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1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS ISO 14707:2000 ICS 71.
2、040.50 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Surface chemical analysis Glow discharge optical emission spectrometry (GD-OES) Introduction to use Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI This British St
3、andard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 November 2000 BSI 11-2000 ISBN 0 580 36667 7 BS ISO 14707:2000 Amendments issued since publication Amd. No.Da
4、teComments National foreword This British Standard reproduces verbatim ISO 14707:2000 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee CII/60, Surface chemical analysis, which has the responsibility to: aid enquirers to under
5、stand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on
6、this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled International Standards Correspondence Index,
7、or by using the Find facility of the BSI Standards Electronic Catalogue. 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 confer i
8、mmunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to v, a blank page, pages 1 to 8, an inside back cover and a back cover. The BSI copyright notice displayed this document indicates when the document was last i
9、ssued. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTERNATIONAL STANDARD ISO 14707 First edition 2000-08-15 Reference number ISO 14707:2000(E) Surface chemical analysis Glow discharge optical emission spectrometry (GD-OES) Introduction
10、to use Analyse chimique des surfaces Spectromtrie dmission optique dcharge luminescente Introduction son emploi Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 14707:2000(E) ii? Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:1
11、1:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 14707:2000(E) ?iii Contents?Page 1? Scope .?1 2? Normative references .?1 3? Terms and definitions ?1 4?Principle .?2 5?Apparatus ?2 6?Procedure ?4 Annex A? Safety?8 A.1General .?8 A.2Use of a high-voltage power supply and grounding of the instrume
12、nt ?8 A.3Use of radio frequencies .?8 A.4Use and storage of compressed-gas cylinders .?8 A.5Safety checks before and during operation .?8 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 14707:2000(E) iv? Foreword ISO (the International O
13、rganization 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 com- mittees. Each member body interested in a subject for which a technical committee has been est
14、ablished has the right to be represented on that committee. International organizations, governmental and non-governmental, in liai- son with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standard
15、ization. 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 at least
16、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 14707 was prepared
17、 by Technical Committee ISO/TC 201,Surface chemical analysis, Subcommittee SC 8,Glow discharge spectroscopy. Annex A of this International Standard is for information only. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 14707:2000(E) ?v
18、 Introduction Glow discharge optical emission spectrometry (GD-OES) is used to determine the elemental composition of solid samples. GD-OES may be used for either bulk or depth profile analysis. In bulk analysis, changes in elemental com- position with depth into the specimen are assumed to be negli
19、gible. In contrast, the main goal of depth profile analy- sis is usually to gain information concerning such changes of composition. Layer thicknesses amenable to GD-OES depth profiling range from a few nanometres to approximately one hundred micrometres. As is true for any instrumental analysis met
20、hod, the quality of a GD-OES analysis depends markedly on the correct optimization and operation of the instrumentation. This document provides guidelines of practice that should be fol- lowed to ensure that GD-OES analyses are of the highest possible quality. Licensed Copy: sheffieldun sheffieldun,
21、 na, Mon Nov 27 04:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTERNATIONAL STANDARD?ISO 14707:2000(E) ?1 Surface chemical analysis Glow discharge optical emission spectrometry (GD-OES) I
22、ntroduction to use 1Scope This International Standard provides guidelines that are applicable to bulk and depth profiling GD-OES analyses. The guidelines discussed herein are limited to the analysis of rigid solids, and do not cover the analysis of powders, gases or solutions. Combined with specific
23、 standard methods which will become available in the future, these guide- lines should enable the regulation of instruments and the control of measuring conditions. Although several types of glow discharge optical emission source have been developed over the years, the guide- lines contained in this
24、 document use the Grimm type as an example. This is because the Grimm type device ac- counts for a very large majority of glow discharge optical emission devices currently in use. It should be clearly understood that the guidelines contained herein are equally applicable to other source designs, suc
25、h as the Marcus type, and that the Grimm type device is used only as an example. 2Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or
26、revisions of, any of these publica- tions do not apply. However, parties to agreements based on this International Standard are encouraged to investi- gate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of t
27、he normative document referred to applies. Members of ISO and IEC maintain reg- isters of currently valid International Standards. ISO 3497:1990,Metallic coatings Measurement of coating thickness X-ray spectrometric methods. ISO 5725-1:1994,Accuracy (trueness and precision) of measurement methods an
28、d results Part 1: General prin- ciples and definitions. ISO 5725-2:1994,Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method. ISO 5725-3:1994,Accuracy (trueness and precis
29、ion) of measurement methods and results Part 3: Intermediate measures of the precision of a standard measurement method. ISO 5725-4:1994,Accuracy (trueness and precision) of measurement methods and results Part 4: Basic methods for the determination of the trueness of a standard measurement method.
30、ISO 6955:1982,Analyticalspectroscopicmethods Flameemission,atomicabsorption,andatomic fluorescence Vocabulary. 3Terms and definitions For the purposes of this International Standard, the terms and definitions given in ISO 3497, ISO 5725-1, ISO 5725-2, ISO 5725-3, ISO 5725-4 and ISO 6955 apply. Licen
31、sed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 14707:2000(E) 2? 4Principle Analysis by GD-OES involves the following operations: a)preparation of the sample to be analysed, generally in the form of a flat plate or disc of dimensions appropri
32、ate to the instrument or analytical requirement (round or rectangular samples with a width of?to?are suit- able); b)atomization and excitation of the analytes to be determined by means of ion sputtering and energy transfer pro- cesses occurring in the glow discharge; c)measurement of the emission in
33、tensities of characteristic spectral lines of the analytes (for depth profiling, emis- sion intensities are recorded as a function of time); d)determination of the analyte concentrations contained in the sample by calibration with reference samples of known composition (for depth profiling, the sput
34、tered depth as a function of time is also determined by calibration with reference samples of known composition and sputtering rates). A diagram of a typical GD-OES system is presented in Figure 1. GD-OES is based on the use of a glow discharge device as an optical emission source. The glow discharg
35、e device consists of a vacuum chamber filled with an inert gas, usually argon. The glowing plasma, from which the discharge takes its name, is maintained by a controlled high voltage of?to?applied between the anode and cathode in the inert gas. The solid sample to be analysed serves as the cathode.
36、Atomization of sample material in the glow discharge is the result of ion sputtering. Inert gas ions formed in the plasma are accelerated toward the cathode surface by the electric field in the plasma. When an ion collides with the surface, its kinetic energy may be transferred to atoms on the surfa
37、ce, causing some of these surface atoms to be ejected into the plasma. Once in the plasma, these sputtered sample atoms may be excited through inelastic colli- sions with electrons or other species. The majority of these excited analyte atoms then emit characteristic optical emission upon relaxing i
38、nto the lower electronic state. This optical emission is translated into an analytical signal by means of appropriate optical and electric components. A polychromator is commonly employed, so that many ele- ments may be quantified simultaneously. Spectral lines that are not contained in the line set
39、 of the polychromator can be accessed by means of a scanning monochromator, if one is available. In practice almost all elements in the peri- odic table can be determined, including metals, metalloids and non-metals. 5?Apparatus At a minimum, the apparatus consists of the following: 5.1Glow discharg
40、e optical emission source A diagram of a Grimm type glow discharge optical emission device is shown in Figure 2. Several modifications in the device have been introduced by instrument manufacturers, but the basic principle is not different from that shown in Figure 2. As noted in clause 4, the sampl
41、e effectively serves as the cathode. The anode takes the form of a tube with an inner diameter of typically?to?. The distance between the front face of the anode and the surface of the cathode is usually between?and?. As a result, ion sputtering is confined to a circular region of the sample surface
42、 with a diameter approximately equal to the inner diameter of the anode. The glow discharge device requires several peripheral pieces of equipment for its operation. These include an elec- tric power supply, one or two vacuum pumps, a source of inert gas, a means of delivering that gas into the devi
43、ce in a controlled manner and a vacuum gauge. A cooling device, such as a metal block with circulating cooling liquid, is sometimes necessary for thin samples. a)Source parameters Glow discharge devices may be operated in either direct current (dc) or radio-frequency (rf) mode. Combinations of these
44、 two modes, such as the use of an rf voltage superposed onto a dc voltage, have also been reported. 1)For dc operation, the pertinent electrical parameters are discharge current (?to?) and voltage (?to?). In addition to the electrical parameters, other parameters are important for the character- 10
45、mm 100 mm 500 V 1 000 V 2,5 mm 8 mm 0,1 mm 0,3 mm 5 mA 200 mA 400 V 2 000 V Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 04:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 14707:2000(E) ?3 istics of the device. These include the inner diameter of the anode (?to?), gas type and purity
46、(for example, argon,?), gas flow rate (?to?, see note below) and physical characteris- tics of the sample material (for example, secondary electron emission yield and sputtering yield). The com- bined effects of all of these factors determine the spectrochemical character of the glow discharge. Gene
47、rally, it is recommended that the gas flow rate be varied in real time, in order to achieve constant voltage and cur- rent. As an example, typical operating conditions for dc GD-OES bulk analysis of low-alloy steels are argon flow rate,?to?discharge voltage and?to?discharge current, for an anode of?
48、inner diameter. NOTEIt should be understood that the discharge gas flow rate is the practical means of controlling the source operating pressure, and so suggested ranges are very much source specific, and are provided here only with reference to the Grimm lamp example. 2)Typical conditions for rf gl
49、ow discharge include the same range of argon flow rate and similar discharge power and voltage as in dc operation. In terms of the electrical parameters, it is important to note that GD-OES instruments usually measure either the incident power or the applied RMS voltage. In the former case, it must be understood that the incident power is the power delivered to the glow discharge system by Key 1Spectrometer 2?Vacuum chamber for UV spectra 3?Electrical lead-in 4?Preamplifier 5?Light intensity meas- uring circuit 6?Vacuum control sys- tem 7?Phot
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