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1、INTERNATIONAL STANDARD IS0 7530-6 First edition 1990-12-15 Nickel alloys - Flame atomic absorption spectrametric analysis - Par-t 6: Determination of manganese content All/ages de nickel - Analyse par spectromtitrie d absorption atomique dans la flamme - Partie 6: Dosage du mangan8se Reference numbe
2、r IS0 7530-6: 1990(E) IS0 7530-6:1990(E) Foreword IS0 (the International Organization for Standardization) is a worldwide federation of national standards bodies (IS0 member bodies). The work of preparing International Standards is normally carried out through IS0 technical committees. Each member b
3、ody interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, govern- mental and non-governmental, in liaison with ISO, also take part in the work. IS0 collaborates closely with the International Elect
4、rotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an Inter- national Standard requires approval by at least 75% of the member bodies casting
5、 a vote. International Standard IS0 7530-6 was prepared by Technical Committee ISO/TC 155, Nickel and nickel alloys. IS0 7530 consists of the following parts, under the general title Nickel alloys - Flame atomic absorption spectrometric analysis: - Part I: Genera/ requirements and sample dissolution
6、 - Part 2: Determination of cobalt content - Part 3: Determination of chromium content - Part 4: Determination of copper content - Part 5: Determination of iron content - Part 6: Determination of manganese content - Part 7: Determination of aluminiwn content - Part 8: Determination of silicon conten
7、t - Part 9: Determination of vanadium content 6 IS0 1990 All rights reserved. No part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permisslon in writing from the publisher. international Organiz
8、ation for Standardization Case Postale 56 l CH-1211 Genbve 20 l Switzerland Printed in Switzerland ii INTERNATIONAL STANDARD IS0 7530-6:1990(E) Nickel alloys - Flame atomic absorption spectrometric analysis - Part 6: Determination of manganese content 1 Scope This part of IS0 7530 specifies a flame
9、atomic ab- sorption spectrometric method for the determination of manganese in the range of 0,Ol % (m/m) to 4 % (m/m) in nickel alloys. Typical compositions of some nickel alloys are given in IS0 7530-1, annex B. The general requirements concerning the appar- atus, sampling, dissolution of the test
10、sample, atomic absorption measurements, calculations and test report are given in IS0 7530-I. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this part of IS0 7530. At the time of publication, the editions indicated we
11、re valid. All standards are subject to revision, and parties to agreements based on this part of IS0 7530 are encouraged to investi- gate the possibility of applying the most recent edi- tions of the standards indicated below. Members of IEC and IS0 maintain registers of currently valid Internationa
12、l Standards. IS0 5725:1986, Precision of test methods - Determi- nation of repeatability and reproducibility for a stan- dard test method by inter-laboratory tests. IS0 7530-l:- ), Nickel alloys - Flame atomic ab- sorption spectrometric analysis - Part I: General requirements and sample dissolution.
13、 1) To be published. 3 Principle Dissolution of a test portion in acid and aspiration of the test solution into an air-acetylene flame of an atomic absorption spectrometer. Measurement of the absorbance of the resonance line energy from the spectrum of manganese and comparison with that of calibrati
14、on solutions at a wavelength of 279,5 nm. 4 Reagents In addition to the reagents listed in IS0 7530-1, the following special reagents are required. 4.1 Strontium chloride, solution Transfer 113,5 g of strontium chloride hexahydrate (SrCI,GH,O) to a 600 ml beaker, dissolve in 400 ml of hot water (50
15、C to 60 “C), cool and transfer to a 1000 ml one-mark volumetric flask. Make up to the mark with water and mix. The strontium chloride should be free of heavy metals. 4.2 Manganese, standard reference solution (1,000 g/l). Weigh, to the nearest 0,001 g, 1,000 g of manganese metal of 99,9 % (nz/m) min
16、imum purity and transfer to a 400 ml beaker. Add 30 ml of hydrochloric acid (20 = I,18 g/ml) diluted 1 i- 1 and 2 ml of nitric acid (ppe = I,41 g/ml). Heat to initiate the reaction and complete dissolution. Add 0,5 ml of hydrogen peroxide (4.4). Cool, transfer to a 1000 ml one-mark volumetric flask
17、and add 50 ml of hydrochloric acid 1 -,-,- IS0 7530- two for sample 902 and one for samples 3927 and 7049. Also two laboratories were rejected as Dixon stragglers for sample 7049. 9 Test report Refer to clause 9 of IS0 7530-I Sample 825 902 3920 3927 7013 7049 Sample reference 825 0,74 0,015 902 0.3
18、7 0,0032 3920 0,28 0,0038 3927 0,39 0,005o 7013 0,058 0,0007 7049 0,81 0,0048 Table 1 - Nominal composition of test samples % (m/m) Al 02 094 0,15 071 175 1 co 0,07 0,05 2 1 17 0,Ol Cr 21 li 20 20 15 1 cu I,6 0,04 I 0,1 0,05 02 0,15 Fe I Mn 1 Ni 30 0,7 48 0,4 3 T 033 44 074 092 0,05 7 08 Remainder R
19、emainder Remainder Remainder Remainder Remainder 1 Si 094 171 0,35 23 076 2,3 078 W-3 0,7 2,4 0,3 2,3 Ti I I Table 2 - Results of statistical analvsis I Within-laboratory Between Mean % (m/m) standard laboratory deviation standard Repeatability Reproducibility deviation I 0.027 0.043 0:017 0:009 0,0
20、093 0,011 0,016 0,014 0,0016 0,001 9 0,0074 0,013 0,088 0,050 0,028 0,048 0,0048 0,025 1 3 -,-,- IS0 7530-6:1990(E) _ _- ._- ._- _ UDC 669.245:543.422:546.711 Descriptors: nickel alloys, chemical analysis, determination of content, manganese, atomic absorption spectrometric method. Price based on 3 pages - -,-,-