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1、J IS JAPANESE INDUSTRIAL STANDARD Translated and Published by Japanese Standards Association Methods for determination of arsenic in copper and copper alloys ICs 77.120.30 Reference number : JIS H 1059 : 2005 (E) PROTECTED BY COPYRIGHT 9s Copyright Japanese Standards Association Provided by IHS unde
2、r license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 19:59:26 MDTNo reproduction or networking permitted without license from IHS -,-,- H 1059 : 2005 Foreword This translation has been made based on the original Japanese Industrial Standard revised by the
3、 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 Copper and Brass Association (JCBA)/Japanese Standards Association (JSA) with the draft being attac
4、hed, 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 1059 : 1987 is replaced with this Standard. Attention is drawn to the possibility that some parts of this Standard may confli
5、ct with a patent right, application for a patent after opening to the public, utility model right or application for registration of utility model after opening to the public which have technical properties. The relevant Minister and the Japanese Industrial Standards Committee are not responsible fo
6、r identifying the patent right, application for a patent after opening to the public, utility model right or application for registration of utility model after opening to the public which have the said technical properties. Date of Establishment: 1987-11-01 Date of Revision: 2005-03-20 Date of Publ
7、ic Notice in Official Gazette: 2005-03-22 Investigated by: Japanese Industrial Standards Committee Standards Board Technical Committee on Non-Ferrous Metals JIS H 1059 :2005, First English edition published in 2005-09 Translated and published by: Japanese Standards Association 4-1-24, Akasaka, Minat
8、o-ku, Tokyo, 107-5440 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, iio part of this publication may be reproduced or utilized in any forin or by any ineaiis, electronic or mecha
9、nical, includiiig photocopying and microfilm, without permission in writing from the publisher. Printed in Japan KKIAT PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007
10、 19:59:26 MDTNo reproduction or networking permitted without license from IHS -,-,- H 1059 : 2005 Contents Page Introduction . 1 2 3 4 5 5.1 5.2 5.3 5.4 5.5 5.6 5.7 6 6.1 6.2 6.3 6.4 6.5 6.6 6.7 Scope Normative reference General matters . Classification of determination methods . Molybdoarsenate ext
11、raction absorptiometry Summary . Reagents Weighing out amount of sample . Operation Blank test Preparation of working curve Calculation Bromide extraction separation molybdoarsenate blue absorptiometry . Summary . Reagents Weighing out amount of sample . Operation Blank test Preparation of working c
12、urve Calculation Annex (informative) Comparison table between JIS and corresponding International Standard . 1 1 1 1 1 2 2 2 2 2 3 3 4 4 4 4 5 5 6 7 7 9 (i PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wi
13、ng, Bernie Not for Resale, 03/14/2007 19:59:26 MDTNo reproduction or networking permitted without license from IHS -,-,- JAPANESE INDUSTRIAL STANDARD JIS H 1059 : 2005 Methods for determination of arsenic in copper and copper alloys Introduction This Japanese Industrial Standard has been prepared by
14、 adopting the first edition of IS0 3220 Copper and copper alloys-Determination of arsenic- Photometric method published in 1975 for the corresponding part (clause 6, Bromide extraction separation molybdoarsenate blue absorptiometry) and by adding the clauses (those other than clause 6) not given in
15、the original International Standards, as pro- visions that are unique to the Japanese Industrial Standard. The portions given sidelines or dotted underlines are the matters which have been added to or modified from the original International Standard. A list of modifica- tions with the explanations
16、is given in annex (informative). 1 Scope per and copper alloys (wrought copper). This Standard specifies the methods for determination of arsenic in cop- The International Standard corresponding to this Standard is as fol- lows. In addition, symbols which denote the degree of correspondence in the c
17、ontents between the relevant International Standard and JIS are IDT (identical), MOD (modified), and NEQ (not equivalent) ac- cording to ISO/IEC Guide 21. IS0 3220 : 1975 Copper and copper alloys-Determination of arsenic- Photometric method (MOD) Remarks : 2 Normative reference The following standar
18、d contains provisions which, through reference in this text, constitute provisions of this Standard. The most recent edi- tion of the standard (including amendments) indicated below shall be applied. JIS H 1012 General rules for chemical analysis of copper and copper alloys 3 General matters dance w
19、ith JIS H 1012. General matters common to this method shall be in accor- 4 Classification of determination methods The method for determination of arsenic shall be in accordance with either of the following methods. they are applicable shall be as given in table 1. The determination methods and allo
20、y numbers of copper or copper alloys to which 4 Molybdoarsenate extraction absorptiometry This method applies to the sample of 0.005 % (m/m or over up to and including 0.08 % (m/m) in arsenic content. b) Bromide extraction separation molybdoarsenate blue absorptiometry This method applies to the sam
21、ple of 0.002 % (m/m) or over up to and including 0.8 % (m/m) in arsenic content. . PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 19:59:26 MDTNo reproduction or netw
22、orking permitted without license from IHS -,-,- 2 H 1059 : 2005 Alloy number C4430 Table 1 Determination method and subject alloy number Molybdoarsenate Bromide extraction extraction absorptiometry separation molybdoarsenate blue absorptiometry O O C6871 C6872 I C6870 I O I O I O O O O 5 Molybdoarse
23、nate extraction absorptiometry 5.1 Summary After decomposing a sample with the mixture of hydrochloric and nitric acid, it is joined by sodium hypobromite and hexaammonium heptamolybdate, and molybdoarsenic acid is generated. Thereafter, it is extracted with ethyl acetate, butanol and the absorbance
24、 is measured by using a photometer. Reagents The reagents shall be as follows: Mixed acid (hydrochloric acid 1, nitric acid 3, and water 4) Copper in arsenic content, and 0.000 3 % (m/m) max. in phosphorus content. Zinc arsenic content, and 0.000 3 % (m/m) max. in phosphorus content. Sodium hypobrom
25、ite solution 3 ml of bromine water (saturated), 11 ml of water, and 2 ml of sodium hydroxide solution (20 g/L) are mixed. This solution is prepared at each service. It is the copper of 99.96 % (m/m) min. in purity, 0.000 5 % (m/m) max. It is the zinc of 99.9 % (m/m) min. in purity, 0.000 5 % (m/m) m
26、ax. in Ammonium molybdate solution 10 g of hexaammonium heptamolybdate tetrahydrate is dissolved with water to 100 ml. This solution is prepared at each service. Ethyl acetate butanol mixed solvent (ethyl acetate 1 and butanol i) Arsenic standard solution (200 pgAs/ml) 0.265 g diarsenic trioxide is
27、weighed out, transferred into a beaker (200 mi) and dissolved by adding 10 ml of sodium hydroxide solution (20 g/L). It is diluted to approximately 50 ml with water, slightly acidified by adding 3 ml of sulfuric acid (1+10) and cooled to ordinary temperature. Thereafter, it is transferred into a tra
28、nsfer flask of 1 O00 ml by using water and diluted to the marked line with water. Weighing out amount of sample The weighing out amount of a sample shall be 2.00 g. 5.4 Operation PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employ
29、ees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 19:59:26 MDTNo reproduction or networking permitted without license from IHS -,-,- 3 H 1059 : 2005 5.4.1 Preparation of sample solution according to the following procedures: The sample solution shall be prepared a) Weigh out a sample and
30、transfer it into a beaker (300 mi). b) Cover it with a watch glass, add 30 ml of mixed acid and decompose it by gen- tly heating. After washing the bottom face of the watch glass and the inside wall of the beaker with water, expel nitrogen oxide or the like by gently boiling and cool it to ordinary
31、temperature. Thereafter, wash the bottom face of the watch glass and the inside wall of the beaker with water and remove the watch glass. Transfer the solution into a transfer flask of 50 ml by using water and dilute it to the marked line with water. c) 5.4.2 Extraction of complex cording to the fol
32、lowing procedures: The extraction of complex shall be conducted ac- a) Separately take 25.0 ml of the solution obtained in 5.4.1 c) into a separatory funnel (100 mi), accurately add 0.5 ml of sodium hypobromite solution 5.2 d) and let it stand for 5 min. b) After adding 3 ml of ammonium molybdate so
33、lution 5.2 e), let it stand for 15 min. Accurately add 20 ml of ethyl acetate butanol mixed solvent and mix them by shaking for 1 min. After letting it stand still until it separates into two phases discard the aqueous phase of the lower layer. 5.4.3 Measurement of absorbance Take a portion of the o
34、rganic phase obtained in 5.4.2 b) into the absorption cell (10 mm) of a photometer, utilizing ethyl acetate. butanol mixed solvent as contrast solution, and measure the absorbance at nearly 400 nm in wavelength. 5.5 Blank test The absorbance of the solution without addition of standard ar- senic sol
35、ution obtained in the working line preparing operation of 5.6 shall be made the absorbance of a blank test. 5.6 Weigh out copper 15.2 b) and zinc 15.2 c) and transfer them into each of several beakers (300 mi) so that respective mass con- tained in the samples weighed out in 5.4.1 a) becomes the sam
36、e mass to the nearest 10 mg. Operate each of the samples in accordance with the procedure of 5.4.1 b). After transferring the solution into a transfer flask of 50 ml by using water, stepwise add O to 8.0 ml of arsenic standard solution 5.2 g) (O to 1600 pg as arsenic) and dilute the solution to the
37、marked line with water. Separately take 25.0 ml of this solution into a separatory funnel (100 mi), accurately add 0.5 ml of sodium hypobro- mite solution 5.2 d) and let it stand for 5 min. Hereinafter, operate it in accor- dance with the procedures of 5.4.2 b) and 5.4.3, while at the same time cond
38、ucting the same procedure on the sample, and prepare the relation curve between the ob- tained absorbance and the amount of arsenic and in parallel translate the relation curve so as to pass through the origin to be the working curve. Preparation of working curve PROTECTED BY COPYRIGHT Copyright Jap
39、anese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 19:59:26 MDTNo reproduction or networking permitted without license from IHS -,-,- 4 H 1059 : 2005 5.7 Calculation The amount of arsenic shall be obtained
40、 from the absorbance to be obtained in 5.4.3 and 5.5 and the working curve prepared in 5.6 and the content of arsenic in a sample shall be calculated from the following formula: where, As : arsenic content in a sample % (m/m) Al : detection amount of arsenic in aliquot sample so- lution (g) As : det
41、ection amount of arsenic in aliquot blank test solution (g) m : weighing out amount of sample (g) 6 Bromide extraction separation molybdoarsenate blue absorptiometry 6.1 Summary A sample is decomposed with hydrochloric acid and hydrogen per- oxide and concentrated by heating. After adding hydrochlor
42、ic acid, hydrobromic acid, and perchloric acid, arsenic is extracted with benzene as bromide. After washing the organic phase with hydrochloric acid, arsenic is back-extracted with water. It is joined by potassium permanganate and arsenic (III) is oxidized to arsenic (V) by heating. It is then joine
43、d by hexaammonium heptamolybdate and ascorbic acid, heated, and molybdoarsenate blue complex is generated. Its absorbance is measured by using a photometer. Reagents The reagents shall be as follows: Hydrochloric acid Hydrochloric acid (l+l) Perchloric acid 70 % (m/m)l Hydrobromic acid Copper max. i
44、n arsenic content. It is the copper of 99.96 % (m/m) min. in purity and 0.000 5 % (m/m) Hydrogen peroxide Potassium permanganate solution (3.2 g/L) Ammonium molybdate solution 0.95 g of hexaammonium heptamolybdate tetrahydrate is dissolved with 200 ml of sulfuric acid (1+20). This solution is prepar
45、ed at each service. L(+)-Ascorbic acid solution (20 g/L) This solution is prepared at each service. Benzene Standard arsenic solution (20 pgAs/ml) 0.132 g of diarsenic trioxide is weighed out, transferred into a polyethylene beaker (100 mi), dissolved by adding 10 ml PROTECTED BY COPYRIGHT Copyright
46、 Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 19:59:26 MDTNo reproduction or networking permitted without license from IHS -,-,- 5 H 1059 : 2005 Arsenic content %I (mm) 0.002 or over to and excl.
47、0.02 of sodium hydroxide solution (40 g/L) and joined by 12.5 ml of hydrochloric acid (l+ll). Thereafter, it is transferred into a transfer flask of 250 ml by using water and diluted to the marked line with water to prepare stock solution (400 pgAs/ml). Accurately 25 ml of this solution is taken at
48、each service, joined by 20 ml of hydrochloric acid (l+i) and diluted accurately to the marked line with water to prepare standard arsenic solution. Weighing out amount of sample g 1.00 6.3 be as given in table 2. Weighing out amount of sample The weighing out amount of a sample shall Table 2 Weighing out amount of sample 0.04 or over to and excl. 0.08 0.08 or over to and excl. 0.2 0.25 0.50 I 0.02 or over to and excl. 0.04 I 0.50 I 0.2 or over up to and incl. 0.8 I 0.25 6.4 Operation 6.4.1 Decomposition of sample Weigh out a sample, transfer it into a beaker (100 mi