BS-7455-9-1994 ISO-7530-9-1993.pdf

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1、BRITISH STANDARD BS 7455-9: 1994 ISO 7530-9: 1993 Analysis of nickel alloys by flame atomic absorption spectrometry Part 9: Method for determination of vanadium UDC 669.245:543.422:546.881 Licensed Copy: London South Bank University, London South Bank University, Fri Dec 08 14:00:41 GMT+00:00 2006,

2、Uncontrolled Copy, (c) BSI BS 7455-9:1994 This British Standard, having been prepared under the direction of the Non-ferrous Metals Standards Policy Committee, was published under the authority of the Standards Board and comes into effect on 15 June 1994 BSI 11-1999 The following BSI references rela

3、te to the work on this standard: Committee reference NFM/10 Draft for comment 92/42776 DC ISBN 0 580 23365 0 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Non-ferrous Metals Standards Policy Committee (NFM/-) to Technical Committee NFM

4、/10, upon which the following bodies were represented: Association of Bronze and Brass Founders British Non-ferrous Metals Federation British Stainless Steel Association British Steel Industry Department of Trade and Industry (Laboratory of the Government Chemist) Engineering Equipment and Materials

5、 Users Association Institute of British Foundrymen London Metal Exchange Ministry of Defence Nickel Development Institute Non-ferrous Metal Stockists Steel Casting Research and Trade Association Coopted members Amendments issued since publication Amd. No.DateComments Licensed Copy: London South Bank

6、 University, London South Bank University, Fri Dec 08 14:00:41 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 7455-9:1994 BSI 11-1999i Contents Page Committees responsibleInside front cover National forewordii 1Scope1 2Normative references1 3Principle1 4Reagents1 5Apparatus1 6Sampling and sample prep

7、aration1 7Procedure1 8Expression of results2 9Test report2 Table 1 Nominal composition of test samples % (m/m)2 Table 2 Results of statistical analysis2 List of referencesInside back cover Licensed Copy: London South Bank University, London South Bank University, Fri Dec 08 14:00:41 GMT+00:00 2006,

8、Uncontrolled Copy, (c) BSI BS 7455-9:1994 ii BSI 11-1999 National foreword This Part of BS 7455 has been prepared under the direction of the Non-ferrous Metals Standards Policy Committee. It is identical with ISO 7530-9:1993 Nickel alloys Flame atomic absorption spectrometric analysis Part 9: Determ

9、ination of vanadium content, published by the International Organization for Standardization (ISO). At present this British Standard consists of nine Parts all concerned with methods for flame spectrometric analysis of nickel alloys. Further International Standards are in preparation on the same sub

10、ject and when available, these will be published as further Parts of this British Standard. 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

11、 of itself confer immunity from legal obligations. Cross-references International StandardCorresponding British Standard ISO 5725:1986BS 5497 Precision of test methods Part 1:1987 Guide for the determination of repeatability and reproducibility for a standard test method by inter-laboratory tests (I

12、dentical) ISO 7530-1:1990BS 7455 Analysis of nickel alloys by flame atomic absorption spectrometry Part 1:1991 General requirements and sample dissolution (Identical) Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages 1 and 2, an inside back cover an

13、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. Licensed Copy: London South Bank University, London South Bank University, Fri Dec 08 14:00:41 GMT+00:00 2006, Uncont

14、rolled Copy, (c) BSI BS 7455-9:1994 BSI 11-19991 1 Scope This part of ISO 7530 specifies a flame atomic absorption spectrometric method for the determination of vanadium in the range of 0,05 % (m/m) to 1 % (m/m) in nickel alloys. Typical compositions of nickel alloys are given in Annex B of ISO 7530

15、-1:1990. The general requirements concerning the apparatus, sampling, dissolution of the test sample, atomic absorption measurements, calculations and test report are given in ISO 7530-1. 2 Normative references The following standards contain provisions which, through reference in this text, constit

16、ute provisions of this part of ISO 7530. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this part of ISO 7530 are encouraged to investigate the possibility of applying the most recent editions of the standards

17、indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 5725:1986, Precision of test methods Determination of repeatability and reproducibility for a standard test method by inter-laboratory tests. ISO 7530-1:1990, Nickel alloys Flame atomic absorpt

18、ion spectrometric analysis Part 1: General requirements and sample dissolution. 3 Principle Dissolution of a test portion in acid and aspiration of the test solution into a nitrous oxide-acetylene flame of an atomic absorption spectrometer. Measurement of the absorbance of the resonance line energy

19、from the spectrum of vanadium and comparison with that of calibration solutions at a wavelength of 318,4 nm. 4 Reagents In addition to the reagents listed in clause 4 of ISO 7530-1:1990, the following special reagents are required. 4.1 Ammonium metavanadate (NH4VO3), an alternative to pure vanadium

20、metal. 4.2 Strontium chloride, solution. Transfer 113,5 g of strontium chloride hexahydrate (SrCl2.6H2O) to a 600 ml beaker, dissolve in 400 ml of hot water (50 C to 60 C), cool and transfer to a 1 000 ml one-mark volumetric flask. Make up to the mark with water and mix. The strontium chloride shoul

21、d be free of heavy metals. 4.3 Vanadium, standard reference solution (1,000 g/l). 4.3.1 Preparation from vanadium metal Weigh, to the nearest 0,001 g, 1,000 g of vanadium metal of 99,9 % (m/m) minimum purity and transfer to a 400 ml beaker. Add 60 ml of hydrochloric acid (20= 1,18 g/ml) and 20 ml of

22、 nitric acid (20= 1,41 g/ml) and heat to complete dissolution. Cool and transfer to a 1 000 ml one-mark volumetric flask. Make up to the mark with water, mix and store in a polyethylene bottle. 4.3.2 Preparation from ammonium metavanadate Weigh 2,296 g of ammonium metavanadate (4.1) and transfer to

23、a 600 ml beaker. Add about 400 ml of water and heat to dissolve the salt. Transfer the warm solution to a 1 000 ml one-mark volumetric flask and dilute with 400 ml of cold water. Add 50 ml of hydrochloric acid (20= 1,18 g/ml) and 10 ml of nitric acid (20= 1,41 g/ml), and cool to ambient temperature.

24、 Make up to the mark with water, mix and store in a polyethylene bottle. 4.4 Vanadium, standard solution (250 mg/l). Pipette 50 ml of the vanadium standard reference solution (4.3) into a 200 ml one-mark volumetric flask. Make up to the mark with water, mix and store in a polyethylene bottle. 5 Appa

25、ratus The apparatus required is specified in clause 5 of ISO 7530-1:1990. 6 Sampling and sample preparation Refer to clause 6 of ISO 7530-1:1990. 7 Procedure 7.1 Preparation of test solution Proceed as directed in 7.1.1 to 7.1.4 of ISO 7530-1:1990, using 3 ml of hydrochloric acid (20= 1,18 g/ml) and

26、 1 ml of nitric acid (20= 1,41 g/ml) instead of 5 ml of hydrochloric acid (20= 1,18 g/ml) to dissolve the salts. 7.1.1 Primary dilution for 0,05 % (m/m) to 0,35 % (m/m) vanadium Transfer the test solution (7.1) to a 100 ml one-mark volumetric flask. Add 5 ml of the strontium chloride solution (4.2),

27、 make up to the mark with water and mix. Remove any products of hydrolysis by settlement and dry filtration or by centrifuging. Licensed Copy: London South Bank University, London South Bank University, Fri Dec 08 14:00:41 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 7455-9:1994 2 BSI 11-1999 7.1.2

28、 Secondary dilution for 0,35 % (m/m) to 1,0 % (m/m) vanadium Pipette 20,0 ml of the solution from 7.1.1 into a 100 ml one-mark volumetric flask. Add 4 ml of the strontium chloride solution (4.2), 3 ml of hydrochloric acid (20= 1,18 g/ml) and 1 ml of nitric acid (20= 1,41 g/ml). Make up to the mark w

29、ith water and mix. 7.2 Reagent blank solution Carry out a blank test in parallel with the determination, following the same procedure and using the same quantities of all the reagents. 7.3 Vanadium calibration solutions Using a burette, transfer to each of five 100 ml one-mark volumetric flasks, 0 m

30、l, 4,0 ml, 8,0 ml, 12,0 ml and 16,0 ml of the vanadium standard solution (4.4). Add 5 ml of the strontium chloride solution (4.2), 3 ml of hydrochloric acid (20= 1,18 g/ml) and 1 ml of nitric acid (v20= 1,41 g/ml). Make up to the mark with water and mix. These calibration solutions correspond to 0 m

31、g/l, 10 mg/l, 20 mg/l, 30 mg/l, and 40 mg/l of vanadium. 7.4 Calibration and determination 7.4.1 Atomic absorption measurements Proceed as directed in 7.4.1 of ISO 7530-1:1990, using a wavelength of 318,4 nm and a fuel-rich nitrous oxide-acetylene flame. 7.4.2 Preparation of calibration curves Proce

32、ed as directed in 7.4.2 of ISO 7530-1:1990. 7.5 Number of determinations Carry out the determination at least in duplicate. 8 Expression of results 8.1 Calculation Proceed as directed in 8.1 of ISO 7530-1:1990. 8.2 Precision 8.2.1 Laboratory tests Six laboratories in four countries participated in t

33、he testing of this procedure using the IN100 sample. Nine laboratories in five countries analysed sample NPK31 and sample 925. The nominal composition of the samples is given in Table 1. 8.2.2 Statistical analysis 8.2.2.1 Results were treated according to ISO 5725 as described in 8.2.2 of ISO 7530-1

34、:1990. The results of this analysis are given in Table 2. 8.2.2.2 One laboratory was rejected as a Cochran outlier for sample 925. 9 Test report Refer to clause 9 of ISO 7530-1:1990. Table 1 Nominal composition of test samples % (m/m) Table 2 Results of statistical analysis SampleAlCoCrFeMoNiNbTiVZr

35、 IN100 NPK31 925 5,5 0,5 0,3 15 14 0,2 10 20 21 0,5 1 27 3 4,5 3 Remainder Remainder Remainder 5 0,4 5 2 2 1 0,3 0,05 0,05 Sample reference Mean % (m/m) Within-laboratory standard deviation Between-laboratory standard deviation RepeatabilityReproducibility IN100 NPK31 925 0,965 0,286 0,042 0,005 8 0

36、,008 7 0,001 2 0,035 7 0,026 2 0,005 9 0,016 5 0,024 7 0,003 4 0,101 7 0,076 1 0,017 0 Licensed Copy: London South Bank University, London South Bank University, Fri Dec 08 14:00:41 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 7455-9:1994 BSI 11-1999 List of references See national foreword. Licens

37、ed Copy: London South Bank University, London South Bank University, Fri Dec 08 14:00:41 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 7455-9: 1994 ISO 7530-9: 1993 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent national body responsible for prepari

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