BS-6783-7-1986 EN-27526-1991 ISO-7526-1985.pdf

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1、BRITISH STANDARD BS 6783-7: 1986 EN 27526:1991 ISO 7526:1985 Incorporating Amendment No. 1 Sampling and analysis of nickel, ferronickel and nickel alloys Part 7: Method for determination of sulphur in nickel, ferronickel and nickel alloys by infra-red absorption after induction furnace combustion IS

2、O title: Nickel, ferronickel and nickel alloys Determination of sulfur content Infra-red absorption method after induction furnace combustion This European Standard EN 27526:1991 has the status of a British Standard UDC 669.24:669.1524-198:620.1:543.422.4:543.845 BS 6783-7:1986 This British Standard

3、, having been prepared under the direction of the Non-ferrous Metals Standards Committee, was published under the authority of the Board of BSI and comes into effect on 31 December 1986 BSI 10-1999 The following BSI references relate to the work on this standard: Committee reference NFM/10 Draft for

4、 comment 84/39889 DC ISBN 0 580 15526 9 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Non-ferrous Metals Standards Committee (NFM/-) to Technical Committee NFM/10, upon which the following bodies were represented: British Non-ferrous M

5、etals Federation British Steel Industry Engineering Equipment and Materials Users Association Ministry of Defence Process Plant Association Stainless Steel Fabricators Association of Great Britain Coopted members Amendments issued since publication Amd. No.Date of issueComments 6993April 1992Indicat

6、ed by a sideline in the margin BS 6783-7:1986 BSI 10-1999i Contents Page Committees responsible Inside front cover National foreword ii 1Scope and field of application3 2References3 3Principle3 4Reagents and materials3 5Apparatus3 6Sampling and samples3 7Procedure3 8Expression of results4 9Notes on

7、procedure and equipment5 10Test report6 Annex A Examples of compositions of nickel, ferronickel and nickel alloys7 Annex B Features of commercial high frequency induction furnaces and infra-red sulfur analysers7 Table 1 Calibration example4 Table 2 Results of statistical analysis5 Table 3 Examples o

8、f composition of nickel (%)7 Table 4 Examples of composition of ferronickel (%)7 Table 5 Examples of composition of nickel alloys (%)8 Publications referred toInside back cover BS 6783-7:1986 ii BSI 10-1999 National foreword This Part of BS 6783 has been prepared under the direction of the Non-ferro

9、us Metals Standards Committee. It is identical with ISO 7526:1985 “Nickel, ferronickel and nickel alloys Determination of sulfur content Infra-red absorption method after induction furnace combustion” published by the International Organization for Standardization (ISO). In 1991 the European Committ

10、ee for Standardization (CEN) accepted ISO 7526:1985 as European Standard EN 27526:1991 without any modifications. At present this British Standard consists of nine Parts all concerned with analysis of nickel, ferronickel and nickel alloys. Further International Standards are in preparation on sampli

11、ng and analysis of nickel, ferronickel and nickel alloys and, when available, these will be published as further Parts of this British Standard. Terminology and conventions. The text of the International Standard has been approved as suitable for publication as a British Standard without deviation.

12、Some terminology and certain conventions are not identical with those used in British Standards; attention is drawn especially to the following. The comma has been used as a decimal marker. In British Standards it is current practice to use a full point on the baseline as the decimal marker. Whereve

13、r the words “International Standard” appear, referring to this standard, they should be read as “Part of BS 6783”. In British Standards it is current practice to use the symbol “L” for litre (and in its submultiples) rather than “l” and to use the spelling “sulphur”, etc., instead of sulfur, etc. A

14、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 immunity from legal obligations. Cross-references International StandardsCor

15、responding British Standards ISO 5725:1981BS 5497 Precision of test methods Part 1:1979 Guide for the determination of repeatability and reproducibility for a standard test method (Technically equivalent) ISO 7525:1985BS 6783 Sampling and analysis of nickel, ferronickel and nickel alloys Part 6:1986

16、 Method for determination of sulphur in nickel by methylene blue molecular absorption spectrometry after generation of hydrogen sulphide (Identical) Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN title page, pages 2 to 8, an inside back cover an

17、d a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 27526:1991 November 1991 UDC 669.24:669.1524-198:620.1:543.422.4

18、:543.845 Descriptors: Nickel, nickel alloys, ferronickel, chemical analysis, determination of content, sulphur, infrared spectroscopy, combustion analysis, induction furnaces English version Nickel, ferronickel and nickel alloys Determination of sulfur content Infra-red absorption method after induc

19、tion furnace combustion (ISO 7526:1985) Nickel, ferro-nickel et alliages de nickel Dosage du soufre Mthode par absorption dans linfrarouge aprs combustion dans un sour induction (ISO 7526:1985) Nickel, Ferronickel und Nickellegierungen Bestimmung des Schwefelgehaltes Verfahren der Infrarotabsorption

20、 nach Verbrennung im Induktionsofen (ISO 7526:1985) This European Standard was approved by CEN on 1991-11-06. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alter

21、ation. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by transl

22、ation under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg

23、, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels CEN 1991 Copyright reserved to all CEN members Ref. No. EN

24、 27526:1991 E 2 blank EN 27526:1991 BSI 10-19993 1 Scope and field of application This International Standard specifies an infra-red absorption method after combustion for the determination of the sulfur content of nickel and ferronickel in the range 0,001 to 0,3 % (m/m), and of nickel alloys in the

25、 range 0,001 to 0,1 % (m/m). Examples of compositions are given in Annex A. NOTEIt may be possible to apply this method in the range 0,000 2 to 0,001 % (m/m). However, there were insufficient laboratory test data to support the inclusion of this lower level in the scope. 2 References ISO 5725, Preci

26、sion of test methods Determination of repeatability and reproducibility by inter-laboratory tests. ISO 7525, Nickel Determination of sulfur content Methylene blue molecular absorption spectrometric method after generation of hydrogen sulfide. 3 Principle Combustion of a test portion in a flow of oxy

27、gen at a high temperature in a high frequency induction furnace in the presence of fluxes and accelerators. Measurement of the sulfur dioxide formed using an infra-red analyser and an integration procedure. 4 Reagents and materials 4.1 Oxygen (O2), 99,5 % (m/m) minimum. 4.2 Ascarite or soda lime, 0,

28、7 to 1,2 mm (14 to 22 mesh). 4.3 Magnesium perchlorate Mg(ClO4)2, 0,7 to 1,2 mm (14 to 22 mesh). 4.4 Glass-wool 4.5 Crucibles and lids 4.5.1 Ceramic crucibles shall be of precise dimensions so that the sample is positioned correctly in the induction coil of the furnace (see 9.1). 4.5.2 Pre-ignite th

29、e crucibles in air or oxygen in a furnace for not less than 1 h at 1 100 C and store in a desiccator or closed container. A resistance furnace with a combustion tube through which a flow of oxygen passes may be used. Crucible lids, used to help retain the solid oxidation products in the hot zone, ar

30、e pre-ignited in a similar manner. 4.6 Fluxes: Low sulfur tin, copper plus tin, copper or vanadium pentoxide (see 9.2). 4.7 Accelerators: Low sulfur copper, iron, tungsten or nickel (see 9.2). 4.8 Nickel, low sulfur of known value 1 700 C) is maintained after the test portion is fused so that the su

31、lfur dioxide may be completely removed from the furnace to the infra-red analyser. 9.3.6 The flow rate of oxygen may vary from one instrument to another but is usually about 2,0 l/min during the combustion period. 9.3.7 After the equipment has been idle for a few hours or after cleaning the furnace

32、chamber or filters, the instrument should be stabilized as directed in 7.1. 10 Test report The test report shall include the following information: a) the reference to the method used; b) the results of the analysis; c) the number of independent replications; d) any unusual features noted during the

33、 analysis; e) any operation not included in this International Standard or regarded as optional. EN 27526:1991 BSI 10-19997 Annex A Examples of compositions of nickel, ferronickel and nickel alloys (This annex does not form part of this International Standard.) The examples of compositions given in

34、Table 3, Table 4 and Table 5 are not to be interpreted as specifications for chemical compositions. Table 3 Examples of composition of nickel (%) Table 4 Examples of composition of ferronickel (%) Annex B Features of commercial high frequency induction furnaces and infra-red sulfur analysers (This a

35、nnex does not form part of this International Standard.) B.1 Combustion furnace B.1.1 The combustion furnace consists of an induction coil and a high frequency generator. The furnace chamber consists of a silica tube which fits inside the induction coil. This tube has metal plates at the top and bot

36、tom which are sealed to the tube by O-rings. Gas inlet and outlet points are made through the metal plates. B.1.2 The generator is usually a 1,5 to 2,5 kVA apparent power unit but the frequency used by various manufacturers may be different. Values of 2 to 6; 15; and 20,0 MHz have been used. The pow

37、er from the generator is fed to the induction coil which surrounds the silica furnace tube and is usually air cooled. B.1.3 The crucible containing the sample, flux and accelerator is supported on a pedestal post which is precisely positioned so that, when raised, the metal in the crucible is correc

38、tly placed within the induction coil for effective coupling when the power is applied. B.1.4 The induction coil diameter, the number of turns and the furnace chamber geometry and the power of the generator determine the degree of coupling which can occur. These factors are determined by the instrume

39、nt manufacturer. B.1.5 The temperature attained during combustion depends in part on the factors in B.1.4 but also on the characteristics of the metal in the crucible, the form of the test portion and the mass of material. Some of these factors may be varied to some extent by the operator. B.2 Infra

40、-red gas analyser B.2.1 In most instruments the gaseous products of combustion are transferred in a continuous flow of oxygen to the analyser system. The gases flow through an infra-red cell, for example of the Luft type, where the absorbance of the infra-red radiation due to sulfur dioxide is measu

41、red and integrated over a pre-programmed time period. The signal is amplified and converted to a digital display of the percentage concentration of sulfur. B.2.2 In some analysers the products of combustion may be collected in oxygen in a fixed volume at controlled pressure and the mixture analysed

42、for sulfur dioxide. Ni + Co Co (max.) C (max.) Cu (max.) Fe (max.) S (max.) 99,95 99,9 99,0 0,1 0,5 1,5 0,015 0,03 0,15 0,005 0,03 0,2 0,02 0,03 0,4 0,002 5 0,03 0,01 TypeNiC Cr (max.) Cu (max.) Fe S (max.) Si (max.) LC15 60 0,005 0,03 0,100,20Rem.0,030,20 MC15 60 0,03 1,0 0,50,20Rem.0,101,0 HC15 60

43、 1,0 2,5 2,00,20Rem.0,404,0 NOTECo is usually 1/40 to 1/20 of Ni. EN 27526:1991 8 BSI 10-1999 B.2.3 Electronic controls are usually provided for adjusting the instrument zero, compensating for the blank, adjusting the slope of the calibration line and correction for non-linear response. The analyser

44、 generally has means of entering the mass of the standard or test portion for automatic correction of the read-out. Instruments may also be equipped with an integrated automatic balance for weighing the crucible, weighing the test portion and transferring the mass to the analyser. Table 5 Examples o

45、f composition of nickel alloys (%)a AlloybAlBCCocCrCuFeMnMoNiPSSiTiOthers A0,30 28,0 34,0 2,52,063,0d0,0250,5 B0,15 14,0 17,0 0,5 6,0 10,0 1,072,0d0,0150,5 C 0,4 1,0 0,08 14,0 17,0 0,5 5,0 9,0 1,070,0d0,0150,5 2,2 2,8 Nb plus Ta 0,7 to 1,2 D 0,2 0,8 0,0060,08 17,0 21,0 0,3Rem.0,4 2,8 3,3 50,0 55,0 0

46、,0150,0150,4 0,6 1,2 Nb plus Ta 4,7 to 5,5 E 0,15 0,60 0,10 19,0 23,0 0,7Rem.1,5 30,0 35,0 0,0151,0 0,15 0,60 F 0,08 0,15 5,0 18,0 21,0 0,55,01,0Rem.d0,0201,0 0,2 0,6 Pb 0,005 G 1,0 2,0 0,0200,13 15,0 21,0 18,0 21,0 0,21,51,0Rem.0,0151,0 2,0 3,0 Zr 0,15 H 4,5 4,9 0,003 0,010 0,12 0,17 18,0 22,0 14,0

47、 15,7 0,21,01,0 4,5 5,5 Rem.0,0151,0 0,9 1,5 Zr 0,15 I 0,3 0,6 0,005 0,04 0,08 19,0 21,0 19,0 21,0 0,20,70,6 5,6 6,1 Rem.0,0070,4 1,9 2,4 Ti plus Al 2,4 to 2,8 J0,021,01,02,01,0 26,0 30,0 Rem.d0,0400,0350,1 K 1,2 1,6 0,003 0,010 0,02 0,10 12,0 15,0 18,0 21,0 0,12,01,0 3,5 5,0 Rem.0,0150,0150,1 2,8 3

48、,3 Zr 0,02 to 0,08 L0,022,5 14,5 16,5 4,0 7,0 1,0 15,0 17,0 Rem.0,0400,0350,08 V 0,35 W 3,0 to 4,5 a Single values are maximum limits, except for nickel, where single values are minimum. b Alloy letters are used instead of commercial names until a neutral ISO designation is developed. c Where no lim

49、its are given, cobalt is up to a maximum of 1,5 % of (m/m). d Cobalt counts as nickel in some alloys. BS 6783-7:1986 BSI 10-1999 Publications referred to See national foreword. BS 6783-7: 1986 EN 27526:1991 ISO 7526:1985 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the international level. It is incorp

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