DIN EN 15471-2017 Liquefied petroleum gases - Determination of dissolved residues - High-temperature gravimetric method German version EN 15471 2017《液化石油气 溶解的残留物的测定 高温重量分析法 德文版本EN .pdf

1、September 2017 English price group 8No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 75.160.20!%muf“2748267www.din.d

2、eDIN EN 15471Liquefied petroleum gases Determination of dissolved residues Hightemperature gravimetric method;English version EN 15471:2017,English translation of DIN EN 15471:2017-09Flssiggas Bestimmung der gelsten Rckstnde Gravimetrisches Hochtemperaturverfahren;Englische Fassung EN 15471:2017,Eng

3、lische bersetzung von DIN EN 15471:2017-09Gaz de ptrole liqufi Dtermination des rsidus dissous Mthode gravimtrique haute temprature;Version anglaise EN 15471:2017,Traduction anglaise de DIN EN 15471:2017-09SupersedesDIN EN 15471:200802www.beuth.deDocument comprises 12 pagesDTranslation by DIN-Sprach

4、endienst.In case of doubt, the German-language original shall be considered authoritative.09.17 DIN EN 15471:2017-09 2 A comma is used as the decimal marker. National foreword This document (EN 15471:2017) has been prepared by Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants and r

5、elated products of petroleum, synthetic and biological origin” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparation was DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-06-31 AA “Liquified gases: Requirements

6、 and testing”. Amendments This standard differs from DIN EN 15471:2008-02 as follows: a) numerous changes of both technical and editorial nature have been made to add clarity to the text; b) it has been clarified that the use of a drying agent in the desiccator is not recommended; c) the description

7、 of the equipment used has been improved; d) a note on the filter discs (6.3) used has been included; e) references to ASTM D 381 have been replaced by references to EN ISO 6246. Previous editions DIN EN 15471: 2008-02 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15471 July 2017 ICS 75.160.2

8、0 Supersedes EN 15471:2007English Version Liquefied petroleum gases - Determination of dissolved residues - High-temperature gravimetric method Gaz de ptrole liqufi - Dtermination des rsidus dissous - Mthode gravimtrique haute tempratureFlssiggas - Bestimmung der gelsten Rckstnde - Gravimetrisches H

9、ochtemperaturverfahren This European Standard was approved by CEN on 24 April 2017. 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 an

10、d bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre 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

11、responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugosla

12、v Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EU

13、ROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2017 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15471:2017 EEN 15471:2017 (E) 2 Contents Page European fore

14、word 3 1 Scope . 4 2 Normative references . 4 3 Terms and definitions 4 4 Principle 4 5 Reagents 4 6 Apparatus 5 7 Sampling 6 8 Procedure 6 8.1 Apparatus assembling 6 8.2 Evaporation of the LPG . 7 8.3 Jet evaporation procedure 7 9 Calculation 8 10 Expression of results . 8 11 Precision 8 11.1 Gener

15、al . 8 11.2 Repeatability, r 8 11.3 Reproducibility, R 8 Bibliography 10 DIN EN 15471:2017-09 EN 15471:2017 (E) 3 European foreword This document (EN 15471:2017) has been prepared by Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants and related products of petroleum, synthetic and

16、biological origin”, 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 January 2018, and conflicting national standards shall be withdrawn at the latest by Ja

17、nuary 2018. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 15471:2007. The changes of this second version compared to th

18、e previous version are as follows: a) numerous changes of both technical and editorial nature have been made to add clarity to the text; b) clarification that the use of a drying agent in the desiccator is not recommended; c) the description of the equipment used has been improved; d) a note to filt

19、er discs (6.3) was added; e) references to ASTM D381 have been replaced by references to EN ISO 6246. According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia,

20、 Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey a

21、nd the United Kingdom. DIN EN 15471:2017-09 EN 15471:2017 (E) 4 1 Scope This European Standard specifies a method for determining the dissolved residual matter in liquefied petroleum gases (LPG), which remains after evaporation at 105 C using the jet evaporation equipment described in EN ISO 6246. T

22、he measurement range is from 20 mg/kg to 100 mg/kg. Higher concentrations can be determined by adjusting the sample size. The precision data of the method have been determined from 20 mg/kg to 100 mg/kg, with samples amount from 100 g to 50 g. NOTE An alternative European Standard, EN 15470 1, speci

23、fies a gas chromatography method. WARNING The use of this standard can involve hazardous materials, operations and equipment. This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of users of this standard to take appropriate measures

24、to ensure the safety and health of personnel prior to application of the standard, and fulfil statutory and regulatory requirements for this purpose. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its applica

25、tion. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN ISO 4257, Liquefied petroleum gases - Method of sampling (ISO 4257) EN ISO 6246, Petroleum products - Gum content of fuels - Jet ev

26、aporation method (ISO 6246) 3 Terms and definitions For the purposes of this document, the following term and definition applies. 3.1 liquefied petroleum gas LPG petroleum gas that can be stored and/or handled in the liquid phase under moderate conditions of pressure and at ambient temperature, cons

27、isting predominantly of propane and butanes, with small proportions of propene, butenes and pentanes/pentenes 4 Principle A known mass of LPG is sampled and concentrated by evaporation. The concentrate is transferred into a beaker of 100 ml capacity and then evaporated by jet evaporation under contr

28、olled conditions of temperature and airflow. The oily residue remaining after this procedure is cooled and weighed. 5 Reagents 5.1 n-heptane, analytical grade. 5.2 propan-2-ol, technical grade, for the cooling bath. DIN EN 15471:2017-09 EN 15471:2017 (E) 5 5.3 Carbon dioxide, solid for the cooling b

29、ath. 5.4 Air, supply of filtered air at a pressure not more than 34,5 kPa. 5.5 Propan-2-one (acetone), analytical grade. 6 Apparatus 6.1 Sample cylinder, of a total mass compatible with the balance (6.10) used; preferably made of stainless steel fitted with two stainless steel valves free of oily ma

30、terials, conforming to EN ISO 4257. 6.2 In-line filter support, made of stainless steel and for use at suitable high pressure. 6.3 Filter discs, plain membrane with nominal pore dimension of 0,8 m. NOTE This method enables to quantify the total dissolved residual matter in LPG; the purpose of the fi

31、lter disc is to remove any particulate matter present in the LPG sample which would contribute to the total residual matter. 6.4 Cooling coil, made by coiling 4 m of stainless steel tube of external diameter 6 mm and internal diameter 4 mm onto a mandrel of a diameter of approximately 50 mm and fitt

32、ed with the necessary connections (see 3 in Figure 2). 6.5 Cooling bath, comprised of a 0,5l to 2l Dewar flask, filled with propan-2-ol (5.2) cooled by adding solid carbon dioxide (5.3), to achieve a temperature of approximately 77 C. 6.6 Beaker, made of glass, with a capacity of 1 l. 6.7 Boiling re

33、gulating rod, made of glass and a length of about 28 cm. 6.8 Beaker, made of glass and with a capacity 100 ml. 6.9 Balance for weighing the sample cylinder (6.1), capable of weighing to the nearest 1 g. 6.10 Analytical balance, capable of weighing to the nearest 0,1 mg. 6.11 Desiccator, (a drying ag

34、ent is not recommended). 6.12 Apparatus, for determining evaporation residues by air jet evaporation according to Figure 1 (for further information, see EN ISO 6246 ). 6.13 Oven, static type (without fan assisted circulation), explosion-proof, capable of heating to (105 5) C. DIN EN 15471:2017-09 EN

35、 15471:2017 (E) 6 Key 1 dry air supply 5 flow indicator 2 dry and clean steam supply 6 removable adaptor 3 thermometer and well (optional) 7 heating block 4 thermometer 8 thermo-regulator Figure 1 Apparatus for determining oily residues by jet evaporation 7 Sampling Samples shall be taken as describ

36、ed in EN ISO 4257 and/or in accordance with the requirements of national standards or regulations for the sampling of automotive LPG. 8 Procedure 8.1 Apparatus assembling Assemble the apparatus, as shown in Figure 2, and operate the following instructions: a) connect the lower valve of the sample cy

37、linder to the in-line filter (6.2); b) purge and fill the in-line filter and the cooling coil with the LPG to be analysed; c) close the lower valve of the sample cylinder; d) disconnect the in-line filter from the sample cylinder and weigh the cylinder to obtain its mass m1in grams; e) reconnect the

38、 sample cylinder to the purged in-line filter and cooling coil; f) position the 1 l beaker (6.6) and open the lower valve of the sample cylinder to obtain a steady flow of LPG sample into the beaker, until a mass of approximately 250 g is obtained (corresponding to approximately 500 ml); g) close th

39、e lower valve of the sample cylinder; h) disconnect the in-line filter from the sample cylinder and weigh the sample cylinder once more to obtain the post sample cylinder mass m2in grams. DIN EN 15471:2017-09 EN 15471:2017 (E) 7 Key 1 sample cylinder with two valves (6.1) 5 1 l beaker (6.6) 2 in-lin

40、e filter support (6.2) 6 boiling regulating rod (6.7) 3 stainless steel cooling coil (6.4) 7 earthing 4 Dewar flask filled as stipulated in 6.5 Figure 2 Apparatus assembling The test sample mass, ms, in grams, is determined by subtraction by the following formula: s= 12mmm (1) 8.2 Evaporation of the

41、 LPG Place the beaker with the sample (see 8.1) into an explosion-proof hood. Leave to evaporate until there is no visible volume of liquid left in the beaker. 8.3 Jet evaporation procedure The 100 ml beaker (6.8) is washed/rinsed with acetone (5.5) and distilled water and then dried at 105 C for 30

42、 min. When found necessary one may also immerse the beaker in a mildly detergent solution or, for a deeper cleaning action, use an oxidative acid cleaning solution. After a few hours soaking period, rinse the beaker with distillated water and dry. After cooling, this 100 ml beaker is placed in a des

43、iccator (6.11) for 30 min, and then weighed to the nearest 0,1 mg to obtain the mass m3. After evaporation of the sample, rinse the walls of the 1 l beaker (6.6) twice very carefully with approximately 20 ml n-heptane (5.1) each time and transfer the contents into the previously prepared 100 ml beak

44、er. Place the 100 ml beaker into the jet evaporation apparatus (6.12) as shown in Figure 1 and let the contents evaporate for a period of 30 min at 105 C with an air stream of 18 l/min to 24 l/min. Remove the beaker from the jet evaporation apparatus and place it in a desiccator for between 30 min a

45、nd 1 h. Finally, weigh the beaker to the nearest 0,1 mg to obtain the mass m4. The difference between this mass and the tare mass of the beaker gives the mass mrof the dissolved residue obtained during the test. DIN EN 15471:2017-09 EN 15471:2017 (E) 8 = r 43mmm (2) where mris the mass, in milligram

46、s, of residue obtained during the test; m3is the tare mass, in milligrams, of the 100 ml beaker; m4is the mass, in milligrams, of the 100 ml beaker plus residue. 9 Calculation Calculate the dissolved residue of the sample, ER, after evaporation, in milligrams per kilogram, using the following formul

47、a: = rs1000mERm(3) where mris the mass, in milligrams, of residue obtained during the test; msis the mass, in grams, of the LPG sample. 10 Expression of results Report the result to the nearest 1 mg/kg. 11 Precision 11.1 General The precision of this method, established during interlaboratory tests

48、relating to LPG samples with oily residue contents between 20 mg/kg and 100 mg/kg, and determined on the basis of statistical examination of interlaboratory test results 2, is as follows: 11.2 Repeatability, r The difference between two test results obtained by the same operator with the same appara

49、tus under constant operating conditions on nominally identical test material would, in the long run, in the normal and correct operation of the test method, exceed the value as given in Table 1 in only one case in 20 (see Table 2 for further details). 11.3 Reproducibility, R The difference between two single and independent results obtained by different operators working in different laboratories on nominally identical test material would, in t