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1、DRAFT FOR DEVELOPMENT DD ISO/TS 13899-3:2005 Steel Determination of Mo, Nb and W contents in alloyed steel Inductively coupled plasma atomic emission spectrometric method Part 3: Determination of W content ICS 77.080.20 ? Licensed Copy: London South Bank University, London South Bank University, Sat
2、 Dec 30 06:30:47 GMT+00:00 2006, Uncontrolled Copy, (c) BSI DD ISO/TS 13899-3:2005 This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 29 December 2006 BSI 2006 ISBN 0 580 49855 7 National foreword This Draft for Development was published by
3、 BSI. It is the UK implementation of ISO/TS 13899-3:2005. This publication is not to be regarded as a British Standard. It is being issued in the Draft for Development series of publications and is of a provisional nature. It should be applied on this provisional basis, so that information and exper
4、ience of its practical application can be obtained. Comments arising from the use of this Draft for Development are requested so that UK experience can be reported to the international organization responsible for its conversion to an international standard. A review of this publication will be init
5、iated not later than 3 years after its publication by the international organization so that a decision can be taken on its status. Notification of the start of the review period will be made in an announcement in the appropriate issue of Update Standards. According to the replies received by the en
6、d of the review period, the responsible BSI Committee will decide whether to support the conversion into an international Standard, to extend the life of the Technical Specification or to withdraw it. Comments should be sent to the Secretary of the responsible BSI Technical Committee at British Stan
7、dards House, 389 Chiswick High Road, London W4 4AL. The UK participation in its preparation was entrusted to Technical Committee ISE/18, Sampling and analysis of iron and steel. A list of organizations represented on ISE/18 can be obtained on request to its secretary. This publication does not purpo
8、rt to include all the necessary provisions of a contract. Users are responsible for its correct application. Amendments issued since publication Amd. No. DateComments Licensed Copy: London South Bank University, London South Bank University, Sat Dec 30 06:30:47 GMT+00:00 2006, Uncontrolled Copy, (c)
9、 BSI Reference number ISO/TS 13899-3:2005(E) TECHNICAL SPECIFICATION ISO/TS 13899-3 First edition 2005-02-15 Steel Determination of Mo, Nb and W contents in alloyed steel Inductively coupled plasma atomic emission spectrometric method Part 3: Determination of W content Aciers Dosage du Mo, du Nb et
10、du W dans les aciers allis Mthode par spectromtrie dmission atomique avec plasma induit par haute frquence Partie 3: Dosage du W DD ISO/TS 13899-3:2005 Licensed Copy: London South Bank University, London South Bank University, Sat Dec 30 06:30:47 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii License
11、d Copy: London South Bank University, London South Bank University, Sat Dec 30 06:30:47 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iii Contents Page Forewordiv 1 Scope 1 2 Normative references . 1 3 Principle. 1 4 Reagents 2 5 Apparatus 3 6 Sampling and samples. 4 7 Procedure 4 7.1 Preparation of te
12、st solution, Tn. 4 7.2 Preparation for spectrometric measurements. 5 7.3 Pre-analysis of the test solution 5 7.4 Preparation of calibration solutions for bracketing, KLn and KHn 6 7.5 Analysis of test solutions 6 8 Expression of results 6 8.1 Method of calculation. 6 8.2 Precision 6 9 Test report .
13、7 Annex A (normative) Procedure for the determination of instrumental criteria 8 Annex B (informative) Additional information on the international collaborative trial . 10 Annex C (informative) Graphical representation of precision data. 12 DD ISO/TS 13899-3:2005 Licensed Copy: London South Bank Uni
14、versity, London South Bank University, Sat Dec 30 06:30:47 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is norm
15、ally 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 that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in t
16、he work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare
17、 International Standards. 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 75 % of the member bodies casting a vote. In other circumstances, particularly when there
18、 is an urgent market requirement for such documents, a technical committee may decide to publish other types of normative document: an ISO Publicly Available Specification (ISO/PAS) represents an agreement between technical experts in an ISO working group and is accepted for publication if it is app
19、roved 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 and is accepted for publication if it is approved by 2/3 of the members of the committee casting a vote. An ISO/
20、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/PAS or ISO/TS is confirmed, it is reviewed again after a further three years, at which time it must either be t
21、ransformed 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 be held responsible for identifying any or all such patent rights. ISO/TS 13899-3 was prepared by Technical C
22、ommittee ISO/TC 17, Steel, Subcommittee SC 1, Methods of determination of chemical composition. ISO/TS 13899 consists of the following parts, under the general title Steel Determination of Mo, Nb and W contents in alloyed steel Inductively coupled plasma atomic emission spectrometric method: Part 1:
23、 Detemination of Mo content Part 2: Detemination of Nb content Part 3: Detemination of W content DD ISO/TS 13899-3:2005 Licensed Copy: London South Bank University, London South Bank University, Sat Dec 30 06:30:47 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 1 Steel Determination of Mo, Nb and W cont
24、ents in alloyed steel Inductively coupled plasma atomic emission spectrometric method Part 3: Determination of W content 1 Scope This Technical Specification specifies a method for the determination of tungsten content in steel by means of inductively coupled plasma atomic emission spectrometry. Thi
25、s method is applicable to tungsten contents between 0,1 % and 20 % (mass fraction). 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 latest edition of th
26、e referenced document (including any amendments) applies. ISO 648:1977, Laboratory glassware One-mark pipettes ISO 1042:1998, Laboratory glassware One-mark volumetric flasks ISO 3696:1987, Water for analytical laboratory use Specification and test methods ISO 5725-1:1994, Accuracy (trueness and prec
27、ision) of measurement methods and results Part 1: General principles 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,
28、 Accuracy (trueness and precision) of measurement methods and results Part 3: Intermediate measures of the precision of a standard measurement method ISO 14284:1996, Steel and iron Sampling and preparation of samples for the determination of chemical composition 3 Principle The sample is dissolved i
29、n a hydrochloric, nitric and hydrofluoric acid mixture and fumed with a phosphoric and perchloric acid mixture. Hydrofluoric acid and an internal standard element (if used) are added and the solution is diluted to known volume. The solution is filtered and nebulized into an inductively coupled plasm
30、a (ICP) spectrometer and the intensity of the emitted light from the element is measured simultaneously with the light emitted from the internal standard element. DD ISO/TS 13899-3:2005 Licensed Copy: London South Bank University, London South Bank University, Sat Dec 30 06:30:47 GMT+00:00 2006, Unc
31、ontrolled Copy, (c) BSI 2 The method uses a calibration based on close matrix matching of the calibration solutions to the sample and close bracketing of the tungsten content around the approximate concentration of tungsten in the sample to be analysed. This compensates for matrix interferences and
32、provides high accuracy, even in highly alloyed steels where spectral interferences can be severe. Nonetheless, all interferences shall be kept to a minimum and it is therefore essential that the spectrometer used meets the performance criteria specified in the method for the selected analytical line
33、s. In order to accurately matrix match, it is necessary to know the content of all elements in the sample (to the nearest %). To this end, it may be necessary to carry out a preliminary analysis of the sample by a semi-quantitative method. 4 Reagents During the analysis, unless otherwise stated, use
34、 only reagents of recognised analytical grade and only grade 2 water as specified in ISO 3696. 4.1 Hydrofluoric acid, HF, 40 % (mass fraction), approximately 1,14 g/ml 4.2 Hydrochloric acid, HCl, approximately 1,19 g/ml 4.3 Nitric acid, HNO3, approximately 1,40 g/ml 4.4 Phosphoric acid, H3PO4, appro
35、ximately 1,70 g/ml, diluted 1 + 1 4.5 Perchloric acid, HClO4, approximately 1,54 g/ml, diluted 1 + 1 4.6 Fuming acid mixture: mix 100 ml of the phosphoric acid (4.4) and 300 ml of the perchloric acid (4.5) 4.7 Internal standard solution, 1 000 mg/l Choose a suitable element to be added as internal s
36、tandard and prepare a 1 000 mg/l solution. The internal standard chosen shall be pure, shall not be present in the sample, and shall not interfere with analytical wavelengths, nor should the internal standard element wavelength be interfered with by elements in the test solution. The internal standa
37、rd shall be soluble in the acids used and it shall not cause precipitation. Moreover, the excitation conditions of the analytical line and the internal standard element line should match. 4.8 Tungsten stock standard solution, 1 000 mg/l Weigh, to the nearest 0,001 g, 0,5 g of high purity tungsten mi
38、nimum 99,95 % (mass fraction) and dissolve in a mixture of 10 ml hydrofluoric acid (4.1) and 20 ml nitric acid (4.3). Cool and transfer the solution quantitatively to a calibrated 500 ml one-mark plastic volumetric flask. Dilute to the mark with water and mix. 1 ml of this solution contains 1 mg of
39、W. It is not permitted to use pre-prepared tungsten standard solutions supplied by second parties. 4.9 Tungsten standard solution, 100 mg/l Transfer, with a calibrated micropipette, 25 ml of the tungsten stock standard solution (4.8) into a calibrated 250 ml one-mark plastic volumetric flask. Add 5
40、ml of hydrofluoric acid (4.1) and 10 ml of nitric acid (4.3). Dilute to the mark with water and mix. 1 ml of this solution contains 0,1 mg of W. DD ISO/TS 13899-3:2005 Licensed Copy: London South Bank University, London South Bank University, Sat Dec 30 06:30:47 GMT+00:00 2006, Uncontrolled Copy, (c
41、) BSI 3 NOTE If calibrated micropipettes of suitable volume are not available it would be more advantageous to use more concentrated standard solutions. These solutions must, however, be prepared for each series of analysis, in order to avoid possible precipitation. 4.10 Standard solutions of interf
42、ering and matrix elements Prepare standard solutions for each element of which more than 1 % (mass fraction) is contained in the test sample. Use pure elements or oxides with tungsten contents less than 10 g/g. Commercial certified standard solutions can also be used if the tungsten content is less
43、than the value specified above. NOTE If a large amount of an element is to be added (e.g. iron), it might be more advantageous to use the pure metal and weigh the correct amount (see 7.3 and 7.4). In this case, use the dissolution procedure described in 7.1.2. 5 Apparatus The plastic pipettes and fl
44、asks to be used shall be calibrated in accordance with ISO 648 or ISO 1042, as appropriate. Ordinary laboratory apparatus and 5.1 Atomic emission spectrometer, equipped with an inductively coupled plasma (ICP) and a nebulization system resistant to hydrofluoric acid. When a polytetrafluoroethylene (
45、PTFE) nebulizer is used, it is recommended that a surface active agent should be added to improve wetting in the nebulizer and spray chamber. Modern nebulizers are, however, often manufactured of plastic materials with better wetting-characteristics than PTFE and can therefore (as is the case with s
46、apphire nebulizers) be used without a surface active agent. The ICP-ES spectrometer used will be satisfactory if, after optimising according to 7.2.1 to 7.2.4, it meets the performance criteria given in 5.1.2 to 5.1.4. The spectrometer can be either the simultaneous or the sequential type. A sequent
47、ial type can be used either with or without an internal standard. However, if a sequential spectrometer is to be used with an internal standard, it shall be fitted with an arrangement which allows for the simultaneous measurement of the internal standard line. 5.1.1 Analytical lines This standard do
48、es not specify any particular emission line. It is mandatory that each laboratory carefully investigates the line/lines available on its own equipment to find the most suitable one regarding sensitivity and freedom from interferences. In Table 1, however, a suggestion is given together with possible
49、 interferences. The line for the internal standard element should be selected according to 4.7. Table 1 Example of analytical line and lines for internal standard element Wavelength Element nm Possible interferences W 207,91 Cr, V, Mo Sr (as internal standard) 407,77 Sc (as internal standard) 363,07 Cd (as internal standard) 214,44 DD ISO/TS 13899-3:2005 Licensed Copy: London South Bank University, London South Bank University, Sat Dec