1、BRITISH STANDARD BS EN ISO 6326-5:1998 BS 3156-11.4.5: 1994 Incorporating Amendment No. 1 to BS 3156-11.4.5:1994 (renumbers the BS as BS EN ISO 6326-5: 1998) Natural gas Determination of sulfur compounds Part 5: Lingener combustion method ICS 75.060BSENISO6326-5:1998 This British Standard, having be
2、en prepared under the direction of the Materials andChemicals Sector Board (I/-), was published under the authority of the Standards Board and comes into effect on 15 December 1994 BSI 06-1999 The following BSI references relate to the work on this standard: Committee reference PTI/15 Special announ
3、cement in BSINews, September 1994 ISBN 0 580 23615 3 Committees responsible for this British Standard The preparation of this British Standard was entrusted to Technical Committee PTI/15, Natural gas and gas analysis upon which the following bodies were represented: AEA Technology British Coal Corpo
4、ration British Compressed Gases Association British Gas plc British Glass Manufacturers Confederation Chemical Industries Association Department of Trade and Industry (Gas and Oil Measurement Branch) Department of Trade and Industry (National Physical Laboratory) Institute of Petroleum Institution o
5、f Gas Engineers Sira Limited Society of Chemical Industry Society of Glass Technology Amendments issued since publication Amd. No. Date Comments 9992 June 1998 New front cover and addition of European title page and foreword, and consequent changes to national foreword.BSENISO6326-5:1998 BSI 06-1999
6、 i Contents Page Committees responsible Inside front cover National foreword ii Foreword 2 Introduction 3 1 Scope 3 2 Normative references 3 3 Principle 3 4 Reagents and materials 3 5 Apparatus 3 6 Procedure 4 7 Analytical determination 9 8 Precision 11 9 Test report 12 Annex A (informative) Bibliog
7、raphy 13 Figure 1 Schematic layout of the apparatus 4 Figure 2 Combustion vessel 5 Figure 3 Receiver with cooling jacket 6 Figure 4 Flame tube 7 Figure 5 Burner 8 Figure 6 Intermediate piece 8 Figure 7 Reitmeyer attachment 9 Table 1 11 List of references Inside back coverBSENISO6326-5:1998 ii BSI 06
8、-1999 National foreword This British Standard has been prepared by Technical Committee PTI/15 and is the English language version of ENISO6326-5:1997 Natural gas Determination of sulfur compounds Part5: Lingener combustion method, published by the European Committee for Standardization (CEN). It is
9、identical with ISO6326-5:1989, published by the International Organization for Standardization (ISO). ISO6326-5 was prepared by Technical Committee158, Analysis of gases, in which the United Kingdom participated. BS EN ISO 6326-5 retains the secondary identifier BS3156-11.4.5, so that it remains cro
10、ss-referenced within the BS3156 series of standards. Each Subsection of Section11.4 of BS3156 is identical with the corresponding Part of ISO6326, and Section11.4 of BS3156 consists of the following Subsections: In the United Kingdom the preferred method is that given in Subsection11.4.4 of BS3156.
11、The flame photometric detector is available from most manufacturers of chromatographs, both laboratory and process units, and is applicable to any sulfur compound. By contrast, the electrochemical detector is available from a single supplier and is operated under completely different conditions, in
12、order to measure carbonyl sulfide to those used for all other sulfur compounds. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself c
13、onfer immunity from legal obligations. Subsection 11.4.1 Subsection 11.4.2 Subsection 11.4.3 (BS EN ISO 6326-3) Subsection 11.4.4 Subsection 11.4.5 (BS EN ISO 6326-5) Introduction Odoriferous sulfur compounds by gas chromatography using an electrochemical detector Hydrogen sulfide, mercaptan sulfur,
14、 and carbonyl sulfide sulfur by potentiometry Hydrogen sulfide, carbonyl sulfide and sulfur-containing odorants by gas chromatography using a flame photometric detector Lingener combustion method Cross-reference Publication referred to Corresponding British Standard ISO 1042:1983 BS 1792:1982 Specif
15、ication for one-mark volumetric flasks Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, theEN ISO title page, pages 2 to 14, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporat
16、ed. This will be indicated in the amendment table on the inside front cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 6326-5 December 1997 ICS 75.060 Descriptors: Natural gas, gas analysis, determination of content, sulfur, combustion analysis English version Natural gas Determination
17、 of sulfur compounds Part 5: Lingener combustion method (ISO 6326-5:1989) Gaz naturel Dtermination des composs soufrs Partie 5: Mthode de combustion Lingener (ISO 6326-5:1989) Erdgas Bestimmung von Schwefelverbindungen Teil 5: Verbrennung nach dem Lingener-Verfahren (ISO 6326-5:1989) This European S
18、tandard was approved by CEN on6November1997. 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
19、 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 langu
20、age and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Sw
21、itzerland and UnitedKingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1997 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members
22、Ref. No. EN ISO 6326-5:1997 EENISO6326-5:1997 BSI 06-1999 2 Foreword The text of the International Standard from Technical Committee ISO/TC193, Natural gas, of the International Organization for Standardization (ISO) has been taken over as a European Standard by CEN/CS. This European Standard shall
23、be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by June1998, and conflicting national standards shall be withdrawn at the latest by June1998. According to CEN/CENELEC Internal Regulations, the following countries are bound to im
24、plement this European Standard: Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the UnitedKingdom.ISO6326-5:1989(E) BSI 06-1999 3 Introduction The standardization of several
25、 methods for the determination of sulfur compounds in natural gas is necessary in view of the diversity of these compounds hydrogen sulfide, carbonyl sulfide, thiols (mercaptans), tetrahydrothiophene (THT), etc. and the purposes of the determinations (required accuracy, measurement at the drilling h
26、ead or in the transmission pipes, etc.). In order to enable the user to choose the method most appropriate to his needs and to perform the measurements under the best conditions, ISO6326 has been prepared in several parts. ISO 6326-1 gives a rapid comparison of standardized methods and therefore pro
27、vides information for the choice of the method. The other parts of ISO6326, including this part, describe in detail the various standardized methods. The determination of total sulfur is specified in ISO4260:1987, Petroleum products and hydrocarbons Determination of sulfur content Wickbold combustio
28、n method. 1 Scope This part of ISO 6326 specifies a method for the determination of total sulfur in natural gas. The method is applicable to gases with sulfur contents between0,5mg/m 3and1000 mg/m 3 . With a total sulfur content of more than0,1mg sulfur in the absorption solution, visual titration w
29、ith an indicator can be chosen, whereas for lower contents turbidimetric titration is preferable. NOTEIn all parts of ISO6326,1m 3of gas is expressed at normal conditions (0C;101,325kPa). 2 Normative references The following standards contain provisions which, through reference in this text, constit
30、ute provisions of this part of ISO6326. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this part of ISO6326 are encouraged to investigate the possibility of applying the most recent editions of the standards li
31、sted below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 385-1:1984, Laboratory glassware Burettes Part1: General requirements. ISO 648:1977, Laboratory glassware One-mark pipettes. ISO 1042:1983, Laboratory glassware One-mark volumetric flasks. ISO 3585:
32、1976, Glass plant, pipeline and fittings Properties of borosilicate glass3.3. 3 Principle A measured volume of gas is burnt with air at atmospheric pressure in a glass combustion apparatus. The resulting sulfur oxides are converted into sulfuric acid by absorption in hydrogen peroxide solution. Depe
33、nding on the sulfur content of the test gas, the sulfate ions in the absorption solution are determined using either visual titration with an indicator or turbidimetric titration. 4 Reagents and materials During the analysis, use only reagents of recognized analytical grade and only distilled water
34、or water of equivalent purity. 4.1 Hydrogen peroxide, 10% (m/m) aqueous solution, sulfur-free, as absorbing liquid for the sulfur oxides. 4.2 Activated carbon, for adsorption of sulfur impurities from the combustion air. 4.3 Absorbing liquid: 30% (m/m) aqueous solution of potassium hydroxide, for th
35、e purification of the combustion air. 5 Apparatus The schematic layout of the apparatus is shown in Figure 1. Ordinary laboratory apparatus and 5.1 Combustion device (A) The combustion device is manufactured of borosilicate glass complying with ISO3585. It consists of the parts shown inFigure 2. 5.1
36、.1 Receiver with cooling jacket (seeFigure 3). 5.1.2 Flame tube (see Figure 4) The outer diameter of the flame tube is determined by the inside diameter of the receiver with cooling jacket and the annular gap shown in Figure 2. 5.1.3 Burner (see Figure 5) For the combustion of natural gases a univer
37、sal burner with a needle valve is often preferable. 5.1.4 Intermediate piece (see Figure 6) The thermometer shall have a measuring range of0C to at least100C. The scale interval shall be not less than1C. 5.1.5 Reitmeyer attachment (see Figure 7). 5.2 Pressure-equalizing vessel (B).ISO6326-5:1989(E)
38、4 BSI 06-1999 5.3 Capillary flow meter (C), measuring range10l/min to30l/min. 5.4 U-tube manometer (D), arm length500mm. 5.5 Dry gas meter (E) The range of the meter shall be appropriate for the quantity of sample to be burned and the meter shall have been recently calibrated. The gas meter shall be
39、 equipped with a thermometer for the measurement of the gas temperature. The thermometer shall have a measuring range of0C to at least30C. The scale intervals shall be not less than0,5C. NOTEThe gas meter should be flushed with the gas to be analysed before the combustion, in particular when analysi
40、ng gases with different sulfur contents, to avoid disturbance by adsorption and desorption phenomena. 5.6 Condensate separator (F). 5.7 Vacuum pump (G) The suction capacity of the vacuum pump shall be at least25l/min. It is recommended that a drying tower with a drying agent be included between the
41、condensate separator (F) and the vacuum pump (G) to protect the oil in the vacuum pump. 6 Procedure 6.1 Preparation for combustion Draw air, which if necessary should be cleaned of sulfur impurities with activated carbon (4.2) and/or absorbing liquid (4.3), through the combustion apparatus with the
42、aid of the vacuum pump (G), with a required volumetric flow about20 l/min. Remove the burner (5.1.3) and pour sufficient hydrogen peroxide solution (4.1) into the receiver(5.1.1) to rise around the flame tube (5.1.2) to the height of the burner tip throughout the period of combustion. After connecti
43、on of the cooling water, the combustion apparatus is ready for use. Figure 1 Schematic layout of the apparatusISO6326-5:1989(E) BSI 06-1999 5 Figure 2 Combustion vesselISO6326-5:1989(E) 6 BSI 06-1999 Figure 3 Receiver with cooling jacketISO6326-5:1989(E) BSI 06-1999 7 Figure 4 Flame tubeISO6326-5:19
44、89(E) 8 BSI 06-1999 Figure 5 Burner Figure 6 Intermediate pieceISO6326-5:1989(E) BSI 06-1999 9 6.2 Combustion With a preliminary pressure of about2kPa on the U-tube manometer (D), ignite the gas at the removed burner. Carefully introduce the burner, with the flame directed downwards, into the flame
45、tube and note the reading on the gas meter (E). The air flow and cooling water flow may have to be adjusted. The temperature and pressure of the gas shall be read during the combustion period. The exhaust gas temperature on the thermometer shall be kept between50C and70C. As soon as the required qua
46、ntity of gas, up to500 litres depending on sulfur content (see clause7) has been burnt, shutoff first the gas supply and then the vacuum pump. Drain the absorbing solution into a beaker(7.1.2.5 or7.2.2.6), rinse the receiver with water and note the reading on the gas meter (E). 6.3 Determination of
47、gas volume The volume of gas burnt, shown by the difference in readings on the gas meter, shall be reduced to normal conditions: where V is the volume of the gas sample measured in accordance with6.2 at temperature T (kelvins) and pressure p amb + p e(kilopascals); T n is the thermodynamic temperatu
48、re, inkelvins, at normal ambient conditions(273,15K); T is the thermodynamic temperature, in kelvins, of the gas sample; p n is the pressure, in kilopascals, at normal conditions (101,325kPa); p amb is the atmospheric pressure, in kilopascals, measured during gas sampling; p e is the excess pressure
49、, in kilopascals, measured with the water manometer during gas sampling. 7 Analytical determination With a total sulfur content of more than0,1mg sulfur in the absorption solution, visual titration with an indicator can be chosen, whereas for lower contents turbidimetric titration is preferable. 7.1 Determination of sulfur content by visual titration 7.1.1 Reagents During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 7
