1、BRITISH STANDARD BS7455-9: 1994 ISO7530-9: 1993 Analysis of nickel alloys by flame atomic absorption spectrometry Part9: Method for determination of vanadium UDC 669.245:543.422:546.881BS7455-9:1994 This British Standard, having been prepared under the directionof the Non-ferrous Metals Standards Po
2、licy Committee, was published underthe authority of the Standards Board and comesinto effect on 15June1994 BSI11-1999 The following BSI references relate to the work on this standard: Committee reference NFM/10 Draft for comment92/42776DC ISBN 0 580 23365 0 Committees responsible for this British St
3、andard The preparation of this British Standard was entrusted by the Non-ferrous Metals Standards Policy Committee (NFM/-) to Technical Committee NFM/10, upon which the following bodies were represented: Association of Bronze and Brass Founders British Non-ferrous Metals Federation British Stainless
4、 Steel Association British Steel Industry Department of Trade and Industry (Laboratory of the Government Chemist) Engineering Equipment and Materials Users Association Institute of British Foundrymen London Metal Exchange Ministry of Defence Nickel Development Institute Non-ferrous Metal Stockists S
5、teel Casting Research and Trade Association Coopted members Amendments issued since publication Amd. No. Date CommentsBS7455-9:1994 BSI 11-1999 i Contents Page Committees responsible Inside front cover National foreword ii 1 Scope 1 2 Normative references 1 3 Principle 1 4 Reagents 1 5 Apparatus 1 6
6、 Sampling and sample preparation 1 7 Procedure 1 8 Expression of results 2 9 Test report 2 Table 1 Nominal composition of test samples % (m/m) 2 Table 2 Results of statistical analysis 2 List of references Inside back coverBS7455-9:1994 ii BSI 11-1999 National foreword This Part of BS7455 has been p
7、repared under the direction of the Non-ferrous Metals Standards Policy Committee. It is identical with ISO7530-9:1993 Nickel alloys Flame atomic absorption spectrometric analysis Part9:Determination of vanadium content, published by the International Organization for Standardization (ISO). At presen
8、t 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 subject and when available, these will be published as further Parts of this British Standard. A British Standar
9、d 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 Standard Corresponding Brit
10、ish Standard ISO5725:1986 BS5497 Precision of test methods Part1:1987 Guide for the determination of repeatability and reproducibility for a standard test method by inter-laboratory tests (Identical) ISO7530-1:1990 BS7455 Analysis of nickel alloys by flame atomic absorption spectrometry Part1:1991 G
11、eneral requirements and sample dissolution (Identical) Summary of pages This document comprises a front cover, an inside front cover, pagesi andii, pages1 and 2, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This
12、will be indicated in the amendment table on the inside front cover.BS7455-9:1994 BSI 11-1999 1 1 Scope This part of ISO7530 specifies a flame atomic absorption spectrometric method for the determination of vanadium in the range of0,05%(m/m) to1% (m/m) in nickel alloys. Typical compositions of nickel
13、 alloys are given in Annex B ofISO7530-1:1990. The general requirements concerning the apparatus, sampling, dissolution of the test sample, atomic absorption measurements, calculations and test report are given in ISO7530-1. 2 Normative references The following standards contain provisions which, th
14、rough reference in this text, constitute provisions of this part of ISO7530. 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 ISO7530 are encouraged to investigate the possibility of applying the mos
15、t recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO5725:1986, Precision of test methods Determination of repeatability and reproducibility for a standard test method by inter-laboratory tests. ISO7530-1:1990, N
16、ickel alloys Flame atomic absorption spectrometric analysis Part1: 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 absorban
17、ce of the resonance line energy from the spectrum of vanadium and comparison with that of calibration solutions at a wavelength of318,4nm. 4 Reagents In addition to the reagents listed in clause4 ofISO7530-1:1990, the following special reagentsare required. 4.1 Ammonium metavanadate (NH 4 VO 3 ), an
18、 alternative to pure vanadium metal. 4.2 Strontium chloride, solution. Transfer113,5g of strontium chloride hexahydrate (SrCl 2 .6H 2 O) to a600ml beaker, dissolve in400ml of hot water(50 C to60 C), cool and transfer to a1000ml one-mark volumetric flask. Make up to the mark with water and mix. The s
19、trontium chloride should be free of heavy metals. 4.3 Vanadium, standard reference solution(1,000g/l). 4.3.1 Preparation from vanadium metal Weigh, to the nearest0,001g,1,000g of vanadium metal of99,9% (m/m) minimum purity and transferto a400ml beaker. Add60ml of hydrochloric acid( 20 =1,18g/ml) and
20、20ml of nitric acid( 20 =1,41g/ml) and heat to complete dissolution. Cool and transfer to a1000ml 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 Weigh2,296g of ammonium metavanadate(4.1) and transfer to
21、a600ml beaker. Add about400ml of water and heat to dissolve the salt. Transfer the warm solution to a1000ml one-mark volumetric flask and dilute with400ml of cold water. Add50ml of hydrochloric acid( 20 =1,18g/ml) and10ml of nitric acid( 20 =1,41g/ml), and cool to ambient temperature. Make up to the
22、 mark with water, mix and store in a polyethylene bottle. 4.4 Vanadium, standard solution(250mg/l). Pipette50ml of the vanadium standard reference solution(4.3) into a200ml one-mark volumetric flask. Make up to the mark with water, mix and store in a polyethylene bottle. 5 Apparatus The apparatus re
23、quired is specified in clause5 ofISO7530-1:1990. 6 Sampling and sample preparation Refer to clause6 of ISO7530-1:1990. 7 Procedure 7.1 Preparation of test solution Proceed as directed in7.1.1 to7.1.4 of ISO7530-1:1990, using3ml of hydrochloric acid( 20 =1,18g/ml) and1ml of nitric acid( 20 =1,41g/ml)
24、 instead of5ml of hydrochloric acid( 20 =1,18g/ml) to dissolve the salts. 7.1.1 Primary dilution for0,05% (m/m) to0,35% (m/m) vanadium Transfer the test solution(7.1) to a100ml one-mark volumetric flask. Add5ml of the strontium chloride solution(4.2), make up to the mark with water and mix. Remove a
25、ny products of hydrolysis by settlement and dry filtration or by centrifuging.BS7455-9:1994 2 BSI 11-1999 7.1.2 Secondary dilution for0,35% (m/m) to1,0% (m/m) vanadium Pipette20,0ml of the solution from7.1.1 into a100ml one-mark volumetric flask. Add4ml of the strontium chloride solution(4.2),3ml of
26、 hydrochloric acid( 20 =1,18g/ml) and1ml of nitric acid ( 20 =1,41g/ml). Make up to the mark with 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 calibrat
27、ion solutions Using a burette, transfer to each of five100ml one-mark volumetric flasks,0ml,4,0ml,8,0ml,12,0ml and16,0ml of the vanadium standard solution(4.4). Add5ml of the strontium chloride solution(4.2),3ml of hydrochloric acid( 20 =1,18g/ml) and1ml of nitric acid (v 20 =1,41g/ml). Make up to t
28、he mark with water and mix. These calibration solutions correspond to0mg/l,10mg/l,20mg/l,30mg/l, and40mg/l of vanadium. 7.4 Calibration and determination 7.4.1 Atomic absorption measurements Proceed as directed in7.4.1 of ISO7530-1:1990, using a wavelength of318,4nm and a fuel-rich nitrous oxide-ace
29、tylene flame. 7.4.2 Preparation of calibration curves Proceed as directed in7.4.2 of ISO7530-1:1990. 7.5 Number of determinations Carry out the determination at least in duplicate. 8 Expression of results 8.1 Calculation Proceed as directed in8.1 of ISO7530-1:1990. 8.2 Precision 8.2.1 Laboratory tes
30、ts Six laboratories in four countries participated in the testing of this procedure using the IN100 sample. Nine laboratories in five countries analysed sample NPK31 and sample925. The nominal composition of the samples is given in Table 1. 8.2.2 Statistical analysis 8.2.2.1 Results were treated acc
31、ording to ISO5725 as described in8.2.2 of ISO7530-1:1990. The results of this analysis are given in Table 2. 8.2.2.2 One laboratory was rejected as a Cochran outlier for sample925. 9 Test report Refer to clause9 of ISO7530-1:1990. Table 1 Nominal composition of test samples % (m/m) Table 2 Results o
32、f statistical analysis Sample Al Co Cr Fe Mo Ni Nb Ti V Zr 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 Repeatability
33、Reproducibility IN100 NPK31 925 0,965 0,286 0,042 0,0058 0,0087 0,0012 0,0357 0,0262 0,0059 0,0165 0,0247 0,0034 0,1017 0,0761 0,0170BS7455-9:1994 BSI 11-1999 List of references See national foreword.BS7455-9: 1994 ISO7530-9: 1993 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstituti
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