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1、STD-JIS H LObS-ENGL 1997 Li733b08 05482b7 175 J IS . r JIS HI 1069 : 1997 JAPANESE I NDUSTRIAL STANDARD Translated and Published by Japanese Standards Association Methods for determination of cadmium in copper and copper alloys ICs 77.120.30 Descriptors : copper, copper alloys, cadmium, determinatio
2、n of content Reference number : JIS H 1069 : 1997 (E) 7 s Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:21:59 MDTNo reproduction or networking permitted without license from IHS -,-,-
3、STD-JIS H LObS-ENGL 1777 m Li733b08 05Li82bB 02L = H 1069 : 1997 This translation has been made based on the original Japanese Industrial Standard established by the Minister of International Trade and Industry through deliberations at Japanese Industrial Standards Committee in accordance with the I
4、ndustrial Standardization Law: Date of Establishment: 1997-05-20 Date of Public Notice in Official Gazette: 1997-05-20 Investigated by: Japanese Industrial Standards Committee Divisional Council on Non-Ferrous Metals c d I JIS H 1069 : 1997, First English edition published in 1997-12 Translated and
5、published by: Japanese Standards Association 4-1-24, 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. 0 JSA 1997 All rights reserved. Unless otherwise specified, no part of this publication may be reproduc
6、ed or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from the publisher. Printed in Japan Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing,
7、Bernie Not for Resale, 03/13/2007 08:21:59 MDTNo reproduction or networking permitted without license from IHS -,-,- 4 STD-JIS H LObS-ENGL 1797 Li933b08 05482b7 Tb W JAPANESE INDUSTRIAL STANDARD JIS H 1069 1 1997 Methods for determination of cadmium in copper and copper alloys Introduction IS0 5960,
8、 Copper alloys-Determination of cadmium content - Flame atomic absorption spectrometric method published as the first edition in 1984 is the corresponding International Standard to this Japanese Industrial Standard which specifies the corresponding parts of IS0 (Atomic absorption spectrometric metho
9、d) without any modification -in technical content. The trioctylamine extraction atomic absorption spectrometric method which has no the corresponding International Standard is specified as Japanese Industrial Standard. 1. Scope This Japanese Industrial Standard specifies the methods for determinatio
10、n of cadmium in copper and copper alloys (rolled coppers). Remarks 1. Normative reference to this Standard is shown as follows. JIS H 1012 General rules for chemical analysis of copper and copper alloys 2. The corresponding International Standard is as follows. IS0 5960 :1984 Copper alloys - Determi
11、nation of cadmium content- Flame atomic absorption spectrometric method 2. General requirements General requirements common to methods for determina- tion shall be in accordance with JIS H 1012. 3. Division of determination methods The method for determination of cadmium content shall be in accordan
12、ce with either of the following. (i) Trioctylamine extraction atomic absorption spectrometric method This method is applicable to the sample of copper content is not less than 99.90 %(mim), cadmium content 0.000 02 %(m/m)or over up to and including 0.000 3 %(mim). (2) Atomic absorption spectrometric
13、 method This method is applicable to the sample of cadmium content 0.000 5 %(mim) or over up to and including 2.0 %(m/m). 4. Trioctylamine extraction atomic absorption spectrometric method 4.1 Summary Dissolve the sample with nitric acid, add sulfuric acid and heat to re- move nitric acid by generat
14、ing the white fume with sulfuric acid. Add hydrochloric acid and extract cadmium chloride complex formed with 4-methyl-2-pentanone contained trioctylamine. Atomize the organic phase into an air-acetylene flame of the atomic ab- Copyright Japanese Standards Association Provided by IHS under license w
15、ith JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:21:59 MDTNo reproduction or networking permitted without license from IHS -,-,- 2 H 1069 : 1997 sorption spectrometer and measure the absorbance. Reagents The reagents shall be as follows. Hydrochloric acid (l+
16、l) Nitric acid (l+l) Sulfuric acid (1 +i) Extracting reagent Add 4-metyl-2-penthanone (I) to 2 ml of triocthylamine and make up the volume to 100 ml. 4-metyl-Z-pentanone Butyl acetate Standard cadmium solution (1 not less than 99.9 %(m/m) and place it in a beaker (200 ml), cover the beaker with a wa
17、tch glass, add 25 ml of nitric acid (l+l) and heat gently to dissolve the sample. After cooling to ordinary temperature, remove the watch glass after rinsing rear bottom of it and inside wall of the beaker with water. Transfer the solution into a 1 O00 ml volumetric flask with water, dilute to the m
18、ark with water and make the stock solution (1 mgCd/ml). The needed amounts of the standard cadmium solution A shall be prepared fleshly from this stock solution with 20 times correct dilution by water at each time before use. (5) Standard cadmium solution B (5ugCd/ml) The needed amounts of the stand
19、ard cadmium solution B shall be prepared fleshly from above standard cadmium solu- tion A (4) with 10 times correct dilution by water at each time before use. i Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for
20、 Resale, 03/13/2007 08:21:59 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS H LObS-ENGL I777 4933b08 0548273 479 5 H 1069 : 1997 5 . 3 Test portion Test portion shall be 1.0 g of the sample. 5 . 4 Procedure 5.4.1 shall be given by the following procedures. Preparat
21、ion of the sample solution The preparation of the sample solution (i) Weigh the sample and transfer into a tetrafluoroethylene resin beaker (200 mi) or a polyethylene beaker (200 mi). (2) Cover the beaker with a tetrafluoroethylene resin lid or polyethylene lid, add 40 ml of mixed acid (1) and heat
22、gently to dissolve the sample. (3) After cooling to ordinary temperature, remove the lid after rinsing rear bottom of it and inside wall of the beaker with water. Transfer the solution into a 100 ml, 1 O00 ml, 2 O00 ml volumetric flasks with water in accordance with cadmium contents; 0.000 5 %(mim)
23、or over to and excluding 0.05 %(m/m), 0.05 %(m/m) or over to and excluding 0.5 %(m/m), 0.5 %(m/m) or over up to and including 2 %(m/m) respec- tively. Dilute the solutions of each flask to the mark with water. 5.4.2 Preliminary measurement Preliminary measurement shall be given by the following proc
24、edures. (1) Measurement of the absorbance Aspirate a portion of the solution obtained in 5.4.1 (3) into the air - acetylene flame of the atomic absorption spectrometer which is adjusted to zero absorbance in relation to water and measure the absorbance of it at a wavelength 228.8 nm. (2) Blank test
25、of preliminary measurement The absorbance of the solution without adding the standard cadmium solution which is obtained according to procedures of establishing the working curve in (3) shall be applicable to the absorbance of the blank test of the preliminary measurement. (3) Establish the working
26、curve (a) Take the copper solution 5.2 (3), the standard cadmium solution A 5.2 (4) and the standard cadmium solution B 5.2 ( 5 ) into 9 flasks ( refer to Table l), 7 flasks (refer to Table 2) and 5 flasks (refer to Table 3) of 100 ml volumetric flasks as shown in Table 1 to Table 3, depending on th
27、e expected cadmium contents in the sample. Dilute to the mark with water and mix. (b) In parallel with the same procedures of the sample solution, aspirate a part of above solution into an air-acetylene flame of the atomic absorption spectrometer which is adjusted to zero absorbance in relation to w
28、ater and measure the ab- sorbance of it at a wavelength 228.8 nm. Carry out establishing the correlation curve by plotting the absorbance values obtained against the mass of cadmium and by parallel displacement of the line so as to pass through the origin of graph and use it as working curve. Copyri
29、ght Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:21:59 MDTNo reproduction or networking permitted without license from IHS -,-,- STDmJIS H LObS-ENGL I997 4933b08 0548274 325 D Standard Cd Solut
30、ion A 5.2 (4)1 ml O 1 2 4 6 8 10 6 H 1069 : 1997 Mass of Cd Cu solution Mass Corresponding 5.2 (3)1 of Cu Cd contents in the sample IJg ml g % (mlm) O 5 0.1 O 50 5 0.1 0.05 100 5 o. 1 0.1 200 5 o. 1 0.2 300 5 o. 1 0.3 400 5 o. 1 0.4 500 5 0.1 0.5 I (4) Convert the difference calculated by subtractin
31、g the absorbance obtained in (2) from the absorbance obtained in (1) into the corresponding mass of cadmium by using the working curve established in (3). This is used as value of the preliminary measure. Table 1 Sampling volume of copper solution and standard cadmium solution in the case of cadmium
32、 contents between 0.000 5 % (dm) and 0.06 % (Mio) Standard Cd solution B 5.2 (511 ml O 1 2 6 10 15 20 Standard Cd solution ml A 5.2 (411 6 10 Mass of Cd ug O 5 10 30 50 75 100 300 500 Cu solution 5.2 (311 ml 50 50 50 50 50 50 50 50 50 Mass of Cu g Corresponding Cd contents in the sample %(m/m) O 0.0
33、00 5 0.001 0.003 0.005 0.007 5 0.010 0.030 0.050 Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:21:59 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS H
34、 LOb7-ENGL 1777 4733b8 0548275 2bL Standard Cd Solution A 5.2 (41 ml O 5 10 15 20 7 H 1069 : 1997 Mass of Cd Cu solution Mass Corresponding 5.2 (3)1 of Cu Cd contents in the sample Lig ml g % (m/m) O 2.5 0.05 O 250 2.5 0.05 0.5 500 2.5 0.05 1.0 750 2.5 0.05 1.5 1 O00 2.5 0.05 2.0 5.4.3 Preparation o
35、f bracket solution Prepare 2 types of the bracket solution in ac- cordance with the procedure (3) (a) in 5.4.2. For the volumes of standard cadmium solu- tion A 5.2 (4) and solution B 5.2 (5), take the optimum volumes of cadmium contents (ug) so as to be rather much amount and rather little amount o
36、f cadmium contents re- spectively than the value (m) obtained in the preliminary measurement of 5.4.2(4). 5.4.4 Measurement of absorbance Aspirate a part of the solution obtained in 5.4.1(3) and 2 type solutions prepared in 5.4.3 into an air-acetylene flame of the atomic absorp- tion spectrometer wh
37、ich is adjusted to zero absorbance in relation to water and measure the absorbance of it at a wavelength 228.8 nm. 5.5. Blank test Weigh copper 5.2 (2) as much as taken in 5.4.1 (i), transfer into a tetrafluoroethylene resin beaker (200 mi) or polyethylene beaker (200 mi). In parallel with the same
38、procedures of the sample solution in accordance with 5.4.1 (2) to 5.4.2 (1) hereinafter, and convert difference subtracted the absorbance obtained in 5.4.2 (2) from the absorbance obtained by above procedures into the corresponding mass of cadmium by using the working curve established in 5.4.2 (3).
39、 5.6. Calculation The cadmium contents in the sample shall be given by the following e qua tion. c, +(e, -C,)x -c3 x 100 A2 -4 100 B Cd = rn x _ x 1000000 where, Cd : cadmium contents in the sample %(m/m) C, : cadmium contents in the bracket solution which is prepared less than the preliminary analy
40、tical value in 5 . 4 . 3 ( C, : cadmium contents in the bracket solution which is prepared more than the preliminary analytical value in 5 . 4 . 3 (ug) Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale,
41、03/13/2007 08:21:59 MDTNo reproduction or networking permitted without license from IHS -,-,- 8 H 1069 : 1997 A, : absorbance of the sample solution obtained in 5.4.4 A, : absorbance corresponded to C, obtained in 5.4.4 4 : absorbance corresponded to C, obtained in 5.4.4 C, : cadmium contents in the
42、 blank test obtained in 5.5 (ug) rn : test portion (g) B : volume of the volumetric flask used in 5.4.1 (3) (mi). Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:21:59 MDTNo reproduction
43、 or networking permitted without license from IHS -,-,- h t m m 4 STD-JIS H LOb7-ENGL 1777 Li733bD O548277 034 9 H 1069 : 1997 (Reference) c E -u .- 4 % 3 B al * C al Y 0 h I II 6 a c h tn al R R U -u - e v I I ) x - - L R R s 1 II o 0 1 O I O O0 O al P m u h i v O O Copyright Japanese Standards Ass
44、ociation Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:21:59 MDTNo reproduction or networking permitted without license from IHS -,-,- 1 0 . H 1069 : 1997 (Reference) 2 E o 1 d =I cd vi E Copyright Japanese Standards Associat
45、ion Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:21:59 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS H LObS-ENGL 1997 4733b08 05Li8279 907 Errata for JIS (English edition) are printed in S
46、tandardization Journal, published monthly by the Japanese Standards Association, and also provided to subscribers of TIS (English edition) in Monthly information. Errata will be provided upon request, please contact: Standardization Promotion Department, Japanese Standards Association 4-1-24, Akasak
47、a, Minato-ku, Tokyo, 107 JAPAN TEL. 03-3583-8002 FAX. 03-3583-0462 Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:21:59 MDTNo reproduction or networking permitted without license from IHS -,-,-