1、EUROPEAN STANDARD EUROPISCHE NORM NORME EUROPENNE H 3404583 OL078LO 071 EN 60867 January 1994 Supersedes 11) 497 S1 : 1987 Descriptors: Liquid electrical insulating materials, aromatic hydrocarbons, specifications, characteristics, tests English version Insulating liquids - Specifications for unused
2、 liquids based on synthetic aromatic hydrocarbons (IEC 867 : 1993 ) Isolants liquides Spcifications pour liquides neufs base dhydrocarbures aromatiques de synthse synthetischer aromatischer (CE1 867 : 1993) Kohlenwasserstoffe Isolierflssigkeiten Bestimmungen fr ungebrauchte Isolierflssigkeiten auf B
3、asis (IEC 867 : 1993) This European Standard was approved by CENELEC on 1993-12-08. CENELEC members are bound to comply with the CENKENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists
4、 and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CENELEC member. This European Standard exists in t,hree official versions (English, French, German). A version in any other language made by translation under the re
5、sponsibility of a CENELEC member into its own language and notified to the Central Secretariat has the same status as the official versions. CENELEC members are the national electrotechnical committees of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembour
6、g, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CENELEC European Committee for Electrotechnical Standardization Comit Europen de Normalisation Electrotechnique Europisches Komitee fr Elektrotechnische Normung Central Secretariat: rue de Stassart 35, B-1050 Brussels O
7、 1994 Copyright reserved to CENELEC members Ref. No. EN 60867 : 1994 E H 3404583 OLO78Ll TOB Page 2 EN 60867 : 1994 Foreword The text of document 10(C0)269, as prepared by IEC Technical Committee No. 10: Fluids for electrotechnical applications, was submitted to the IEC-CENELEC parallel vote in Octo
8、ber 1992. The reference document was approved by CENELEC as EN 60867 on 8 December 1993. This European Standard replaces HD 497 S1 : 1987. The following dates were fixed: - latest date of publication of an identical national standard (dop) 1994-12-01 - latest date of withdrawal of conflicting nation
9、al standards (dow) 1994-12-01 For products which have complied with HD 497 S1 : 1987 before 1994-12-01, as shown by the manufacturer or by a certification body, this previous standard may continue to apply for production until 1999-12-01. Annexes designated normative are part of the body of the stan
10、dard. In this standard, annex LA is normative. E 3404583 OL07L2 944 Page 3 EN 60867 : 1994 CONTENTS Page Clause 1 2 3 4 5 6 7 8 9 10 11 Scope 4 Normative references 4 Definitions . 5 Identification and general delivery requirements . 5 Sampling 5 Test methods 6 Precision and interpretation of test r
11、esults . 9 Specifications for capacitor and cable alkylbenzenes . 9 Specifications for capacitor alkyldiphenylethanes . 9 Specifications for Capacitor alkyinaphthalenes . 10 Specifications for capacitor methylpolyarylmethanes 10 Sheets of specifications 1 to 4 . 11 Annex ZA (normative) Other interna
12、tional publications quoted in this standard with the references of the relevant European publications 15 = 3404583 Ol1078L3 880 = Page 4 EN 60867 : 1994 INSULATING LIQUIDS - SPECIFICATIONS FOR UNUSED LIQUIDS BASED ON SYNTHETIC AROMATIC HYDROCARBONS 1 Scope This International Standard covers specific
13、ations and test methods for unused synthetic aromatic hydrocarbons intended for use as insulating liquid in electrical equipment. 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. A
14、t the time of publication, the editions indicated were valid. All normative documents are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below.
15、 Members of IEC and IS0 maintain registers of currently valid International Standards. IEC 156: 1963, Method for the determination of the electric strength of insulating oils IEC 247: 1978, Measurement of relative permittivity, dielectric dissipation factor and d.c. resis tivit y of ins ula ting liq
16、uids IEC 475: 1974, Method of sampling liquid dielectrics IEC 628: 1985, Gassing of insulating liquids under electrical stress and ionization IEC 8 14: 1 985, Determination of water in insulating liquids by automatic coulometric Karl Fischer titration IEC 1039: 1990, General classification of insula
17、ting liquids IS0 2719: 1988, Petroleum products and lubricants - Determination of flash point - Pensky-Martens closed cup method IS0 301 6: 1974, Petroleum oils - Determination of pour point IS0 31 04: 1976, Petroleum products - Transparent and opaque liquids - Determination of kinematic viscosity a
18、nd calculation of dynamic viscosity IS0 3675: 1976, Crude petroleum and liquid petroleum products - Laboratory deter- mination of density or relative density - Hydrometer method IS0 5662: 1978, Petroleum products - Electrical insulating oils - Detection of corrosive sulphur Page 5 EN 60867 : 1994 3
19、Definitions General remark Gas chromatographic analyses can be useful for composition identification and detection of impurities. For the purposes of this International Standard, the following definitions apply. 3.1 alkylbenzenes: Insulating liquids consisting of a benzene ring and an alkylgroup. Th
20、e alkyl group may be a straight chain or a branched-chain type. NOTE - The two types of alkylbenzene can be distinguished by infra-red spectrophotometric analysis. The straight-chain type shows a single absorption peak in the region 1 360 cm-1 to 1 380 cm-l and !he branched chain type shows a double
21、 peak in that region. 3.2 alkyldiphenylethanes: Insulating liquids consisting of diphenylethanes derivatives; normally the two aryl groups carry short alkyl groups. NOTE - This type of product is characterized by infrared absorption bands at 3 070, 1 606 and 705 cm-l. 3.3 alkylnaphthalenes: Insulati
22、ng liquids consisting of a naphthalene structure with substituent aklyl groups. NOTE - This type of product is characterized by infrared absorption bands at 3 070. 1 605, 1 380 and 1 360 cm-. 3.4 rnethylpolyarylmethanes: Insulating liquids consisting of methylpolyarylmethanes derivatives mainly base
23、d on a blend of mono/di-benzyl toluene (M/DBT). NOTE - This type of product is characterized by infrared absorption bands at 3 025, 1 606 and 705 cm-l. 4 Identificatlon and general delivery requirements 4.1 The products are normally delivered in road or rail tank wagons or in drums, which shall be s
24、pecially cleaned for this purpose. 4.2 The drums and sample containers shipped by the supplier shall carry at least the fo I low i ng markings : - number of this standard; - suppliers designation; - type of product. 5 Sampling Sampling shall be carried out in accordance with the procedure described
25、in IEC 475. = 3404583 0307835 653 Page 6 EN 60867 : 1994 6 Test methods 6.1 Appearance Appearance shall be evaluated by examining, in transmitted light, a representative sample of the liquid having a thickness of approximately 10 cm, at ambient temperature. 6.2 Density Any recognized test method may
26、 be used. In case of dispute, the method to be used shall be that given in IS0 3675. Density shall be measured at 20 OC. 6.3 Kinematic viscosity Kinematic viscosity shall be measured according to IS0 31 04. 6.4 Flash-point Flash-point shall be determined according to IS0 2719. 6.5 Pour-point Pour-po
27、int shall be determined according to IS0 301 6. 6.6 Neutralization value 6.6.1 Reagents a) Standard alcoholic potassium hydroxide (KOH) solution 0,l mol/dmJ. b) Toluene, sulphur-free. c) Azeotropic ethanol (boiling-point 782 OC). d) Standard hydrochloric acid solution (HCI) 011 mol/dmJ. e) Alkali bl
28、ue indicator solution: 2 g of alkali blue 6 B are dissolved in 100 cm3 of azeotropic ethanol containing 1 cm3 hydrochloric acid 0,l moI/cm3. After 24 h, carry out an acid value test to check whether the indicator has been sufficiently sensitized. The indicator is satisfactory if the colour changes d
29、istinctly from blue to a red comparable to that of a 10 Y solution of cobalt nitrate Co(N0,),.6H20. Should sensitization be insufficient, repeat the addition of 0,l mol/dm3 hydrochloric acid and check again after 24 h. Continue until sensitization is satisfactory. Filter and store in a brown glass b
30、ottle in the dark. 6.6.2 Procedure Weigh 20 g of the sample to the nearest 0.05 g into a 250 cm3 stoppered conical flask. To a mixture of 60 cm3 of toluene and 40 cm3 of ethanol in a second flask add 2 cm3 of indicator solution. Neutralize the solution with 0,l mol/dmJ KOH solution until a red colou
31、r comparable to that of a solution of 10 % cobalt nitrate Co(N0,),.6H20 is obtained and persists for at least 15 s. 3404583 01078Lb 57T Page 7 EN 60867 : 1994 Add this solution to the sample, swirl and immediately titrate at a temperature not above 25 OC with 0,l mol/dm3 KOH solution to the above en
32、d-point. The neutralization value (NV) is calculated from the expression: V x N x 56,l m NV= where V is the number of cubic centimeters of 0,l molldm3 KOH used in the titration N is the molarity of the KOH solution m is the mass of the sample in grams 6.7 Chlorine content The method described in thi
33、s subclause IS suitable for obtaining the total chlorine content in hydrocarbon liquids. However, any other chemical or instrumental method known to pro- duce comparable results could be used. 6.7.1 Reagents - Standard solution of nitric acid (HNO,), analytical grade. Dilute 190 g of concen- trated
34、nitric acid to 1 dm3 with distilled water. - Isopropyl alcohol, analytical grade. - Silver nitrate (ASNO,), analytical grade. Standard solution (0,025 mol/drn3) - Weigh accurately 0,4247 g of silver nitrate. Transfer it to 1 litre volumetric flask and add distilled water to dissolve. Add 3 cm3 of co
35、ncentrated nitric acid (density 1,42 kg/dm3) and then add distilled water to the 1 dm3 mark of the volumetric flask. Standardize this solution against a pure chloride standard. Check the solution at least monthly to assure a constant reagent. NOTES 1 A sodium chloride crystal as used in infra-red sp
36、ectrometer cells is a suitable chloride standard. 2 the solution must be protected from light by storage in brown glassware in the dark. Dry the silver nitrate overnight in a desiccator before making up the solution. Both the solid material and - Sodium diphenyl solution (C,H5C6H,Na) NOTE - Organic
37、halogen reagent: 30 cm3 of this reagent are normally required to give excess reagent. Preparation of sodium diphenyl solution is described in McCoy - The Inorganic Analysis of Petroleum, Chemical Publishing Co. Inc 212 Fifth Avenue, New York. 6.7.2 Apparatus - Separatory funnel, 250 cm3. - Potentiom
38、etric titration apparatus. - Electrodes: silver and glass electrode combination is preferred. A silver electrode with a mercurous sulphate reference electrode is an acceptable alternative. - Microburette, 5 cm3 with 0.01 cm3 divisions. Page u EN 60867 : 1994 3404583 Ol107BL7 426 6.7.3 Procedure 6.7.
39、3.1 Dissolve 3559 f 0,1 g of the liquid under test in 25 cm3 toluene in a 150 cm3 beaker by stirring with a small glass rod. Transfer the solution to a separatory funnel. Rinse the beaker several times with a total of 25 cm3 toluene and add the rinses to the funnel. 6.7.3.2 Add an excess (about 30 c
40、m3 is usually sufficient) of sodium diphenyl solution to the contents of the separatory funnel. The excess is indicated by a colour change of blue or green. Stopper the vessel and gently shake to thoroughly mix the solution, venting occa- sionally to release the excess pressure build-up. 6.7.3.3 All
41、ow the blue-green mixture to stand 5 min to ensure complete reaction. Remove stopper, add 2 cm3 of isopropyl alcohol, and swirl with stopper removed until excess reagent is destroyed. 6.7.3.4 Add slowly 50 cm3 of the nitric acid solution. Ensure that the organic and aqueous phases are in intimate an
42、d uniform contact by gentle swirling and rocking for 5 min. Loosen the stopper occasionally to release slight pressure. Drain the aqueous phase into a beaker. Extract the organic phase twice more with 50 cm3 portions of nitric acid solution. Drain the aqueous phases into the beaker containing the fi
43、rst extract. 6.7.3.5 Place the beaker containing the aqueous phase on the titration stand and insert the electrode system. Start the stirrer and record the initial value of potential or pH. Titrate slowly with ASNO, solution (0,025 mol/dm3), recording readings after the addition of each drop of ASNO
44、, solution. Continue titrating until the point of maximum change in potential or pH scale reading is reached. Plot the volume of silver nitrate as abscissa and voltage or pH reading as ordinates. The end-point is selected at the point of inflection of the curve. 6.7.3.6 Blank. Titrate the same volum
45、e of solvent without the sample, as a blank. 6.7.4 Calculation Calculate the amount of total chlorine as follows: Total chlorine (mg/kg) = (A - B) Nlm 355 x lo3 where A is the number of cubic centimetres of ASNO, solution required for titration of the sample B is the number of cubic centimetres of A
46、SNO, solution required for titration of the blank N is the molarity of the ASNO, solution rn is the mass in grams of sample used 35.5 is the atomic mass of chlorine Page 9 EN 60867 : 1994 = 3404583 0107818 362 6.8 Water content Water content shall be determined according to IEC 814. 6.9 Corrosive su
47、lphur Corrosive sulphur shall be determined according to IS0 5662. 6.1 O Breakdown voltage Breakdown voltage shall be determined according to IEC 156. 6.1 1 Dielectric dissipation factor and volume resistivity The properties shall be determined according to IEC 247 6.12 The gassing shall be determin
48、ed by either Method A or Method B of IEC 628. Stability under electrical stress and ionization (gassing) 7 Precision and interpretation of test results Precision data given in the specified methods are to be used solely as a guide to the expected agreement between duplicate measurements of the prope
49、rty and are not to be regarded as tolerances applicable to the limits specified in sheets 1, 2, 3 and 4. 8 Specifications for capacitor and cable alkylbenzenes When tested in accordance with the methods specified in clause 6, the properties of alkylbenzene-based products which are intended for use as impregnants in capacitors and hollow-core cables shall meet the requirements given in the specification sheet 1. According to IEC 1039 they are designated as follows: L-NY-867-1. NOTE - Alkylbenzenes are sometimes used in transformers but this application is not wide e
