NOTE The appropriate temperature should be determined by preliminary trials, and will be dependent on the bath design, capacity and loading. Normally, it will be in the range 88 C to 95 C.9.8 After 96 h 1 h, remove the apparatus from the bath and allow the mixture of test port

40、ion and water to cool to room temperature. 9.9 Disassemble the apparatus and clean and dry the outside surface of the flask. Weigh, and add water (5.1) if necessary to match the total mass recorded in 9.3 to 0,1 g. 9.10 Transfer the mixture of test portion and water from the flask (6.3) to the separ

41、ating funnel (6.8) and wait until separation is complete. If separation is not complete in 50 min, but sufficient clear liquid is available in each phase to complete 9.11, carry out the procedure given in 9.11. If insufficient clear liquid is available in either phase, leave for up to an additional

42、1 h and take a test portion from each phase as soon as sufficient clear liquid is available. Report the result as “late“. If, after 1 h 50 min, there is still insufficient phase separation, report the result as “unobtainable”. 9.11 Remove a test portion from each of the two phases and determine the

43、acid number in accordance the selected titration method (see Clause 1). 10 Calculation Calculate the hydrolytic stability, HS, expressed in milligrams of KOH per gram, as the sum of the differences in acid number of sample and water before and after thermal stress, using: EN 14833:2005 (E) 8()( )HS

44、A A A A=+21 43(1)where A1is the acid number of the sample before ageing (9.1), expressed to the nearest 0,01 mg KOH per gram;A2is the acid number of the sample after ageing (9.10), expressed to the nearest 0,01 mg KOH per gram;A3is the acid number of the water before ageing (9.2), expressed to the n

45、earest 0,01 mg KOH per gram;A4is the acid number of the water after ageing (9.11), expressed to the nearest 0,01 mg KOH per gram. 11 Expression of results Report the result, calculated following Clause 10, to the nearest 0,01 mg KOH/g. Report the presence of sediment and/or water if noted in 7.2. Re

46、port results as “late“ or “unobtainable“ if the corresponding conditions of 9.10 apply. 12 Precision 12.1 General The precision, as obtained by statistical examination of inter-laboratory test results according to EN ISO 4259 1, is given in 12.2 and 12.3. 12.2 Repeatability The difference between tw

47、o results obtained by the same operator with the same apparatus under constant operating conditions on identical test material would in the long run, in the normal and correct operation of the test method, exceed 0,08 mg KOH/g in only one case in twenty. 12.3 Reproducibility The difference between t

48、wo single and independent test results obtained by different operators working in different laboratories on identical material would in the long run, in the normal and correct operation of the test method, exceed 0,16 mg KOH/g in only one case in twenty. 13 Test report The test report shall contain

49、at least the following information: a) reference to this European Standard; b) type and complete identification of the product tested; c) result of the test (see 11); d) any deviation, by agreement or otherwise, from the procedure specified; e) date of the test. EN 14833:2005 (E)9Bibliography 1 EN ISO 4259, Petroleum products Determination and application of precision data in relation to methods of test (ISO 4259:1992/Cor 1:1993).2 EN ISO 6743-4, Lubricants, industrial oils and related products (clas