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1、Reference number ISO 6143:2001(E) ISO 2001 INTERNATIONAL STANDARD ISO 6143 Second edition 2001-05-01 Gas analysis Comparison methods for determining and checking the composition of calibration gas mixtures Analyse des gaz Mthodes comparatives pour la dtermination et la vrification de la composition
2、des mlanges de gaz pour talonnage Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/11/2007 20:55:44 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 6143:2001
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6、O 2001 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the
7、 country of the requester. ISO copyright office Case postale 56 ? CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.ch Web www.iso.ch Printed in Switzerland ii ISO 2001 All rights reserved Copyright International Organization for Standardization Provided by IHS under
8、 license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/11/2007 20:55:44 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 6143:2001(E) ISO 2001 All rights reservediii ContentsPage Foreword.iv Introduction.v 1Scope 1 2Terms and definitions .1 3
9、Symbols and abbreviated terms 3 4Principle4 5General procedure.6 6Special procedures14 7Test report14 Annex A (normative) Procedures for data evaluation.16 Annex B (informative) Examples .23 Annex C (informative) Computer implementation of recommended methods.31 Bibliography33 Copyright Internationa
10、l Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/11/2007 20:55:44 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 6143:2001(E) iv ISO 2001 All rights reserved Foreword ISO (the In
11、ternational Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee h
12、as been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical
13、 standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by
14、at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 6143 was
15、prepared by Technical Committee ISO/TC 158, Analysis of gases, to cancel and replace the first edition (ISO 6143:1981), of which the methods for the design and evaluation of calibrations of analytical systems have been updated and a method for estimating the uncertainty of the composition of calibra
16、tion gas mixtures has been added. It also cancels and replaces ISO 6711:1981, of which entirely new methods for checking the composition of calibration gases have been specified, thus replacing the method which is no longer in use. Annex A forms a normative part of ISO 6143. Annexes B and C are for
17、information only. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/11/2007 20:55:44 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 6143:2001(E) ISO 2001 All
18、 rights reservedv Introduction In gas analysis, calibration of analytical systems, as specified in the first edition of ISO 6143, has largely been confined to the determination of a straight line through the origin, or of a straight-line segment, using only the minimum number of calibration standard
19、s (one for a straight line through the origin, two for a line segment). The approach adopted in the revision, relating to calibration as well as to uncertainty evaluation, goes far beyond this simple scheme by ?including non-linear response curves and/or functions, ?replacing interpolation by regres
20、sion, ?taking into account the uncertainty on the calibration standards, ?including validation of calculated response curves and/or functions, ?calculating uncertainties by uncertainty propagation. As a consequence of adopting non-linear response models, advanced regression techniques (errors in bot
21、h variables) and uncertainty propagation, the main calculation procedures can only be performed on a computer, using a specific program. Such a program is available (see annex C). As an alternative, sufficient information is given in the document to enable the user to develop a program on his own. C
22、opyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/11/2007 20:55:44 MDTNo reproduction or networking permitted without license from IHS -,-,- Copyright International Organization for Standar
23、dization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/11/2007 20:55:44 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARDISO 6143:2001(E) ISO 2001 All rights reserved1 Gas analysis Comparison me
24、thods for determining and checking the composition of calibration gas mixtures 1Scope This International Standard provides methods for ?determining the composition of a calibration gas mixture by comparison with appropriate reference gas mixtures, ?calculating the uncertainty of the composition of a
25、 calibration gas mixture in relation to the known uncertainty of the composition of the reference gas mixtures with which it was compared, ?checking the composition attributed to a calibration gas mixture by comparison with appropriate reference gas mixtures, ?comparing the composition of several ca
26、libration gas mixtures, e.g. for the purpose of comparing different methods of gas mixture preparation, or for testing consistency among gas mixtures of closely related composition. NOTEIn principle, the method described in this document is also applicable to the analysis of (largely) unknown sample
27、s instead of prospective calibration gas mixtures (i.e. gas mixtures which are intended for use as calibration gas mixtures). Such applications, however, require appropriate care and consideration of additional uncertainty components, for example concerning the effect of matrix differences between t
28、he reference gases used for calibration and the analysed sample. 2Terms and definitions For the purposes of this International Standard, the following terms and definitions apply. 2.1 composition characteristic of a gas mixture given by the kind and content of each specified mixture component (analy
29、te) and the composition of the complementary gas (matrix) NOTEIn this International Standard, the analyte content is specified as a mole fraction, exclusively. Mole fractions have the advantage of being perfectly independent of the pressure and the temperature of the gas mixture. Therefore their use
30、 is recommended. However, for specific measuring systems, other composition measures (e.g. mass concentrations) may be more appropriate. Their use then requires due care concerning the dependence on pressure and temperature. 2.2 comparison method method for determining the content of a specified gas
31、 mixture component (analyte) by measuring an instrumental response NOTEComparison of measuring systems requires calibration, in which the relationship between response and analyte content is established. This is achieved by measuring the response to known values of analyte content provided by refere
32、nce gas mixtures. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/11/2007 20:55:44 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 6143:2001(E) 2 ISO 2001 A
33、ll rights reserved 2.3 calibration set of operations that establish, under specified conditions, the relationship between values of quantities indicated by a measuring instrument or measuring system, or values represented by a material measure or reference material, and the corresponding values real
34、ized by standards VIM 2.4 response function functional relationship between instrumental response and analyte content NOTE 1The response function can be expressed in two different ways as a calibration function or an analysis function, depending on the choice of the dependent and the independent var
35、iable. NOTE 2The response function is conceptual and cannot be determined exactly. It is determined approximately through calibration. 2.4.1 calibration function instrumental response expressed as a function of analyte content 2.4.2 analysis function analyte content expressed as a function of instru
36、mental response 2.5 uncertainty of measurement parameter, associated with the result of a measurement, that characterizes the dispersion of the values that can reasonably be attributed to the measurand GUM NOTEIn keeping with the GUM, in this International Standard the uncertainty of the composition
37、 of a gas mixture is expressed as a standard uncertainty, i.e. as a single standard deviation. 2.6 traceability property of the result of a measurement or the value attributed to a standard whereby it can be related to stated references, usually national or international standards, through an unbrok
38、en chain of comparisons all having stated uncertainties VIM 2.7 measurement standard material measure, measuring instrument, reference material, or measuring system, intended to define, realize, conserve, or reproduce a unit or one or more values of a quantity to serve as a reference VIM 2.8 referen
39、ce standard standard, generally having the highest metrological quality available at a given location or in a given organization, from which measurements made there are derived VIM Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical
40、 Standards 1/9972545001 Not for Resale, 04/11/2007 20:55:44 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 6143:2001(E) ISO 2001 All rights reserved3 2.9 working standard standard that is used routinely to calibrate or check material measures, measuring instruments or
41、reference materials VIM NOTEA working standard is usually calibrated against a reference standard. 2.10 reference material material or substance one or more of whose property values are sufficiently homogeneous and well established to be used for the calibration of an apparatus, the assessment of a
42、measuring method, or for assigning values to materials ISO Guide 30 2.11 calibration gas mixture gas mixture whose composition is sufficiently well established and stable to be used as a working standard of composition 2.12 reference gas mixture gas mixture whose composition is sufficiently well est
43、ablished and stable to be used as a reference standard of composition 3Symbols and abbreviated terms ajparameters of the calibration function F ( j = 0, 1, ., N) bjparameters of the analysis function G ( j = 0, 1, ., N) Dsensitivity matrix Fcalibration function, y = F(x), for the specified analyte G
44、analysis function, x = G(y), for the specified analyte kcoverage factor Llimit of detection Mcal(sample of) calibration gas mixture Mref(sample of) reference gas mixture Qtransform matrix Ssum of weighted squared deviations Sresresidual sum of weighted squared deviations tStudents t-factor U(q)expan
45、ded uncertainty of an estimated quantity q, U(q) = ku(q) Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/11/2007 20:55:44 MDTNo reproduction or networking permitted without license from
46、IHS -,-,- ISO 6143:2001(E) 4 ISO 2001 All rights reserved u(q)uncertainty of an estimated quantity q, expressed as a standard deviation (standard uncertainty) u(p,q)covariance of two estimated quantities p and q u2(q)variance of an estimated quantity q Vvariance/covariance matrix Whalf-width of a co
47、nfidence range xmole fraction of the specified analyte (xi, yi)calibration points (i = 1, 2, ., n) ? , ii xyadjusted calibration points (i = 1, 2, ., n) yinstrumental response of the specified analyte Znormal distribution percentage point ?relative analytical accuracy ?dilution factor ?measure of go
48、odness-of-fit 4Principle The composition of a gas mixture is determined by separate determination of the mole fraction of every specified analyte. Therefore the procedure for determining the mole fraction of only one specified analyte is described. Possible interferences of other components on the measurement of the analyte under consideration should be considered by the user and taken into account. However, this subject is not addresse