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1、INTERNATIONAL STANDARD IS0 7530-5 First edition 1990-12-15 Nickel alloys - Flame atomic absorption spectrometric analysis - Part 5: Determination of iron content Ailiages de nickel - Analyse par spectromtrie d absorption atomique dans la flamme - Partie 5: Dosage du fer IS0 7530-5:1990(E) Foreword I
2、S0 (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 body interested in a subject for which a technical c
3、ommittee 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 Electrotechnical Commission (IEC) on all matters of elec
4、trotechnical 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. International Standard IS0 7530-5 was pre
5、pared 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 specfromefric analysis: - Part 1: General requirements and sample dissolution - Part 2: Determination of cobalt content - Part
6、3: Determination of chromium content - Part 4: Determination of copper content - Parf 5: Determination of iron content - Parf 6: Determination of manganese content - Part 7: Determination of aluminium content - Part 8: Determination of silicon content - Part 9: Determination of vanadium content 0 IS
7、0 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 Organization for Standardization Case Postale 56 l CH-121
8、1 Geneve 20 l Switzerland Printed in Switzerland ii INTERNATIONAL STANDARD IS0 75304:1990(E) Nickel alloys - Flame atomic absorption spectrometric analysis - Part 5: Determination of iron content 1 scope This part of IS0 7530 specifies a flame atomic ab- sorption spectrometric method for the determi
9、nation of iron 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 sample, atomic absorption measurements, calculations and test
10、 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 valid. All standards are subject to revision, and parties
11、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 Standards. IS0 5725:1986, Precision of test methods - Deter
12、mi- nation of repeatability and reproducibilify for a stan- dard tesf method by infer-laboratory tests. IS0 7530-l:- ), Nickel alloys - Flame atomic ab- sorption spectrometric analysis - Pat-f I: General requirements and sample dissolution. 3 Principle Dissolution of a test portion in acid and aspir
13、ation 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 iron and compari- son with that of calibration solutions at a wavelength of 248,3 nm. 4 Reagents In addition to the reagents li
14、sted 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 “C to 60 “C), cool and transfer to a 1000 ml one-mark volumetric flask. Make up t
15、o the mark with water and mix. The strontium chloride should be free of heavy metals. 4.2 iron, standard reference solution (1,000 g/l). Weigh, to the nearest 0,001 g, 1,000 g of iron metal of 99,9 % (m/m) minimum purity and transfer to a 400 ml beaker. Add 30 ml of hydrochloric acid (pPO = 1,18 g/m
16、l) diluted 1 + 1. Heat to initiate the reaction and complete dissolution. Cool to about 50 “C, cautiously add 1 ml of hydrogen peroxide (4.4) and bring to the boil to oxidize the iron. Cool, transfer to a 1000 ml one-mark volumetric flask and add 35 ml of hydrochloric acid (pPO = I,18 g/ml). 1) To b
17、e published. 1 -,-,- IS0 7530&1990(E) Make up to the mark with water, mix and store in a polyethylene bottle. 4.3 Iron, standard solution (50 mg/l). Pipette 50 ml of the iron standard reference solution (4.2) into a 1000 ml one-mark volumetric flask and add 50 ml of hydrochloric acid (p2c = I,18 g/m
18、l). Make up to the mark with water, mix and store in a polyethylene bottle. 4.4 Hydrogen peroxide, 300 g/l, (p2c = I,1 g/ml). 5 Apparatus The apparatus required is specified in clause 5 of IS0 7530-I. 6 Sampling and sample preparation Refer to clause 6 of IS0 7530-I. 7 Procedure 7.1 Preparation of t
19、est solution Proceed as directed in 7.1.1 to 7.1.4 of IS0 7530-I. Add 0,25 ml of hydrogen peroxide (4.4) in the final dissolution of the salts. 7.1.1 Primary dilutions 7.1.1.1 initial dilution for 0,Ol % (m/m) to 0,lO % (m/m) iron Transfer the test solution (7.1) to a 100 ml one-mark volumetric flas
20、k. Add 4 ml of strontium 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 % (m/m) iron Transfer the test solution (7.1) to a 500 ml one-mark volume
21、tric flask. Add 20 ml of hydrochloric acid (20 = 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/nz) to 0,8 % (m/m) iron Pipette 50 ml of the s
22、olution from 7.1.1.2 into a 100 ml one-mark volumetric flask. Add 4 ml of strontium chloride solution (4.1) and 3 ml of hydrochloric acid (p2c = 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 % (m/m) iron Pipette 10 ml of the solution from 7.1.1.2
23、 into a 100 ml one-mark volumetric flask. Add 4 ml of strontium chloride solution (4.1) and 5 ml of hydrochloric acid (p2c = I,18 g/ml). Make up to the mark with water and mix. 7.2 Reagent blank solution Carry out a blank test in parallel with the determi- nation, following the same procedure and us
24、ing the same quantities of all the reagents. 7.3 Iron calibration solutions Using pipettes, transfer to each of five 100 ml one- mark volumetric flasks, 0 ml, 5 ml, 10 ml, 15 ml and 20 ml of iron standard solution (4.3). Add 4 ml of strontium chloride solution (4.1) and 5 ml of hydrochloric acid (p2
25、c = 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 directed in 7.4.1 of IS0 7530-1, using a wavelength of 248,3 nm and an air-acetylene flame. 7.4.2 Preparation of calibration graphs Proceed as directed in 7.4.2 o
26、f 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 directed in 8.1 of IS0 7530-I. 8.2 Precision 8.2.1 Laboratory tests Eleven laboratories in six countries participated in the testing of this procedure usin
27、g two samples of nominal composition given in table 1. 2 -,-,- IS0 7530-5:1990(E) 8.2.2 Statistical analysis 8.2.2.2 One laboratory was rejected as a Cochran outlier for sample 3920. One laboratory was re- jected as both a Cochran and a Dixon outlier for sample 7013. 8.2.2.1 Results were treated acc
28、ording to IS0 5725 as described in 8.2.2 of IS0 7530-I. The results of this analysis are given in table2. 9 Test report Refer to clause 9 of IS0 7530-I. Sample Table 1 - Nominal composition of test samples % (m/m) Al co Cr CU Fe Mn Ni Si Ti 3920 0,15 2 19 O,l 3 0,3 Remainder W-3 ,233 7013 1,5 17 20
29、02 02 0,05 Remainder 0,7 2,4 Table 2 - Results of statistical analysis Within-laboratory Between Sample reference Mean % (m/02) standard laboratory Repeatability Reproducibility deviation standard deviation 3920 3,00 0,029 0,048 0,083 0,16 7013 0,21 0,0023 0,0063 0,007 0,019 -,-,- IS0 7530-5:1990(E) UDC 669.245:543.422:546.72 Descriptors: nickel alloys, chemical analysis, determination of content, iron, atomic absorption spectrometric method. Price based on 3 pages
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