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1、J IS JAPANESE I NDUSTRIAL STANDARD Translated and Published by Japanese Standards Association Method for optical emission spectrochemical analysis of aluminium and aluminium alloys ICs 77.120.10 Reference number : JIS H 1305 : 2005 (E) PROTECTED BY COPYRIGHT I I s Copyright Japanese Standards Associ
2、ation Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 08:30:17 MDTNo reproduction or networking permitted without license from IHS -,-,- H 1305 : 2005 Foreword This translation has been made based on the original Japanese Industri
3、al Standard revised by the Minister of Economy, Trade and Industry through deliberations at the Japanese Industrial Standards Committee, as the result of proposal for revision of Japanese Industrial Standard submitted by Japan Aluminium Association (JAA)/ Japanese Standards Association (JSA) with th
4、e draft being attached, based on the provision of Article 12 Clause 1 of the Industrial Standardization Law applicable to the case of revision by the provision of Article 14. Consequently JIS H 1305 : 1976 is replaced with this Standard. Date of Establishment: 1965-10-01 Date of Revision: 2005-03-20
5、 Date of Public Notice in Official Gazette: 2005-03-22 Investigated by: Japanese Industrial Standards Committee Standards Board Technical Committee on Non-Ferrous Metals JIS H 1305 : 2005, First English edition published in 2005-10 Translated and published by: Japanese Standards Association 4-1-24,
6、Akasaka, Minato-ku, Tokyo, 107-8440 JAPAN In the event of any doubts arising as to the contents, the original JIS is to be the final authority. O JSA 2005 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electroni
7、c or mechanical, including photocopying aiid microfilm, without permission in writing from the publisher, Printed in Japan KWAT PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 0
8、3/15/2007 08:30:17 MDTNo reproduction or networking permitted without license from IHS -,-,- H 1305 : 2005 Contents Page 1 1 1 1 2 3 3 3 3 3 4 5 5 5 7 8 9 12 1 2 3 4 5 6 7 7.1 7.2 7.3 8 9 10 11 12 13 14 Scope Normative reference General requirements . Elements to be determined and concentration rang
9、e . Definitions Summary . Apparatus Emission spectrophotometer Adjustment of apparatus Apparatus performance criteria Standard substance, sample for calibration of working curve and analytical sample . Preparation for sample . Operation Preparation of working curve Test of working curve . Calibratio
10、n of working curve . Calculation Annex (normative) Method for optical emission spectrochemical analysis of aluminium and aluminium alloys (in the case using an optical emission spectrometer with an atmospheric air discharge luminescence stand) (i) PROTECTED BY COPYRIGHT Copyright Japanese Standards
11、Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 08:30:17 MDTNo reproduction or networking permitted without license from IHS -,-,- JAPANESE INDUSTRIAL STANDARD JIS H 1305 : 2005 Method for optical emission spectrochemi
12、cal analysis of aluminium and aluminium alloys 1 Scope This Japanese Industrial Standard specifies the method for optical emission spectrochemical analysis with an argon-atmosphere discharge luminescence stand of aluminium and aluminium alloys. This Standard applies to the determination of component
13、s given in table 1. In addition, the method for optical emission spectrochemical analysis with an at- mospheric air discharge luminescence stand of aluminium and aluminium alloys is as given in annex. 2 Normative reference The following standard contains provisions which, through reference in this t
14、ext, constitutes provisions of this Standard. The most recent edi- tions of the standard (including amendments) indicated below shall be applied. JIS Z 2611 General rules for photoelectric emission spectrochemical analysis of metal materials 3 General requirements sis shall conform to JIS Z 2611. Th
15、e general requirements used in common for analy- 4 Elements to be determined and concentration range determined and concentration range shall be as given in table 1. The elements to be PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS
16、Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 08:30:17 MDTNo reproduction or networking permitted without license from IHS -,-,- 2 H 1305 : 2005 Manganese Magnesium Table 1 Elements to be determined and concentration Unit: o/o (m/m) 0.001 or over up to and incl. 3.0 0.001 or ove
17、r up to and incl. 12.0 I Elements to be determined I Concentration range I Lead Zirconium I Silicon I 0.001 or over up to and incl. 25.0 I 0.002 or over up to and incl. 1.0 0.001 or over up to and incl. 0.50 I Iron I 0.001 or over up to and incl. 2.5 I Beryllium I Copper I 0.001 or over up to and in
18、cl. 7.0 I 0.001 or over up to and incl. 0.10 I Chromium I 0.001 or over up to and incl. 0.50 I I Zinc I 0.001 or over up to and incl. 12.0 I I Titanium I 0.001 or over up to and incl. 0.50 I I Nickel I 0.001 or over up to and incl. 3.0 I I Bismuth I 0.001 or over up to and incl. 1.0 I I Gallium I 0.
19、002 or over up to and incl. 0.10 I I Vanadium I 0.002 or over up to and incl. 0.25 I I Tin I 0.001 or over up to and incl. 6.0 I I Boron I 0.001 or over up to and incl. 0.25 I range Definitions For the purpose of this Standard, the following definitions apply. metallurgical conditions conditions suc
20、h as the rate of solidification of a molten metal sample which affects the form of metallographic structure and deposit and inclusion and the emission intensity measurements even if the chemical composition of a analytical sample is the same, the heating temperature when heat treatment and rolling a
21、nd forging are performed emission intensity measurements the emission intensity of the component to be determined by an optical emission spectrochemical analysis method in the case of an emission intensity method, or the ratio of the emission intensity of the component to be determined to the emissi
22、on intensity of an internal stan- dard element (generally aluminium) in the case of an intensity ratio method percentage content ratio method the method to obtain the quantitative value of the component by canceling the correction after obtaining the corrected per- centage content ratio of the compo
23、nent from the emission intensity ratio of the component in the sample by correcting the standard value of the component to be determined to be the percentage content ratio to the percentage content of aluminium and by obtaining the relation curve of the emission intensity ratio to the corrected perc
24、entage content ratio to make the working curve when pre- paring the working curve using the aluminium standard substance for instru- mental analyses, etc. PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Win
25、g, Bernie Not for Resale, 03/15/2007 08:30:17 MDTNo reproduction or networking permitted without license from IHS -,-,- 3 H 1305 : 2005 6 After cutting or machining a sample, grind it to finish so that it be- comes planate, attach it to the sample holder of an emission spectrophotometer to make it b
26、e an electrode, use tungsten for a counter electrode, discharge between the both electrodes by applying voltage, obtain spectral lines by a spectrometer, and measure the spectral line intensity of the component to be determined. Summary 7 Apparatus 7.1 Emission spectrophotometer The emission spectro
27、photometer shall be in accordance with JIS Z 2611 and as follows: a) Counter electrode For the counter electrode, the electrode obtained by forming the head of a tungsten rod of 0.5 mm to 7 mm in diameter so as to have the shape of the truncated cone with the conical shape of 20“ to 120“ or the plan
28、e surface of 1 mm in diameter shall be used. b) Argon Argon of not less than 99.99 5 % (m/m) in purity with few oxygen, hy- drocarbon and other impurities shall be used(1). Note (I) The purity has a significant effect on the quantitative value. That is, be careful since the stability of repeated mea
29、surements is lowered, the measurements of emission intensity are decreased due to poor discharge, etc. by using argon with many impurities. 7.2 Adjustment of apparatus The adjustment of apparatus shall be performed in accordance with JIS Z 2611. However, for the pressure inside the spectrometer, the
30、 optimal conditions for each analyzer shall be applied. 7.3 Apparatus performance criteria The apparatus performance criteria shall be as follows: a) For the emission spectrophotometer adjusted in accordance with 7.2, the analy- sis conditions (analytical lines, excitation conditions, photometry con
31、ditions, etc.) shall be set so that repeatability and sensitivity may become suitable. b) Repeatability shall be not more than the upper limit of the relative standard deviation specified in table 2. However, it shall not be applied to an Al-Si sys- tem hypereutectic alloy sample (2). In addition, t
32、he relative standard deviation refers to the value calculated ac- cording to the following formula after obtaining the quantitative value for ev- ery measurement by measuring the emission intensity of a homogeneous sample, for example the aluminium standard substance for instrumental analyses in ac-
33、 cordance with clause 10 at least 6 times. o RSD = y x 100 X where, RSD : o: - X : relative standard deviation standard deviation of the quantitative value ob- tained by measuring the same sample repeatedly average value of the quantitative value obtained by measuring the same sample repeatedly PROT
34、ECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 08:30:17 MDTNo reproduction or networking permitted without license from IHS -,-,- 4 H 1305 : 2005 Percentage content of c
35、omponent 7c (mm) Note (2) For Si in Al-Si system hypereutectic alloys such as ACSA, ACSB, ADC14, although this Standard is not applied since it is difficult to get a ho- mogeneous standard substance, actual conditions should be grasped by increasing the number of times of discharge, etc. c) The inve
36、stigation of the apparatus performance criteria shall be performed at regular intervals, and it shall be performed without fail when the analysis con- ditions are changed, or when the condition of the apparatus is changed owing to repair, adjustment, etc. Table 2 Upper limit of relative standard dev
37、iation Upper limit of relative standard deviation I Under 0.01 I 3 I 0.01 or over to and excl. 0.1 I 2 I 0.1 or over I 1 8 Standard substance, sample for calibration of working curve and ana- lytical sample The standard substance, sample for calibration of working curve and analytical sample shall b
38、e as follows: Aluminium standard substance for instrumental analyses It shall be the standard substance used for preparation of the working curve and calibration of the working curve, which is homogeneous, and of which the metallurgical conditions and chemical composition are closely analogous (3) t
39、o those of the analytical sample, and of which the standard value of the component to be de- termined is determined by using the chemical analysis method specified in the International Standard and Japanese Industrial Standard, etc. In addition, when there is no public standard, the standard value s
40、hall be determined by using the chemical analysis method which is technologically con- firmed at the analysis site, and documented. Note (3) When a sufficient number of standard substances which satisfy the percentage content range to be required cannot be not obtained at the time of preparation of
41、the working curve, the binary system alloy stan- dard substance comprised of aluminium and the component to be de- termined may be used. Sample for calibration of working curve It shall be the sample used on a day-to-day basis in order to confirm and calibrate the working curve, and if the sample is
42、 sufficiently homogeneous, the metallurgical conditions and chemical composition ratio in the sample may not be closely analogous to those of the analytical sample. This sample may be used for judgment of the apparatus per- formance criteria. Analytical sample The analytical sample has a molten meta
43、l sample and a product sample. The molten metal sample shall be sampled from the molten metal in accordance with JIS Z 2611, and the section for analysis of 35 mm to 60 mm in diameter and 5 mm to 10 mm in thickness shall be used. The product PROTECTED BY COPYRIGHT Copyright Japanese Standards Associ
44、ation Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 08:30:17 MDTNo reproduction or networking permitted without license from IHS -,-,- 5 H 1305 : 2005 sample shall be the semi-finished product such as a piece, a lump of aluminiu
45、m, or the sample cut out from the product, of which the section for analysis is homogeneous and has the representative composition of the product. When the sample cut out is comprised of many small pieces or the segregation of the component to be determined is large, the samples shall be remelted in
46、 a small smelter, and cast into the mould as is the case with the molten metal. However, in the case of elements of large melting loss, sufficient attention should be given to the temperature, time, etc. 9 Preparation for sample For the sample, the sample taken in accordance with 8 c) shall be machi
47、ned, and shall be prepared so that the surface of analysis becomes smooth. Especially for the molten metal sample, the component segregation section of the sample surface shall be shaved off. For other samples, the oxidized section and contaminated section of the surface shall be shaved off. The sam
48、ple after machining shall have the plane which covers the hole on the sample holder of the analyzer suf- ficiently and does not cause gas leak, and the thickness of 3 mm or more(4). Note (4) When the thickness becomes 3 mm or less, the heat capacity becomes small, and the stability of emission intensity and the precision of an analytical value lower. In such a case, the circular plate or square plate which is 5 mm to 10 mm in thickness and has the almost the same size as that of the sample shall be stuck to the reverse side of the analysis surface of the sample. It is necessary