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1、INTERNATIONAL STANDARD IS0 7530-4 First edition 1990-12-15 Nickel alloys - Flame atomic absorption spectrometric analysis - Part 4: Determination of copper content Alliages de nickel - Analyse par spectromtrie d absorption atomique dans la flamme - Partie 4: Dosage du cuivre Reference number IS0 753
2、0-4:1990(E) IS0 7530-4:1990(E) Foreword IS0 (the International Okganization 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 body intere
3、sted 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 Electrotechnica
4、l 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 a vote. I
5、nternational Standard IS0 7530-4 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 1: General requirements and sample dissolution - Par-l 2
6、: Determination of cobalt content - Part 3., Determination of chromium content - Part 4: Determination of copper content - Part 5: Defermination of iron content - Part 6: Deferminatior? of manganese content - Part 7: Determination of aluminium content - Part 8: Determination of silicon content - Par
7、t 9: Determination of VaDadiUm content 0 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 permission in writing from the publisher. International Organization f
8、or Standardization Case Postale 56 l CH-1211 Gen&ve 20 l Switzerland Printed In Switzerland ii -,-,- INTERNATIONAL STANDARD IS0 7530-4:1990(E) Nickel alloys - Flame atomic absorption spectrometric analysis - Part 4: Determination of copper content 1 Scope This part of IS0 7530 specifies a flame atom
9、ic ab- sorption spectrometric method for the determination of copper 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 6. The general requirements concerning the appar- atus, sampling, dissolution of the test sample,
10、 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 were vali
11、d. All standards are subject to revision, and p.arties 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 International Stan
12、dards. IS0 5725:1986, Precision of test methods - Defermi- nation of repeatability and reproducibilify for a stan- dard test method by inter-laboratory tests. IS0 7530-1:-l), Nickel alloys - Flame atomic ab- sorption spectrometric analysis - Part 1: General requirements and sample dissolution. 3 Pri
13、nciple 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 copper and com- parison with that of calibration solutions at a wave- len
14、gth of 324.8 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,.6H,O) to a 600 ml beaker, dissolve in 400 ml of hot water (50 “C to 60 “C), cool and
15、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 Copper, standard reference solution (1,000 g/l). Weigh, to the nearest 0,001 g, 1,000 g of copper metal of 99,9 % (m/m) minimum purity and transfer to a
16、 400 ml beaker. Add 50 ml of nitric acid (p2u = I,41 g/ml) diluted 1 -t 1 and allow to stand until the reaction ceases. Heat to complete dissol- ution, boil to remove oxides of nitrogen and evapor- ate just to dryness. Cool, add 25 ml of hydrochloric acid (p2c = I,18 g/ml) and evaporate just to dryn
17、ess. Add a further 25 ml of hydrochloric acid (p2c = I,18 g/ml) and repeat the evaporation. Dis- 1) To be published. 1 -,-,- IS0 7530-4:1990(E) solve the salts in 50 ml of hydrochloric acid (pzO = I,18 g/ml) diluted 1 i- 1, heating if necess- ary. Cool and transfer to a 1000 ml one-mark volumetric f
18、lask. Make up to the mark with water, mix and store in a polyethylene bottle. 4.3 Copper, standard solution (50 mg/l). Pipette 50 ml of the copper standard reference sol- ution (4.2) into a 1000 ml one-mark volumetric flask and add 50 ml of hydrochloric acid (20 = I,18 g/ml). Make up to the mark wit
19、h water, mix and store in a polyethylene bottle. strontium chloride solution (4.1) and 3 ml of hydrochloric acid (pso = I,18 g/ml). Make up to the mark with water and mix. 7.1.2.2 Secondary dilution for 0,4 % (m/m) to 4 % (nt/m) copper Pipette 10 ml of the solution from 7.1.1.2 into a 100 ml one-mar
20、k volumetric flask. Add 4 ml of strontium chloride solution (4.1) and 5 ml of hydrochloric acid (p2, = I,18 g/ml). Make up to the mark with water and mix. 7.2 Reagent blank solution 5 Apparatus The apparatus required is specified in clause 5 of is0 7530-I. 6 Sampling and sample preparation Refer to
21、clause 6 of IS0 7530-I. 7 Procedure 7.1 Preparation of test solution Proceed as directed in 7.1.1 to 7.1.4 of IS0 7530-I. 7.1.1 Primary dilutions 7.1.1.1 Initial dilution for 0,Ol % (m/m) to 0,lO % (m/m) copper Transfer the test solution (7.1) to a 100 ml one-mark volumetric flask. Add 4 ml of stron
22、tium chloride sol- ution (4.1). Make up to the mark with water and mix. Remove any products of hydrolysis by settlement and dry filtration or by centrifuging. 7.1.1.2 Initial dilution for 0,l % (m/m) to 4,0 % (n/m) copper Transfer the test solution (7.1) to a 500 ml one-mark volumetric flask. Add 20
23、 ml of hydrochloric acid (pzO = I,18 g/ml). Make up to the mark with water and mix. Remove any products of hydrolysis by settlement and dry filtration or by centrifuging. 7.1.2 Secondary dilutions 7.1.2.1 Secondary dilution for 0,l % (m/m) to 0,8 % (m/m) copper Pipette 50 ml of the solution from 7.1
24、.1.2 into a 100 ml one-mark volumetric flask. Add 4 ml of Carry out a blank test in parallel with the determi- nation, following the same procedure and using the same quantities of all the reagents. 7.3 Copper calibration solutions Using pipettes, transfer to each of five 100 ml one- mark volumetric
25、 flasks, 0 ml, 5 ml, 10 ml, 15 ml and 20 ml of copper standard solution (4.3). Add 4 ml of strontium chloride solution (4.1) and 5 ml of hydrochloric acid (ppO = I,18 g/ml). Make up to the mark with water and mix. 7.4 Calibration and determination 7.4.1 Atomic absorption measurements Proceed as dire
26、cted in 7.4.1 of IS0 7530-1, using a wavelength of 324,8 nm and an air-acetylene flame. 7.4.2 Preparation of calibration graphs Proceed as directed in 7.4.2 of IS0 7530-I 7.5 Number of determinations Carry out the determination at least in duplicate 8 Expression of results 8.1 Calculation Proceed as
27、 directed in 8.1 of IS0 7530-I. 8.2 Precision 8.2.1 Laboratory tests Twelve laboratories in six countries participated in the testing of this procedure using six samples of nominal composition given in table 1. -,-,- IS0 7530-4:1990(E) 8.2.2 Statistical analysis 8.2.2.2 One laboratory was rejected a
28、s a Cochran outlier and one was rejected as a straggler for sample 825. Two laboratories were rejected as Cochran stragglers, for samples 902 and 7013 re- 8.2.2.1 Results were treated according to IS0 5725 as described in 8.2.2 of IS0 7530-I. The results of this analysis are given in table2. spectiv
29、ely. 9 Test report Refer to clause 9 of IS0 7530-I Table 1 - Nominal composition of test samples Oh (/HZ) Sample Al co Cr cu Fe Mn Ni Si Ti 825 0,2 0,07 21 I,6 30 0,7 Remainder 0,4 I,1 902 0,4 0,05 5 0,04 48 0,4 Remainder 0,35 23 3920 0,15 2 19 (41 3 0,3 Remainder 03 3 2,3 3927 O,l 1 20 0,05 44 0,4
30、Remainder 078 0,6 7013 I,5 17 20 02 02 0,05 Remainder 097 2,4 7049 1 0,Ol 15 0,15 7 098 Remainder 0,3 23 - Table 2 - Results of statistical analysis Sample reference Mean % (m/m) 825 I,62 902 0,036 3920 0,ll 3927 0,054 7013 0,20 7049 0.16 Within-laboratory Between laboratory standard deviation I Rep
31、eatability 0,018 0,016 0,001 2 0,0012 0,005 0 0,008 0,0022 0,0024 0,0042 0,006 0,0054 0,008 Reproducibility 0,053 0,0035 0,016 0,0066 0,013 0,017 3 -,-,- IS0 7530-4:1990(E) UDC 669.245:543.422:546.56 Descriptors: nickel alloys, chemical analysis, determination of content, copper, atomic absorption spectrometric method. Price based on 3 pages