1、BSI Standards Publication BS ISO 7530-1:2015 Nickel alloys Flame atomic absorption spectrometric analysis Part 1: Determination of cobalt, chromium, copper, iron and manganeseBS ISO 7530-1:2015 BRITISH STANDARD National foreword This British Standard is the UK implementation of ISO 7530-1:2015. It s
2、upersedes BS 7455-1:1991, BS 7455-2:1991, BS 7455-3:1991, BS 7455-4:1991, BS 7455-5:1991 and BS 7455-6:1991, which are withdrawn. The UK participation in its preparation was entrusted to Technical Committee I/-, Miscellaneous standards materials and chemicals. A list of organizations represented on
3、this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2015. Published by BSI Standards Limited 2015 ISBN 978 0 580 84700
4、 4 ICS 77.120.40 Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 June 2015. Amendments issued since publication Date Text affectedBS ISO 7530-1:2015 ISO 2015
5、 Nickel alloys Flame atomic absorption spectrometric analysis Part 1: Determination of cobalt, chromium, copper, iron and manganese Alliages de nickel Analyse par spectromtrie dabsorption atomique dans la flamme Partie 1: Dtermination du cobalt, du chrome, du cuivre, du fer et du manganse INTERNATIO
6、NAL STANDARD ISO 7530-1 Second edition 2015-06-15 Reference number ISO 7530-1:2015(E)BS ISO 7530-1:2015ISO 7530-1:2015(E)ii ISO 2015 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2015, Published in Switzerland All rights reserved. Unless otherwise specified, no part of this publication may be
7、 reproduced or utilized otherwise in any 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 req
8、uester. ISO copyright office Ch. de Blandonnet 8 CP 401 CH-1214 Vernier, Geneva, Switzerland Tel. +41 22 749 01 11 Fax +41 22 749 09 47 copyrightiso.org www.iso.orgBS ISO 7530-1:2015ISO 7530-1:2015(E)Foreword iv Introduction v 1 Scope . 1 2 Normative references 1 3 Principle 1 4 Reagents 1 5 Apparat
9、us . 4 6 Sampling and sample preparation 4 7 Procedure. 5 7.1 Test portion 5 7.2 Blank test . 5 7.3 Dissolution 5 7.4 Determination of cobalt 5 7.4.1 Preparation of the test solution 5 7.4.2 Preparation of the calibration solutions 6 7.5 Determination of chromium 7 7.5.1 Preparation of the test solu
10、tion 7 7.5.2 Preparation of the calibration solutions 8 7.6 Determination of copper 9 7.6.1 Preparation of the test solution 9 7.6.2 Preparation of the calibration solutions 9 7.7 Determination of iron 11 7.7.1 Preparation of the test solution .11 7.7.2 Preparation of the calibration solutions .12 7
11、.8 Determination of manganese 13 7.8.1 Preparation of the test solution .13 7.8.2 Preparation of the calibration solutions .13 7.9 Adjustment of atomic absorption spectrometer . 15 7.10 Spectrometric measurements .15 7.11 Calibration curves .16 7.12 Expression of results .16 7.13 Precision 16 7.13.1
12、 General.16 7.13.2 Precision for cobalt .17 7.13.3 Precision for chromium 18 7.13.4 Precision for copper .18 7.13.5 Precision for iron 18 7.13.6 Precision for manganese 18 8 Test report 19 Annex A (normative) Procedures for checking the instrumental criteria .20 Bibliography .23 ISO 2015 All rights
13、reserved iii Contents PageBS ISO 7530-1:2015ISO 7530-1:2015(E) 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 normally carried out through ISO technical com
14、mittees. 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 the work. ISO collaborates closely with the
15、 International Electrotechnical Commission (IEC) on all matters of electrotechnical 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 t
16、he different types of ISO documents should be noted. This document was drafted in accordance 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.
17、ISO shall not be held responsible for identifying any or all such patent rights. Details 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 do
18、cument is information given for the convenience of users and does not constitute an endorsement. 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 Tr
19、ade (TBT) see the following URL: Foreword - Supplementary information The committee responsible for this document is ISO/TC 155, Nickel and nickel alloys. This second edition of ISO 7530- 1 cancels and replaces ISO 7530- 1:1 990, ISO 7530-2:1 990, ISO 7530-3:1 990, ISO 7530-4:1990, ISO 7530-5:1990,
20、and ISO 7530-6:1990, which have been technically revised. ISO 7530 consists of the following parts, 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 P
21、art 8: Determination of silicon content Part 9: Determination of vanadium contentiv ISO 2015 All rights reservedBS ISO 7530-1:2015ISO 7530-1:2015(E) Introduction This part of ISO 7530 describes five flame atomic absorption spectrometric methods for the determination of cobalt, chromium, copper, iron
22、, and manganese in nickel alloys. Although the methods are described independently, it is possible 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 7530-1:2015N
23、ickel alloys Flame atomic absorption spectrometric analysis Part 1: Determination of cobalt, chromium, copper, iron and manganese 1 Scope This part of ISO 7530 describes flame atomic absorption spectrometric methods for the determination of cobalt, chromium, copper, iron, and manganese in nickel all
24、oys which can be dissolved in the nitric- hydrochloric acids mixture specified. For each element, the method is applicable to the content range between 0,01 % and 4 %. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensab
25、le for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 385, Laboratory glassware Burettes ISO 648, Laboratory glassware Single-volume pipettes ISO 1042, Laboratory gla
26、ssware One-mark volumetric flasks 3 Principle Dissolution of a test portion in a nitrichydrochloric acids mixture, 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 so
27、lution after suitable dilution, if necessary, into an air/acetylene or a nitrous oxide/acetylene flame of an atomic 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 sol
28、utions of the same element. 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 4.1 Nitric acid, (HNO 3 ) 20= 1,41 g/ml. 4.2 Nitric acid solution, 1 + 1. Add 500 ml of nitric acid (4.1) to 5
29、00 ml of water. INTERNATIONAL ST ANDARD ISO 7530-1:2015(E) ISO 2015 All rights reserved 1BS ISO 7530-1:2015ISO 7530-1:2015(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 mix
30、ture. CAUTION This acid mixture is highly corrosive and unstable. Noxious gas (chlorine) is liberated on standing. It shall be 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). Thi
31、s mixture is not stable and should be prepared only as needed. 4.6 Strontium chloride solution. Transfer 113,5 g of strontium chloride hexahydrate (SrCl 2. 6H 2 O) 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, dilut
32、e 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 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
33、 is completely dissolved. 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 cobalt. 4.9 Cobalt standard solution, 0,02
34、5 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). 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 stan
35、dard 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), 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 volumetr
36、ic 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 chromium. 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
37、 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 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
38、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 reaction ceases. Heat to complete dissolution, boil to remove nitrogen oxides, and evaporate just to dryness. Cool, add 25 ml of hydrochloric acid (4.3), an
39、d 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 (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 soluti
40、on 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 volumetric 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
41、 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 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 immediate
42、ly 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 it 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 dissol
43、ution. 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 volumetric 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 m
44、g 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 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 con
45、tains 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 hydrochloric acid (4.4) and 2 ml of nitric acid (4.1). Cover with a watch glass and heat to initiate the reaction and complete dissolutio
46、n. 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 water and mix well. 1 ml of this solution contains 1,000 mg of manganese. ISO 2015 All rights reserved 3BS ISO 7530-1:2015ISO 7530-1:2
47、015(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 hydrochloric acid (4.3). Dilute to the mark with water and mix well. Prepare this solution immediately prior to use. 1 ml of this solut
48、ion 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 and add 12,5 ml of hydrochloric acid (4.3). Dilute to the mark with water and mix well. Prepare this solution immediately pri
49、or to use. 1 ml of this solution contains 0,010 mg of manganese. 5 Apparatus All volumetric glassware shall be class A in accordance with ISO 385, ISO 648, or ISO 1042 as appropriate. 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 shie
