1、BSI Standards PublicationBS ISO 7530-1:2015Nickel alloys Flame atomicabsorption spectrometricanalysisPart 1: Determination of cobalt, chromium,copper, iron and manganeseBS ISO 7530-1:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 7530-1:2015.It supersedes
2、 BS 7455-1:1991, BS 7455-2:1991, BS 7455-3:1991,BS 7455-4:1991, BS 7455-5:1991 and BS 7455-6:1991, which arewithdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee I/-, Miscellaneous standards materials and chemicals.A list of organizations represented on this committee
3、 can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2015. Published by BSI StandardsLimited 2015ISBN 978 0 580 84700 4ICS 77.120.40Compl
4、iance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 30 June 2015.Amendments issued since publicationDate Text affectedBS ISO 7530-1:2015 ISO 2015Nickel alloys Flame atomic
5、absorption spectrometric analysis Part 1: Determination of cobalt, chromium, copper, iron and manganeseAlliages de nickel Analyse par spectromtrie dabsorption atomique dans la flamme Partie 1: Dtermination du cobalt, du chrome, du cuivre, du fer et du manganseINTERNATIONAL STANDARDISO7530-1Second ed
6、ition2015-06-15Reference numberISO 7530-1:2015(E)BS ISO 7530-1:2015ISO 7530-1:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2015, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in a
7、ny form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCh. de Blan
8、donnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 7530-1:2015ISO 7530-1:2015(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Principle 14 Reagents 15 Apparatus . 46 Sampling and sample preparation 47 Procedur
9、e. 57.1 Test portion 57.2 Blank test . 57.3 Dissolution 57.4 Determination of cobalt 57.4.1 Preparation of the test solution 57.4.2 Preparation of the calibration solutions 67.5 Determination of chromium 77.5.1 Preparation of the test solution 77.5.2 Preparation of the calibration solutions 87.6 Det
10、ermination of copper 97.6.1 Preparation of the test solution 97.6.2 Preparation of the calibration solutions 97.7 Determination of iron 117.7.1 Preparation of the test solution . 117.7.2 Preparation of the calibration solutions .127.8 Determination of manganese 137.8.1 Preparation of the test soluti
11、on . 137.8.2 Preparation of the calibration solutions .137.9 Adjustment of atomic absorption spectrometer .157.10 Spectrometric measurements . 157.11 Calibration curves . 167.12 Expression of results . 167.13 Precision 167.13.1 General. 167.13.2 Precision for cobalt .177.13.3 Precision for chromium
12、187.13.4 Precision for copper .187.13.5 Precision for iron 187.13.6 Precision for manganese 188 Test report 19Annex A (normative) Procedures for checking the instrumental criteria .20Bibliography .23 ISO 2015 All rights reserved iiiContents PageBS ISO 7530-1:2015ISO 7530-1:2015(E)ForewordISO (the In
13、ternational Organization for Standardization) is a worldwide 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 h
14、as 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 the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical
15、 standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in ac
16、cordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).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. Deta
17、ils of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an en
18、dorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee resp
19、onsible for this document is ISO/TC 155, Nickel and nickel alloys.This second edition of ISO 7530-1 cancels and replaces ISO 7530-1:1990, ISO 7530-2:1990, ISO 7530-3:1990, ISO 7530-4:1990, ISO 7530-5:1990, and ISO 7530-6:1990, which have been technically revised.ISO 7530 consists of the following pa
20、rts, under the general title Nickel alloys Flame atomic absorption spectrometric analysis: Part 1: Determination of cobalt, chromium, copper, iron and manganese Part 7: Determination of aluminium content Part 8: Determination of silicon content Part 9: Determination of vanadium contentiv ISO 2015 Al
21、l rights reservedBS ISO 7530-1:2015ISO 7530-1:2015(E)IntroductionThis part of ISO 7530 describes five flame atomic absorption spectrometric methods for the determination of cobalt, chromium, copper, iron, and manganese in nickel alloys.Although the methods are described independently, it is possible
22、 to determine more than one element on a single test solution by adjustment of the sample weight and initial and subsequent dilutions. ISO 2015 All rights reserved vBS ISO 7530-1:2015BS ISO 7530-1:2015Nickel alloys Flame atomic absorption spectrometric analysis Part 1: Determination of cobalt, chrom
23、ium, copper, iron and manganese1 ScopeThis part of ISO 7530 describes flame atomic absorption spectrometric methods for the determination of cobalt, chromium, copper, iron, and manganese in nickel alloys which can be dissolved in the nitric-hydrochloric acids mixture specified.For each element, the
24、method is applicable to the content range between 0,01 % and 4 %.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, th
25、e latest edition of the referenced document (including any amendments) applies.ISO 385, Laboratory glassware BurettesISO 648, Laboratory glassware Single-volume pipettesISO 1042, Laboratory glassware One-mark volumetric flasks3 PrincipleDissolution of a test portion in a nitrichydrochloric acids mix
26、ture, evaporation of acids excess, and dissolution of the salts.Addition of an ionization suppressant if necessary and dilution of the solution to a known volume.Nebulization of the test solution after suitable dilution, if necessary, into an air/acetylene or a nitrous oxide/acetylene flame of an at
27、omic absorption spectrometer.Measurement of the absorption of the energy of the resonance line from the spectrum of the element being determined and comparison with that of calibration solutions of the same element.4 ReagentsDuring the analysis, unless otherwise stated, use only reagents of recogniz
28、ed analytical grade and only distilled water or water of equivalent purity.4.1 Nitric acid, (HNO3) 20= 1,41 g/ml.4.2 Nitric acid solution, 1 + 1.Add 500 ml of nitric acid (4.1) to 500 ml of water.INTERNATIONAL STANDARD ISO 7530-1:2015(E) ISO 2015 All rights reserved 1BS ISO 7530-1:2015ISO 7530-1:201
29、5(E)4.3 Hydrochloric acid, (HCI) 20= 1,18 g/ml.4.4 Hydrochloric acid solution, 1 + 1.Add 500 ml of hydrochloric acid (4.3) to 500 ml of water.4.5 Nitric-hydrochloric acids mixture.CAUTION This acid mixture is highly corrosive and unstable. Noxious gas (chlorine) is liberated on standing. It shall be
30、 prepared and used in a fume cupboard and shall not be kept in a closed container.Carefully mix one part of nitric acid (4.2) and three parts of hydrochloric acid (4.3). This mixture is not stable and should be prepared only as needed.4.6 Strontium chloride solution.Transfer 113,5 g of strontium chl
31、oride hexahydrate (SrCl2. 6H2O) into a 600 ml beaker and dissolve in 400 ml of hot water (50 C to 60 C). Cool, transfer into a 1 000 ml one-mark volumetric flask, dilute to the mark with water, and mix.4.7 Hydrogen peroxide, 300 g/l solution.4.8 Cobalt standard solution, 1,000 g/l.Weigh 1 g 0,001 g
32、of cobalt (Co 99,9 %) and transfer it into a 400 ml beaker. Add 30 ml of hydrochloric acid solution (4.4), cover with a watch glass, and heat gently until the cobalt is completely dissolved. Cool to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, add
33、 35 ml of hydrochloric acid (4.3), dilute to the mark with water, and mix well.1 ml of this solution contains 1,000 mg of cobalt.4.9 Cobalt standard solution, 0,025 g/l.Transfer 5,0 ml of cobalt standard solution (4.8) into a 200 ml one-mark volumetric flask and add 10 ml of hydrochloric acid (4.3).
34、 Dilute to the mark with water and mix well.Prepare this solution immediately prior to use.1 ml of this solution contains 0,025 mg of cobalt.4.10 Chromium standard solution, 1,000 g/l.Weigh 1 g 0,001 g of chromium (Cr 99,9 %) and transfer it into a 400 ml beaker. Add 30 ml of hydrochloric acid (4.4)
35、, cover with a watch glass, and heat to complete dissolution. Cool to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, add 35 ml of hydrochloric acid (4.3), dilute to the mark with water, and mix well.1 ml of this solution contains 1,000 mg of chromiu
36、m.4.11 Chromium standard solution, 0,100 g/l.Transfer 20,0 ml of chromium standard solution (4.10) into a 200 ml one-mark volumetric flask and add 10 ml of hydrochloric acid (4.3). Dilute to the mark with water and mix well.Prepare this solution immediately prior to use.1 ml of this solution contain
37、s 0,100 mg of chromium.2 ISO 2015 All rights reservedBS ISO 7530-1:2015ISO 7530-1:2015(E)4.12 Copper standard solution, 1,000 g/l.Weigh 1 g 0,001 g of copper (Cu 99,9 %) and transfer it into a 400 ml beaker. Add 50 ml of nitric acid (4.2), cover with a watch glass, and allow to stand until the react
38、ion ceases. Heat to complete dissolution, boil to remove nitrogen oxides, and evaporate just to dryness. Cool, add 25 ml of hydrochloric acid (4.3), and evaporate just to dryness. Add again 25 ml of hydrochloric acid (4.3) and repeat the evaporation. Dissolve the salts in 50 ml of hydrochloric acid
39、(4.4) and heat if necessary. Cool, transfer into a 1 000 ml one-mark volumetric flask, dilute to the mark with water, and mix well.1 ml of this solution contains 1,000 mg of copper.4.13 Copper standard solution, 0,100 g/l.Transfer 10,0 ml of copper standard solution (4.12) into a 100 ml one-mark vol
40、umetric flask and add 5 ml of hydrochloric acid (4.3). Dilute to the mark with water and mix well.Prepare this solution immediately prior to use.1 ml of this solution contains 0,100 mg of copper.4.14 Copper standard solution, 0,025 g/l.Transfer 5,0 ml of copper standard solution (4.12) into a 200 ml
41、 one-mark volumetric flask and add 10 ml of hydrochloric acid (4.3). Dilute to the mark with water and mix well.Prepare this solution immediately prior to use.1 ml of this solution contains 0,025 mg of copper.4.15 Iron standard solution, 1,000 g/l.Weigh 1 g 0,001 g of iron (Fe 99,9 %) and transfer i
42、t into a 400 ml beaker. Add 30 ml of hydrochloric acid (4.4) and cover with a watch glass. Heat to initiate the reaction and complete dissolution. Cool to about 50 C, cautiously add 1 ml of hydrogen peroxide (4.7), and bring to the boil to oxidize the iron. Cool, transfer into a 1 000 ml one-mark vo
43、lumetric flask, and add 35 ml of hydrochloric acid (4.3). Dilute to the mark with water and mix well.1 ml of this solution contains 1,000 mg of iron.4.16 Iron standard solution, 0,050 g/l.Transfer 10,0 ml of iron standard solution (4.15) into a 200 ml one-mark volumetric flask and add 10 ml of hydro
44、chloric acid (4.3). Dilute to the mark with water and mix well.Prepare this solution immediately prior to use.1 ml of this solution contains 0,050 mg of iron.4.17 Manganese standard solution, 1,000 g/l.Weigh 1 g 0,001 g of manganese (Mn 99,9 %) and transfer it into a 400 ml beaker. Add 30 ml of hydr
45、ochloric acid (4.4) and 2 ml of nitric acid (4.1). Cover with a watch glass and heat to initiate the reaction and complete dissolution. Add 0,5 ml of hydrogen peroxide (4.7). Cool, transfer into a 1 000 ml one-mark volumetric flask, and add 50 ml of hydrochloric acid (4.3). Dilute to the mark with w
46、ater and mix well.1 ml of this solution contains 1,000 mg of manganese. ISO 2015 All rights reserved 3BS ISO 7530-1:2015ISO 7530-1:2015(E)4.18 Manganese standard solution, 0,100 g/l.Transfer 10,0 ml of manganese standard solution (4.17) into a 100 ml one-mark volumetric flask and add 2,5 ml of hydro
47、chloric acid (4.3). Dilute to the mark with water and mix well.Prepare this solution immediately prior to use.1 ml of this solution contains 0,100 mg of manganese.4.19 Manganese standard solution, 0,010 g/l.Transfer 5,0 ml of manganese standard solution (4.17) into a 500 ml one-mark volumetric flask
48、 and add 12,5 ml of hydrochloric acid (4.3). Dilute to the mark with water and mix well.Prepare this solution immediately prior to use.1 ml of this solution contains 0,010 mg of manganese.5 ApparatusAll volumetric glassware shall be class A in accordance with ISO 385, ISO 648, or ISO 1042 as appropr
49、iate.Ordinary laboratory apparatus and the following.5.1 Atomic absorption spectrometer.WARNING The manufacturers recommendations should be closely followed and particular attention is drawn to the following safety points.a) The explosive nature of acetylene and regulations concerning its use.b) The need to shield the eyes of the operator from ultraviolet radiation by means of tinted glass.c) The need to keep the burner clear of deposits because a badly clogged burner can cause a flashback.d) The need to
