1、DD ISO/TS15338:2009ICS 71.040.40NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWDRAFT FOR DEVELOPMENTSurface chemicalanalysis Glowdischarge massspectrometry (GD-MS) Introduction to useThis Draft for Developmentwas published under theauthority of the StandardsPolicy and Strategy
2、Committee on 31 August2009 BSI 2009ISBN 978 0 580 54750 8Amendments/corrigenda issued since publicationDate CommentsDD ISO/TS 15338:2009National forewordThis Draft for Development is the UK implementation of ISO/TS15338:2009.This publication is not to be regarded as a British Standard.It is being is
3、sued in the Draft for Development series of publications andis of a provisional nature. It should be applied on this provisional basis,so that information and experience of its practical application can beobtained.Comments arising from the use of this Draft for Development arerequested so that UK ex
4、perience can be reported to the internationalorganization responsible for its conversion to an international standard.A review of this publication will be initiated not later than 3 years afterits publication by the international organization so that a decision can betaken on its status. Notificatio
5、n of the start of the review period will bemade in an announcement in the appropriate issue of Update Standards.According to the replies received by the end of the review period,the responsible BSI Committee will decide whether to support theconversion into an international Standard, to extend the l
6、ife of theTechnical Specification or to withdraw it. Comments should be sent tothe Secretary of the responsible BSI Technical Committee at BritishStandards House, 389 Chiswick High Road, London W4 4AL.The UK participation in its preparation was entrusted to TechnicalCommittee CII/60, Surface chemica
7、l analysis.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immun
8、ityfrom legal obligations.DD ISO/TS 15338:2009Reference numberISO/TS 15338:2009(E)ISO 2009TECHNICAL SPECIFICATION ISO/TS15338First edition2009-04-01Surface chemical analysis Glow discharge mass spectrometry (GD-MS) Introduction to use Analyse chimique des surfaces Spectromtrie de masse dcharge lumin
9、escente (GD-MS) Introduction lutilisation DD ISO/TS 15338:2009ISO/TS 15338:2009(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed
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14、ii ISO 2009 All rights reservedDD ISO/TS 15338:2009ISO/TS 15338:2009(E) ISO 2009 All rights reserved iiiContents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 Terms and definitions. 1 4 Safety . 2 4.1 Use of high-voltage power supply and connection of the instrument 2 4.2 Use and storage
15、 of compressed-gas cylinders. 2 4.3 Handling of cryogenic materials . 2 5 Principle. 2 6 Materials 2 7 Apparatus 3 7.1 Ion source 3 7.2 Mass analyser . 5 7.3 Detector system 8 7.4 Vacuum system. 9 7.5 Data acquisition and control . 9 8 Samples and sample preparation . 9 8.1 General. 9 8.2 Sample typ
16、e. 10 8.3 Sample geometry 10 8.4 Sample preparation for bulk analysis. 10 8.5 Sample preparation for depth profiling 11 9 Measurement procedures 11 9.1 System precautions 11 9.2 Selection of discharge parameters and isotopes 12 9.3 Presputtering. 12 9.4 Optimizing the ion current . 12 9.5 Analytical
17、 set-up . 13 9.6 Data analysis . 13 9.7 Depth profile analysis. 14 9.8 Instrument performance 14 9.9 Analysis . 14 10 Test report . 23 Bibliography . 26 DD ISO/TS 15338:2009ISO/TS 15338:2009(E) iv ISO 2009 All rights reservedForeword ISO (the International Organization for Standardization) is a worl
18、dwide 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 has been established has the right to be represented on
19、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 standardization. International Standards are drafted i
20、n accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard
21、 requires approval by at least 75 % of the member bodies casting a vote. In other circumstances, particularly when there is an urgent market requirement for such documents, a technical committee may decide to publish other types of document: an ISO Publicly Available Specification (ISO/PAS) represen
22、ts an agreement between technical experts in an ISO working group and is accepted for publication if it is approved by more than 50 % of the members of the parent committee casting a vote; an ISO Technical Specification (ISO/TS) represents an agreement between the members of a technical committee an
23、d is accepted for publication if it is approved by 2/3 of the members of the committee casting a vote. An ISO/PAS or ISO/TS is reviewed after three years in order to decide whether it will be confirmed for a further three years, revised to become an International Standard, or withdrawn. If the ISO/P
24、AS or ISO/TS is confirmed, it is reviewed again after a further three years, at which time it must either be transformed into an International Standard or be withdrawn. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not
25、 be held responsible for identifying any or all such patent rights. ISO/TS 15338 was prepared by Technical Committee ISO/TC 201, Surface chemical analysis, Subcommittee SC 8, Glow discharge spectrometry, based on Australian Standard AS 3685:1998. DD ISO/TS 15338:2009TECHNICAL SPECIFICATION ISO/TS 15
26、338:2009(E) ISO 2009 All rights reserved 1Surface chemical analysis Glow discharge mass spectrometry (GD-MS) Introduction to use 1 Scope This Technical Specification gives guidelines for the operation of glow discharge mass spectrometry (GD-MS) instruments and recommendations for the use of GD-MS. I
27、t is intended to be read in conjunction with the instrument manufacturers manuals and recommendations. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the l
28、atest edition of the referenced document (including any amendments) applies. ISO 18115, Surface chemical analysis Vocabulary 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 18115 and the following apply. 3.1 accuracy of measurement closeness of the a
29、greement between a result and the accepted reference value 3.2 elemental intensity amount of ion current recorded for a particular element 3.3 pin cell sample cell used for the analysis of wire and rod samples 3.4 precision of measurements closeness of the agreement between independent test results
30、obtained under stipulated conditions, normally reported as a standard deviation 3.5 pin, rod and wire samples samples with cylindrical or square cross-section of nominal length typically 20 mm and not normally exceeding 10 mm across 3.6 transmission ratio of the number of ions reaching the detector
31、relative to the number of ions entering the mass analyser DD ISO/TS 15338:2009ISO/TS 15338:2009(E) 2 ISO 2009 All rights reserved4 Safety 4.1 Use of high-voltage power supply and connection of the instrument Electrical connection should comply with the regulations in force. Particular care should be
32、 taken to ensure that connection of the instrument to ground is correct, and the efficiency of the ground connection should be checked. 4.2 Use and storage of compressed-gas cylinders The compressed-gas cylinders should be regularly tested by the appropriate authorities. Cylinders should not be stor
33、ed or used inside the laboratory. Rather, they should be located outside the laboratory in a place that is well ventilated, away from direct heat, and accessible to service and safety personnel. The cylinders should be provided with suitable pressure-reducing valves. If more than one cylinder is to
34、be used or stored in close proximity, it is advisable to indicate in some way which cylinder or cylinders are currently in use. 4.3 Handling of cryogenic materials Vessels containing cryogenic materials should be located so as to minimize the risk to personnel. Areas where cryogenic liquids are stor
35、ed and used should be ventilated to prevent the accumulation of gas or vapour which could evaporate from the liquid. It is good practice to keep areas where cryogenic liquids are used very clean. All transfer operations should be in accordance with statutory requirements. When a cryogenic liquid is
36、being transferred from one vessel to another, precautions should be taken to minimize any spills and splashing. The requirements of the relevant regulatory authorities should also be met. 5 Principle In a glow discharge source, electrical power is supplied between the sample (cathode) and the anode
37、by a power supply typically operated in direct current (dc) at 0,5 kV to 2 kV and 1 mA to 300 mA. Argon (or another inert gas such as neon, krypton or helium) is introduced into the discharge cell. The pressure inside the discharge cell is typically a few hundred pascals (Pa). A potential difference
38、 is applied between the cathode and the anode and a glow discharge (plasma) is established. Sample material (single atoms and/or clusters) which is sputtered by ions and neutrals diffuses into the plasma. Ions formed in the glow discharge are extracted from the ion source and pass into a mass analys
39、er. The mass analyser is used to transmit ions of given mass-to-charge ratio to the detector(s). The ions reaching the detector(s) are measured as ion current or counted by a counting system. This information is stored in a computer system. Elemental mass fractions are typically calculated by the in
40、strument software using the ion currents of isotopes, by normalizing the signal to the signal of a matrix element and subsequently comparing the normalized signals with those arising from the corresponding elements in calibration samples. 6 Materials 6.1 Deionized water, 18 Mcm or better. 6.2 Argon
41、gas, or other plasma support gases, of purity better than 99,999 9 % or in accordance with the recommendations of the instrument manufacturer. 6.3 Liquid nitrogen, for cryogenic cooling of the discharge cell. 6.4 Compressed gas, to operate pneumatic valves. DD ISO/TS 15338:2009ISO/TS 15338:2009(E) I
42、SO 2009 All rights reserved 37 Apparatus 7.1 Ion source 7.1.1 General A glow discharge ion source consists of a glow discharge cell and a power supply. In some designs, the ion source will also contain a series of focusing plates, external to the cell, whose function is to extract ions from the cell
43、 and focus these ions into the mass spectrometer. Typically the body of the discharge cell is connected to the anode output of the power supply. The sample serves in the glow discharge cell as a cathode and is connected to the cathode output of the power supply. Discharge cells have been designed to
44、 accommodate samples in the geometries recommended in 8.3, and examples of discharge cells are illustrated with the appropriate sample holders in Figures 1 and 2. Key 1 sample holder 2 sample 3 insulator 4 ion exit slit 5 anode plate 6 cathode plate Figure 1 Example of a cell used for the analysis o
45、f pin samples DD ISO/TS 15338:2009ISO/TS 15338:2009(E) 4 ISO 2009 All rights reservedKey 1 sample cathode 2 spring 3 insulator 4 cell body 5 ion exit slit 6 anode plate Figure 2 Example of a cell used for the analysis of flat samples 7.1.2 Source parameters The source parameters are as follows: a) E
46、lectrical potential difference between anode and cathode; current; power. b) Geometrical dimension of sample exposed to plasma; anode-to-sample distance; cathode dimension; mask dimension, where appropriate. DD ISO/TS 15338:2009ISO/TS 15338:2009(E) ISO 2009 All rights reserved 5c) Gas type and press
47、ure. d) Cell temperature. e) Type of sample. 7.1.3 Operational modes The direct-current source may be operated in different modes, including: a) constant current with potential difference adjusted by adjusting the plasma gas pressure; b) constant potential difference with current adjusted by adjusti
48、ng the plasma gas pressure; c) constant current with plasma gas pressure adjusted by adjusting the potential difference. The discharge pressure may be regulated using a mass flow controller, needle valve or knife edge valve. For some types of GD-MS instrument, the high accelerating voltages encounte
49、red require a capillary in the gas line to prevent electrical breakdown through the gas line. Radio-frequency-powered GD sources are also being developed for GD-MS. 7.2 Mass analyser There are two types of mass analyser commonly used for glow discharge mass spectrometry: double-focussing magnetic-sector instruments and quadrupole instruments. Other types, like time-of-flight instruments, are also becoming more common. a) Sector mass spectrometer: This type of instrument (see Figure 3) typically utilizes a
