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1、BRITISH STANDARD Gas analysis Preparation of calibration gas mixtures using dynamic volumetric methods Part 10: Permeation method ICS 71.040.40 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW 6145-10:2008 BS EN ISO Licensed CopyChinese University of Hong Kong, 11/04/2009 08:27
2、, Uncontrolled Copy, (c) BSI BS EN ISO 6145-10:2008 National foreword This British Standard is the UK implementation of EN ISO 6145-10:2008. It is is withdrawn. The UK participation in its preparation was entrusted to Technical Committee PTI/15, Natural gas and gas analysis. A list of organizations
3、represented on this committee can be obtained on request to its secretary. 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 cannot confer immunity from legal obligations. ISB
4、N 978 0 580 60362 4 Amendments/corrigenda issued since publication DateComments 28 February 2009 This corrigendum renumbers BS ISO 6145-10:2002 as BS EN ISO 6145-10:2008 identical with ISO 6145-10:2002. It supersedes BS ISO 6145-10:2002 which BSI 2009 This British Standard was published under the au
5、thority of the Standards Policy and Strategy Committee on 25 March 2002 Licensed CopyChinese University of Hong Kong, 11/04/2009 08:27, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 6145-10 August 2008 ICS 71.040.40 English Version Gas analysis - Preparation of
6、calibration gas mixtures using dynamic volumetric methods - Part 10: Permeation method (ISO 6145-10:2002) Analyse des gaz - Prparation des mlanges de gaz pour talonnage laide de mthodes volumtriques dynamiques - Partie 10: Mthode par permation (ISO 6145-10:2002) Gasanalyse - Herstellung von Kalibrie
7、rgasgemischen mit Hilfe von dynamisch-volumetrischen Verfahren - Teil 10: Permeationsverfahren (ISO 6145-10:2002) This European Standard was approved by CEN on 30 July 2008. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this Europ
8、ean 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 the CEN Management Centre or to any CEN member. This European Standard exists in three official versions (Englis
9、h, 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 CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria,
10、Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATIO
11、N COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2008 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 6145-10:2008: E Licensed CopyChinese University of Hong
12、Kong, 11/04/2009 08:27, Uncontrolled Copy, (c) BSI Foreword The text of ISO 6145-10:2002 has been prepared by Technical Committee ISO/TC 158 “Analysis of gases” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 6145-10:2008 by Technical Committee CEN/SS N2
13、1 “Gaseous fuels and combustible gas” the secretariat of which is held by CMC. 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 February 2009, and conflicting national standards shall be withdrawn
14、at the latest by February 2009. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the
15、 national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Nor
16、way, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 6145-10:2002 has been approved by CEN as a EN ISO 6145-10:2008 without any modification. BS EN ISO 6145-10:2008 Licensed CopyChinese University of Hong Kong, 11/0
17、4/2009 08:27, Uncontrolled Copy, (c) BSI iii Contents Page Introduction.v 1 Scope1 2 Normative reference1 3 Principle1 4 Reagents and materials 2 5 Apparatus.2 6 Procedure.5 6.1 Preliminary checks and operating conditions5 6.2 Determination of mass loss6 7 Expression of results7 7.1 Calculation .7 7
18、.2 Sources of uncertainty8 7.3 Estimation of uncertainties.10 7.4 Example calculation of uncertainties13 Annex A (informative) Example of uncertainty calculation for a two-pan continuous weighing system14 Bibliography16 BS EN ISO 6145-10:2008 Licensed CopyChinese University of Hong Kong, 11/04/2009
19、08:27, Uncontrolled Copy, (c) BSI blank Licensed CopyChinese University of Hong Kong, 11/04/2009 08:27, Uncontrolled Copy, (c) BSI v Introduction This part of ISO 6145 is one of a series of standards dealing with various dynamic volumetric methods used for the preparation of calibration gas mixtures
20、. I BS EN ISO 6145-10:2008 Licensed CopyChinese University of Hong Kong, 11/04/2009 08:27, Uncontrolled Copy, (c) BSI Licensed CopyChinese University of Hong Kong, 11/04/2009 08:27, Uncontrolled Copy, (c) BSI 1 Gas analysis Preparation of calibration gas mixtures using dynamic volumetric methods Par
21、t 10: Permeation method 1 Scope This part of ISO 6145 specifies a dynamic method using permeation membranes for the preparation of calibration gas mixtures containing component mole fractions ranging from 109 and 106. A relative expanded uncertainty of 2,5 % of the component mole fraction can be ach
22、ieved using this method. In the mole fraction range considered, it is difficult to maintain some gas mixtures, for example in cylinders, in a stable state. It is therefore desirable to prepare the calibration gas immediately before use, and to transfer it by the shortest possible path to the place w
23、here it is to be used. This technique has been successfully applied in generating low content calibration gas mixtures of, for example, sulfur dioxide (SO2), nitrogen dioxide (NO2) and benzene (C6H6) in air. If the carrier gas flow is measured as a gas mass-flow, the preparation of calibration gas m
24、ixtures using permeation tubes is a dynamic-gravimetric method which gives contents in mole fractions. 2 Normative reference The following normative document contains provisions which, through reference in this text, constitute provisions of this part of ISO 6145. For dated references, subsequent am
25、endments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this part of ISO 6145 are encouraged to investigate the possibility of applying the most recent edition of the normative document indicated below. For undated references, the latest edition
26、of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 6145-1, Gas analysis Preparation of calibration gas mixtures using dynamic volumetric methods Part 1: Methods of calibration 3 Principle The calibration component
27、for example SO2, NO2, ammonia (NH3), benzene, toluene, xylene is permeated through an appropriate membrane into the flow of a carrier gas, i.e. the complementary gas of the mixture obtained. The calibration component, of known purity, is contained in a tube, which is itself contained in a temperatur
28、e- controlled vessel. This vessel is purged at a known and controlled flow rate by the carrier gas. The composition of the mixture is determined from the permeation rate of the calibration component as well as the flow rate of the high quality carrier gas, free from any trace of the calibration comp
29、onent and from any chemical interaction with the material of the permeation tube. The permeation rate of the calibration component through the membrane depends upon the component itself, the chemical nature and structure of the membrane, its area and thickness, the temperature, and the partial press
30、ure gradient of the calibration component across the membrane. These factors can be kept constant by proper operation of the system. The permeation rate can be measured directly by mounting the tube on a microbalance and weighing the tube either continuously or periodically. BS EN ISO 6145-10:2008 L
31、icensed CopyChinese University of Hong Kong, 11/04/2009 08:27, Uncontrolled Copy, (c) BSI 2 4 Reagents and materials 4.1 Permeating substances for calibration, of the highest possible purity so as to avoid any effect of impurities on the permeation rate; if this is not possible, the nature and quant
32、ities of the impurities shall be known and allowance made for their effect. 4.2 Carrier gas, of known purity, established by an appropriate analytical technique, for example, gas chromatography (GC) and/or Fourier transform infrared (FTIR) spectrometry. 5 Apparatus 5.1 Permeation apparatus, typicall
33、y consisting of one of two modes (5.1.1 and 5.1.2) of application of the permeation method. The materials of the permeation apparatus shall be chosen so as to avoid any effect on the content of the calibration component by sorption (chemical or physical). The smaller the desired final content, the g
34、reater the effect of adsorption phenomena. If possible, use glass as the housing of the temperature-controlled permeation tube. Choose flexible and chemically inert tube materials and metals, especially having regard to the transfer of the gas between the permeation apparatus and the analyser. Pay s
35、pecial attention to all junctions so as to keep them free from leaks. The flow range of the carrier gas is kept constant by a control system and is monitored by a flowmeter. The value of the flow rate can, for example, be controlled by means of a mass flow controller and determined using a mass flow
36、meter. The existence of an outlet for surplus gas enables the analyser under calibration to take the gas flow rate necessary for its proper operation, the remainder of the flow of gas being vented to atmosphere. 5.1.1 Periodic-weighing-mode permeation apparatus, consisting of a permeation tube kept
37、in a temperature- controlled enclosure, swept by carrier gas. The permeation tube is periodically removed from the enclosure to be weighed. Typical examples are given in Figures 1 and 2. 5.1.2 Continuous-weighing-mode permeation apparatus, consisting of a permeation tube kept in a temperature-contro
38、lled enclosure, swept by carrier gas. The permeation tube is suspended from a weighing device and weighed continuously. A typical example is given in Figure 3. BS EN ISO 6145-10:2008 Licensed CopyChinese University of Hong Kong, 11/04/2009 08:27, Uncontrolled Copy, (c) BSI 3 Key 1 Flowmeter 5 Thermo
39、meter 2 Carrier gas 6 Permeation tube 3 Drier 7 Outlet for surplus gas 4 Filter 8 Analyser Figure 1 Example 1 of a periodic-weighing-mode permeation apparatus Key 1 Outlet for surplus gas 2 Sampling system 3 Mixing bulb 4 Flowmeter 2 5 Diluent gas 6 Thermometer 7 Permeation tube 8 Copper tubing 9 Wa
40、ter bath 10 Flowmeter 1 11 Carrier gas 12 Drier Figure 2 Example 2 of a periodic-weighing-mode permeation apparatus BS EN ISO 6145-10:2008 Licensed CopyChinese University of Hong Kong, 11/04/2009 08:27, Uncontrolled Copy, (c) BSI 4 Permeation tube Mass flow controller Tare mass Key 1 High purity air
41、/N2 2 Temperature controller 3 Water 4 Microbalance controller 5 Gas blender 6 RS232 link 7 PC (acquisition, analysis and diagnostics) 8 16-bit ADC 9 Flow rate calibration facility 10 Gas analyser 11 Stable mixture requiring certification Figure 3 Continuous-weighing-mode permeation apparatus BS EN
42、ISO 6145-10:2008 Licensed CopyChinese University of Hong Kong, 11/04/2009 08:27, Uncontrolled Copy, (c) BSI 5 5.2 Permeation membrane, made from polymers and having sufficient chemical and mechanical resistance, e.g. suitable polytetrafluoroethylene (PTFE), polyethylene, polypropylene or a copolymer
43、 of tetrafluoroethylene and hexafluoropropylene (FEP). Take into account variations of the material characteristics which occur with a change of temperature. 5.3 Permeation tubes, or containers, made of stainless steel or glass, fitted with a permeation membrane (5.2) and capable of holding the cali
44、bration component in the liquid phase and gaseous phase; the membrane through which the permeation takes place may be in contact with the liquid phase only, or with the gaseous phase only, or with both. See examples given in Figure 4. Before use, keep the permeation tube in an airtight container und
45、er an anhydrous atmosphere in a cold place (e.g. in a refrigerator at approximately 5 C) so as to maintain the diffusion rate as low as possible, hence to minimize loss of the calibration component and avoid any condensation on the tube. a) Cylindrical tube fitted with a membrane in contact with bot
46、h phases b) Tube fitted with a membrane in contact with only the liquid phase c) Container fitted with a membrane in contact with only the gaseous phase Key 1 Membrane 2 Stainless steel 3 Liquid level 4 Glass Figure 4 Examples of permeation tubes and container 6 Procedure 6.1 Preliminary checks and
47、operating conditions 6.1.1 Permeation tube Before use, assess the purity of the product of the permeation tube by collecting a sample of the permeated gas for analysis by an appropriate analytical technique e.g. GC or FTIR so as to quantify any likely major contaminants. This information may be prov
48、ided by the suppliers of the tube and, if so, a certificate of analysis by an accredited body shall be provided. Periodically check the permeation rate of the tube at a known, fixed temperature by measuring the mass loss. This gives a good indication as to the purity of the permeated gas. If the per
49、meation rate changes by more than 10 % at the known, fixed temperature, discard the permeation tube. When first using the permeation tube, allow the system to reach a state of equilibrium before carrying out the first weighing so as to ensure that the permeation rate is well stabilized at the constant value. The time needed to reach BS EN ISO 6145-10:2008 Licensed CopyChinese University of Hong Kong, 11/04/2009 08:27, Uncontrolled Copy, (c) BSI 6 equilibrium is dependant on the component contained within the permeation tube, but a value of 72